Lactam-containing Reactant Patents (Class 528/323)
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Publication number: 20090005532Abstract: In various embodiments, the present invention can involve a method of synthesizing ?-amino-?-caprolactam. The method can comprise heating a salt of L-lysine in a solvent comprising an alcohol. In other embodiments, the present invention can involve methods for synthesizing ?-caprolactam. The methods can comprise heating a salt of L-lysine in a solvent comprising an alcohol and deaminating the reaction product. In various embodiments, the invention can include methods of converting biomass into nylon 6. The methods can comprise heating L-lysine in a solvent comprising an alcohol to produce ?-amino-?-caprolactam, deaminating to produce ?-caprolactam and polymerizing into nylon 6, wherein the L-lysine is derived from the biomass. In other embodiments, the present invention can include methods of making nylon 6. The methods can comprise synthesizing ?-caprolactam and then polymerizing, wherein the ?-caprolactam is derived from L-lysine.Type: ApplicationFiled: June 26, 2008Publication date: January 1, 2009Applicant: Board of Trustees of Michigan State UniversityInventor: John W. Frost
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Patent number: 7470765Abstract: A process for preparing a polyamide by reacting a mixture which comprises a monomer which has a nitrile group and has at least one other functional group capable of forming a carboxamide group, and comprises water, in the presence of titanium dioxide as catalyst, which comprises using titanium dioxide whose BET surface area, determined to the German standard DIN 66 131 volumetrically by the multipoint method, is in the range from 5 to 35 m2/g.Type: GrantFiled: April 8, 2003Date of Patent: December 30, 2008Assignee: BASF AktiengesellschaftInventors: Helmut Winterling, Christoph Benisch, Thilo Hahn
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Publication number: 20080221265Abstract: A process for preparing a hyperbranched polymer having a weight-average molar mass of at least 30,000, includes coupling a first prepolymer having at least three functional end groups with a second prepolymer having at least two functional end groups by a dehydration condensation reaction between the end groups in the prepolymers. The number of arms and/or molar mass of the functionalized prepolymers can accurately be adjusted, thus affecting the properties of the resulting hyperbranched polymer in a desired way. The polymer can be equipped e.g. with hydrophobic and hydrophilic parts. Also, the number of functional end groups, that optionally can be used for further chemical reactions, in the hyperbranched polymer can easily be adjusted to a desired level. The hyperbranched high molar mass polymer can be prepared in high yields without the use of organic solvents or linking compounds, which is advantageous from an environmental as well as an economical point of view.Type: ApplicationFiled: May 30, 2003Publication date: September 11, 2008Inventors: Niels Dan Anders Sodergard, Erik Mikael Stolt
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Publication number: 20080146738Abstract: The present invention provides curatives for thermosetting adhesive compositions, methods of preparation and uses thereof. In particular, the present invention relates to elastomeric epoxy curative compounds that can be used in thermosetting compounds, methods for preparing the curative compounds and epoxy compositions containing the curative compounds.Type: ApplicationFiled: December 19, 2007Publication date: June 19, 2008Inventor: Stephen M. Dershem
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Patent number: 7388048Abstract: The present invention relates to a flexible semiaromatic polyamide composition with a low moisture uptake comprising, by weight, the total being 100: 60 to 99.5% (preferably 70 to 93%) of at least one copolyamide of formula X/Y,Ar in which: Y denotes the residues of an aliphatic diamine having from 8 to 20 carbon atoms, Ar denotes the residues of an aromatic dicarboxylic acid, X denotes either the residues of aminoundecanoic acid NH2—(CH2)10—COOH, of lactam-12 or of the corresponding amino acid, or X denotes the unit Y,x, residue from the condensation of the diamine with an aliphatic diacid (x) having between 8 and 20 carbon atoms, or X denotes the unit Y,I, residue from the condensation of the diamine with isophthalic acid, ?0.5 to 40% (preferably 7 to 30%) of at least one product chosen from plasticizers, nanofillers, polyolefins, crosslinked polyolefins and additives.Type: GrantFiled: August 2, 2004Date of Patent: June 17, 2008Assignee: Arkema FranceInventors: Philippe Blondel, Thierry Briffaud, Annett Linemann, Helene Egret, Pierre Nogues
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Patent number: 7381788Abstract: Provided is a continuous production method of a polyamide with stabilized polymerization degree and good quality, particularly an aromatic-containing polyamide.Type: GrantFiled: August 27, 2003Date of Patent: June 3, 2008Assignee: Toyo Boseki Kabushiki KaishaInventors: Yasuhito Tsujii, Gaku Maruyama, Kaoru Ogawa, Yoshinori Takada, Kazuhisa Koishi, Kenta Susuki
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Patent number: 7183352Abstract: The present invention relates to novel polyesterpolyols with cyclic imide structure and to their use in coating compositions.Type: GrantFiled: August 11, 2003Date of Patent: February 27, 2007Assignee: Bayer MaterialScience AGInventors: Christian Wamprecht, Hans-Gerd Van Treek, Raul Pires, Ulrich Freudenberg, Robert Reyer
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Patent number: 7148307Abstract: The present invention relates to novel polyesterpolyols with cyclic imide and isocyanurate structure and to their use in coating compositions.Type: GrantFiled: August 11, 2003Date of Patent: December 12, 2006Assignee: Bayer AktiengesellschaftInventors: Christian Wamprecht, Raul Pires, Ulrich Freudenberg, Robert Reyer
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Patent number: 7049391Abstract: The invention relates to a method for reducing the caprolactam content of polyamide 6 obtained especially by hydrolytic polymerization of epsilon-caprolactam. The method is characterized by the use of an additive that forms isocyanuric acid under the influence of heat. The additive or the isocyanuric acid produced externally under the influence of heat is added (a) to the polymerization or (b) to a melt of polyamide 6. This enables the caprolactam content of the polyamide 6 to be reduced considerably compared to that of usual commercial polyamide 6. In particular, the resulting polyamide 6 shows good characteristics for reprocessing e.g. into fiber and molding masses by melt extension.Type: GrantFiled: September 24, 2001Date of Patent: May 23, 2006Assignee: BASF AktiengeselleschaftInventors: Frank Gähr, Frank Hermanutz, Mirko Peczyoski
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Patent number: 6984393Abstract: This invention relates to thermally crosslinked and photo-crosslinked biodegradable and biocompatible elastomeric polymers. The elastomers can be used for biomedical devices such as needles, stents, catheters, scaffolds for tissue engineering, and implantable drug delivery devices. The photo-crosslinked elastomers are particularly useful for delivery devices for proteins and peptides.Type: GrantFiled: May 7, 2002Date of Patent: January 10, 2006Assignee: Queen's University at KingstonInventor: Brian G. Amsden
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Patent number: 6958381Abstract: A process for preparing polyamides comprises polymerizing starting monomers in the presence of from 2.3 to 10 mmol, based on 1 mol of carboxamide group of the polyamide, of a chain regulator containing a nitrile group and a functional group capable of forming a carboxamide group.Type: GrantFiled: November 22, 2001Date of Patent: October 25, 2005Assignee: BASF AktiengesellschaftInventors: Helmut Winterling, Michael Fischer
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Patent number: 6916901Abstract: The present invention provides a method for the production of polyamide 6 by the hydrolytic polymerization of ?-caprolactam, in which, in the first step, caprolactam ring opening occurs under the action of water and, in the following steps, polycondensation is performed at low temperatures under anhydrous conditions.Type: GrantFiled: November 7, 2002Date of Patent: July 12, 2005Assignee: Bayer AktiengesellschaftInventors: Sven Gestermann, Ralph Ulrich
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Patent number: 6906165Abstract: The invention concerns copolyamides obtained by using multifunctional monomers. It consists in using a multifunctional monomer comprising at least three reactive functions and at least another multifunctional monomer, in amounts such that the terminal group concentrations are balanced. The copolyamides are particularly high viscosity copolyamides. The invention also concerns compositions based on said copolyamides.Type: GrantFiled: August 7, 2001Date of Patent: June 14, 2005Assignee: Rhodia Engineering Palstics S.R.L.Inventors: Giuseppe Di Silvestro, Franco Speroni, Cuiming Yuan, Haichun Zhang
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Patent number: 6884865Abstract: The invention concerns copolyamides obtained by using multifunctional monomers. It consists in using at least one multifunctional monomer comprising at least three reactive functions and at least another multifunctional monomer, in amounts such that the terminal group concentrations are balanced. The copolyamides are more particularly high viscosity copolyamides. The invention also concerns compositions based on said copolyamides.Type: GrantFiled: August 7, 2001Date of Patent: April 26, 2005Assignee: Rhodia Engineering Plastics S.R.L.Inventors: Giuseppe Di Silvestro, Franco Speroni, Cuiming Yuan, Haichun Zhang
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Patent number: 6881819Abstract: The invention relates to a liquid initiator for carrying out anionic lactam polymerization. The liquid initiator contains a conversion product of isocyanate (1) with a protic compound (P) and a base (B) in an aprotic solvation agent (S).Type: GrantFiled: November 30, 2000Date of Patent: April 19, 2005Assignee: EMS-Chemie AGInventors: Eduard Schmid, Ivano Laudonia
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Patent number: 6878798Abstract: A process for preparing a polymer, which comprises a) reacting a mixture (I) containing 6-aminocapronitrile and water in the presence of a catalyst to obtain a mixture (II) containing caprolactam, ammonia, water, high boilers and low boilers, then b) removing ammonia from mixture (II) to obtain a mixture (III) containing caprolactam, water, high boilers and low boilers, then c) removing all or some of the water from mixture (III) to obtain a mixture (IV) containing caprolactam, high boilers and low boilers and then d) feeding mixture (IV) to a polymerization reaction, and also the polymer obtainable by this process, the use of the polymer for producing fibers, sheetlike structures and moldings, and also fibers, sheetlike structures and moldings obtainable using such a polymer.Type: GrantFiled: April 30, 2001Date of Patent: April 12, 2005Assignee: BASF AktiengesellschaftInventors: Frank Ohlbach, Helmut Winterling, Andreas Ansmann, Rolf-Hartmuth Fischer, Johann-Peter Melder, Stefan Maixner, Peter Bassler, Hermann Luyken
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Patent number: 6875838Abstract: Disclosed is a process for reducing low molecular weight impurities, namely caprolactam and its oligomers, from Nylon-6 pre-polymer during the preparation of Nylon-6 polymer.Type: GrantFiled: April 28, 2003Date of Patent: April 5, 2005Assignee: Invista North Americal S.a.r.l.Inventors: Albert W. Alsop, Carl E. Camp, John M. Iwasyk, Dilip Rajagopalan
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Patent number: 6872800Abstract: The invention relates to hyperbranched copolyamides (HBPAs), to their production and to their use as additives, in particular as melt viscosity modifiers in thermoplastic polymer compositions. This copolyamide is obtained by a reaction between a monomer (I): A—R—Bf with A and B=polymerization functions of a 1st and 2nd type, respectively, which are capable of reacting with each other, R=hydrocarbon-based species and f=total number of B per monomer (preferably 2?f?10); and a monomer (II) A?—R?—B? or the corresponding lactams, with A?, B? and R? having the same definition as that given above for A, B and R, respectively. This HBPA has a I/II molar ratio such that 0.125?I/II?2. One of the species R or R? of (I) or (II) is aliphatic, cycloaliphatic or arylaliphatic. For example: A=NH2 and B=COOH or A=COOH and B=NH2 with F=2. A?=NH2 and B?=COOH or A?=COOH and B?=NH2. A—R—B2, e.g.: 5-aminoisophthalic acid or 3,5-diaminobenzoic acid and A?—R?—B?=?-caprolactam.Type: GrantFiled: May 5, 2000Date of Patent: March 29, 2005Inventors: Franck Bouquerel, Jean-Francois Sassi
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Patent number: 6852829Abstract: A process for the simultaneous preparation of polyamide-6 with at least two different viscosities comprising prepolymerisation of ?-caprolactam and/or other polyamide-6 precursors in the presence of water, wherein at least part of the necessary water is supplied to the prepolymerisation via the gas phase and the obtained prepolymer is progressively moved and treated with an inert gas in at least two condensation reaction zones or reactors, placed in series, and the prepolymerisation and condensation are carried out in reactor(s) or reaction zones having a self-renewing interface between molten phase and gas phase with a large surface/volume ratio of the molten phase and the molten phase is relatively strong mixed.Type: GrantFiled: April 17, 2001Date of Patent: February 8, 2005Assignee: DSM N.V.Inventor: Wim Buijs
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Patent number: 6846904Abstract: After a melt-processable fluorine-containing copolymer is heated and molten, the copolymer is reheatd in a closed apparatus under a non-static condition at a temperature of, for example, 130° C. to the melting point of the fluorine-containing polymer, whereby a content of volatile materials in the copolymer is reduced to 30% or less of an initial content of volatile materials. Thereby, the content of volatile materials in the melt-processable fluorine-containing copolymer, which has been once molten, can be effectively decreased without using a large apparatus while avoiding the contamination of the copolymer with foreign particles.Type: GrantFiled: August 24, 2000Date of Patent: January 25, 2005Assignee: Daikin Industries, Ltd.Inventors: Hiroyuki Imanishi, Yoshiyuki Hiraga, Masayuki Namimatsu, Satoshi Komatsu
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Patent number: 6846901Abstract: The invention relates to a liquid initiator to be used in anionic lactam polymerization. Said liquid initiator contains a reaction product of carbodiimide with a protic compound and a base in an aprotic solvation agent.Type: GrantFiled: November 28, 2000Date of Patent: January 25, 2005Assignee: EMS-Chemie AGInventors: Eduard Schmid, Ivano Laudonia
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Patent number: 6835799Abstract: The invention relates to a randomly branched polyamide comprising at least units derived from: 1. AB monomers, 2. at least one compound I, being a carboxylic acid (Av) having a functionality v≧2 or an amine (Bw) having a functionality w≧2, 3. at least one compound II, being a carboxylic acid (Av) having a functionality v≧3 or an amine (Bw) having a functionality w≧3, compound II being a carboxylic acid if compound I is an amine or compound II being an amine if compound I is a carboxylic acid and the amounts of all units derived from carboxylic acids and amines in the polyamide satisfying conditions as mentioned in claim 1. The composition of the randomly branched polyamide is such that it cannot form a crosslinked polyamide (and thus no gels, either), in particular during the prepolymerization, the polymerization, the post-condensation, the processing and the storage of the randomly branched polyamide, and this at a variety of ambient factors, for instance at elevated temperature and pressure.Type: GrantFiled: June 18, 2001Date of Patent: December 28, 2004Assignee: DSM IP Assets B. V.Inventors: Atze J. Nijenhuis, René Aberson, Boudewijn J. R. Scholtens
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Patent number: 6835800Abstract: A method for preparing a nylon 6 copolymer containing dimeric acid comonomers. The method includes reacting 80.0˜99.9 mol % of caprolactam, 0.1˜3.0 mol % of dimeric acid and 0.1˜3.0 mol % of 2-methyl-1,5-pentadiamine in a polymerization reaction. Moreover, the invention provides a method for preparing a nylon 66 copolymer containing dimeric acid comonomers, which comprising reacting 60.0˜90 mol % of hexadiacid and hexadiamine, 0.1˜3.0 mol % of dimeric acid and 0.1-3.0 mol % of 2-methyl-1,5-pentadiamine in a polymerization reaction. The reaction temperature for both of the methods are at 200˜280° C.Type: GrantFiled: December 23, 2002Date of Patent: December 28, 2004Assignee: Industrial Technology Research InstituteInventors: Tun-Fun Way, Cheng Yeh, Hsiang-In Tang, Lien-Tai Chen
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Patent number: 6828413Abstract: The invention relates to a process for the preparation of a polyamide comprising at least a step in which a composition that comprises at least (a) a primary aminocarbonamide and (b) an aminocarboxylic acid and/or a lactam is polymerised, said composition comprising at least (a) 10-90 wt. % primary aminocarbonamide; (b) 10-90 wt. % aminocarboxylic acid and/or lactam; (c) 0-4 wt. % water; the amounts being relative to the sum of the compounds (a+b+c). Preferably the sum of the compounds (a+b+c) is at least 75 wt. % of the total composition, more preferably 85 wt. %, most preferably 90 wt. %. The polyamide obtained with the process has a &eegr;rel of more than 2.2. The process is eminently suitable for the preparation of polyamide-6 (polycapronamide) from a composition comprising 6-aminocapronamide, 6-aminocaproic acid and/or &egr;-caprolactam. This composition is preferably obtained via the reductive amination of a 5-formylyalerate ester, preferably 5-formylmethylvalerate in water.Type: GrantFiled: June 24, 2002Date of Patent: December 7, 2004Assignee: OSM IP Asseta, B.V.Inventors: Cornelis E. Koning, Rudy Rulkens, Nicolaas F. Haasen, Albert A. Van Geenen
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Patent number: 6818732Abstract: A series of initiators based on transition metal complexes for the polymerization of optically active beta-lactams into poly-beta-peptides and block copolymers have been developed. These initiators are unique in being able to eliminate chain transfer and chain termination side reactions from these polymerizations resulting in narrow molecular weight distributions, molecular weight control, and the ability to prepare copolymers of defined block sequence and composition.Type: GrantFiled: August 30, 2002Date of Patent: November 16, 2004Assignee: The Regents of the University of CaliforniaInventors: Timothy J. Deming, Jianjun Cheng
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Patent number: 6815527Abstract: The continuous process for preparing a polyamide by reacting at least one aminonitrile with water comprises: (1) reacting at least one aminonitrile with water in the presence of an organic liquid diluent at from 90 to 400° C. and from 0.1 to 35×106 Pa in a flow tube containing a Brönsted acid catalyst selected from a beta-zeolite catalyst, a sheet-silicate catalyst or a titanium dioxide catalyst comprising from 70 to 100% by weight of anatase and from 0 to 30% by weight of rutile and in which up to 40% by weight of the titanium dioxide may be replaced by tungsten oxide, to obtain a reaction mixture, (2) further reacting the reaction mixture at from 150 to 400° C.Type: GrantFiled: January 10, 2003Date of Patent: November 9, 2004Assignee: BASF AktiengesellschaftInventors: Peter Bassler, Helmut Winterling, Rolf-Hartmuth Fischer, Wolfgang Loth
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Publication number: 20040217582Abstract: A composition comprises a solid-stated block copolymer of an aromatic polyester and a caprolactone, wherein the copolymer has been solid state polymerized such that intrinsic viscosity increases at least 20%, the caprolactone content decreases no more than 1.2% absolute and the transesterification increases no more than 3.5% absolute, and wherein the solid-stated copolymer has an intrinsic viscosity of at least 0.82. Particularly preferred chain extension reactions are performed at a temperature of less than 175° C., and even more preferably at less than 165° C. In further aspects of the inventive subject matter, yarns and methods of producing a fiber include contemplated solid-stated block copolymers.Type: ApplicationFiled: June 7, 2004Publication date: November 4, 2004Inventors: Srinivasan Sridharan, John Armstrong Young, Donald James Arthur, Thomas Yiu-Tai Tam
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Patent number: 6812324Abstract: A method for preparing nylon 6 copolymer containing 5-sulfoisophthalate salts comonomer. The method includes the steps of reacting 5-sulfoisophthalate salts ester with aliphatic diamine in a molar ratio of 2˜20 at 160˜200° C., followed by completely removing the unreacted aliphatic diamine, to obtain the intermediate compound with terminal amine, 5-sulfobenzenediamide compound (formula III). Next, caprolactam and aliphatic diacid (formula IV) are reacted at 200˜260° C. to form an oligomer with a low molecular weight. 5-Sulfobenzenediamide (formula III) and catalyst are then added into the oligomer obtained in previous step to cause a polymerization reaction at 200˜280° C. to obtain nylon 6 copolymer containing 5-sulfoisophthalate salt comonomer. The molar ratio of E/C is 0.005˜0.150 and the molar ratio of D/E is 1.05-1.00. Compounds present in the water extract are greatly reduced.Type: GrantFiled: December 23, 2002Date of Patent: November 2, 2004Assignee: Industrial Technology Research InstituteInventors: Tun-Fun Way, Cheng Yeh, Lien-Tai Chen, Chia-Hung Chen
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Patent number: 6812322Abstract: A process for the preparation of novel polyamides, the use of such polyamides for the production of fibers, sheets and moldings, and fibers, sheets and moldings obtainable from such polyamides, are provided.Type: GrantFiled: December 26, 2002Date of Patent: November 2, 2004Assignee: BASF AktiengesellschaftInventors: Paul-Michael Bever, Ulrike Breiner, Bernd-Steffen von Bernstorff, Gerhard Conzelmann
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Patent number: 6812323Abstract: A process for preparing polyamides comprises polymerizing starting monomers or starting oligomers in the presence of at least one compound of the formula (I) where R is a functional group R8 which bears 1-4 identical or different amide-forming groups R7, R1 is H, C1-C20-alkyl, cycloalkyl, benzyl or OR6, where R6 is H, C1-C20-alkyl, cycloalkyl or benzyl, R2, R3, R4 and R5 are independently C1-C10-alkyl, n is a natural number greater than 1, and the piperidine derivatives attached to R are identical or different with regard to the substituents, meaning R1, R2, R3, R4 and R5. The polyamides are useful for preparing filaments, fibers, films, sheetlike structures and moldings.Type: GrantFiled: September 14, 2000Date of Patent: November 2, 2004Assignee: BASF AktiengesellschaftInventors: Ulrike Breiner, Manfred Julius, Rainer Neuberg, Robert Weiss, Axel Wilms, Harry Y. Hu
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Patent number: 6809173Abstract: The invention relates to a polyamide with low viscosity degradation after remelting which can be produced by anionic polymerization of lactam in the presence of alkaline catalysts and if necessary activators and the method for production of the polyamide. The invention relates furthermore to a method for reprocessing anionically produced polyamide.Type: GrantFiled: April 11, 2002Date of Patent: October 26, 2004Assignee: EMS-Chemie AGInventors: Eduard Schmid, Ivano Laudonia, Hansjörg Ernst, Werner Kägi
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Patent number: 6780963Abstract: The polyamide resin composition of the invention is characterized by having a solder reflow heat-resistant temperature of not lower than 250° C. Since the polyamdie resin composition has low water absorption and is excellent in moldability, heat resistance, shape stability and mechanical strength, it can be suitably used for, for example, automobile parts and electric or electronic parts.Type: GrantFiled: August 21, 2002Date of Patent: August 24, 2004Assignee: Mitsui Chemicals, Inc.Inventors: Masahiro Sawada, Kunihiro Ohuchi
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Patent number: 6774208Abstract: A two step method for solid state polymerization of dry crystalline thermoplastic polymers to form polymers with superior mechanical properties, first by mechanically fluidizing dry crystalline thermoplastic polymer particles in the absence of oxygen by means of blades moving through the fluidized polymer particles at velocities sufficient to heat the particles to an incipient melt temperature and maintain the temperature until solid state polymerization provides the desired molecular weight and before chemical degradation of the polymer occurs; and second by immediately quenching by application of liquefied cryogenic gases directly to the surfaces of the polymer particles in amounts sufficient to cool the particles to temperatures lower than the glass transition temperature of the polymer before crystals in the polymer aggregate into large spherulites.Type: GrantFiled: June 30, 2003Date of Patent: August 10, 2004Assignee: Agri-Nutrients Technology Group, Inc.Inventor: William P. Moore
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Patent number: 6774205Abstract: A process for the preparation of novel polyamides, the use of such polyamides for the production of fibers, sheets and moldings, and fibers, sheets and moldings obtainable from such polyamides, are provided.Type: GrantFiled: December 26, 2002Date of Patent: August 10, 2004Assignee: BASF AktiengesellschaftInventors: Paul-Michael Bever, Ulrike Breiner, Bernd-Steffen von Bernstorff, Gerhard Conzelmann
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Patent number: 6767988Abstract: Polyamide elastomer comprising a hard segment derived from polyamide having no divalent aromatic group and a soft segment derived from polycarbonate diol having no divalent aromatic group has high flexibility and high heat resistance in addition to good physical characteristics of the known polyamide elastomers.Type: GrantFiled: April 23, 2002Date of Patent: July 27, 2004Assignee: UBE Industries, Ltd.Inventors: Hiroshi Okushita, Tadao Muramatsu
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Patent number: 6765081Abstract: A thermal responsive, water soluble polymer. The polymer comprises the co-polymerization product of: (a) 5˜95 wt % of N-isopropyl acrylamide (NIP); (b) 0.1˜80 wt % of 1-vinyl-2-pyrrolidinone (VPD); and optionally, (c) 0.1˜30 wt % of acrylic acid (AA). As the proportion of component (b) VPD increases, the Lower Critical Solution Temperature (LCST) and water solubility of the polymer increases. On the other hand, as the proportion of component (c) AA increases, the Lower Critical Solution Temperature (LCST) decreases and the COOH reactive groups increases, which impart high reactivity to the copolymer. By adjusting the proportion of the monomers, a broad range of LCST can be manipulated from about 20 to 80° C.Type: GrantFiled: May 2, 2002Date of Patent: July 20, 2004Assignee: Industrial Technology Research InstituteInventors: Chih-Hsiang Lin, In-Mau Chen, Wen-Ling Lui
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Publication number: 20040127678Abstract: The present invention relates to a process for preparing polyamide 6 (PA 6) by hydrolytic polymerization of &egr;-caprolactam. In a first reaction step, a first intermediate mixture is formed by ring opening &egr;-caprolactam in the presence of water, under conditions of increased pressure and temperature. The first intermediate mixture is then dehydrated to form a dehydrated intermediate having a water content of less than 0.5 wt. %. The dehydrated intermediate is subsequently polymerized to. produce a polyamide 6 product having a low dimer content (e.g., of less than 0.3 wt. %). The invention also relates to an apparatus in which the process may be performed. The apparatus includes, in sequence, a pressure reactor (23) having heat exchange surfaces (36), a dehydration device (24) that is in fluid communication with the pressure reactor (23), and a main reactor (25) that is in fluid communication with the dehydration device (24).Type: ApplicationFiled: November 4, 2003Publication date: July 1, 2004Inventors: Ralph Ulrich, Konrad Triebeneck
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Patent number: 6750312Abstract: A method for preparing a solid support material for carrying out a chemical reaction, said method comprising the following steps: (i) reacting an amino functionalised solid material with a carboxylic acid having at least two similarly protected amino groups to form amide bonds between them, (ii) removing protecting groups in a single step, (iii) optionally repeating steps (i) and (ii) one or more times using the product of the preceding step as the amino functionalised solid material, and (iv) connecting a linkage agent to at least some of the free NH2 groups of the product. The method increases the loading capacity of the solid support material. It is particularly useful in connection with peptide synthesis.Type: GrantFiled: March 26, 2002Date of Patent: June 15, 2004Assignee: Avecia LimitedInventors: Craig Stephen Harris, Donald Alfred Wellings, Francis Joseph Montgomery, Richard John Brown
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Patent number: 6750316Abstract: The invention relates to a process for preparing a high-molecular polyamide or polyester by melt-mixing polyamide or polyester having a lower molecular weight with a carbonyl bislactam having formula 1, in which n=an integer of between 3 and 15. With the process according to the invention a permanent increase in the molecular weight of a polyamide is obtained within 2 minutes, whereas this takes at least 10 minutes under comparable conditions using a bislactam according to the state of the art.Type: GrantFiled: April 19, 2002Date of Patent: June 15, 2004Assignee: DSM N.V.Inventors: Jacobus A. Loontjens, Bartholomeus J. M. Plum, Petrus M. M. Nossin
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Patent number: 6747120Abstract: The invention relates to a semi-aromatic polyamide containing at least tetramethylene terephthalamide units and also hexamethylene terephthalamide units. The copolyamide has a melting point higher than approximately 290° C., a high crystallinity and a good stability. Preferably the copolyamide according to the invention contains approximately 30-75 mol % hexamethylene terephthalamide units and also approximately 0.01-20 mol % other units. The invention also relates to a process for the preparation of a semi-aromatic copolyamide containing at least tetramethylene terephthalamide units and hexamethylene terephthalamide units, characterized in that, successively, a first polymerization is effected in the melt phase, followed by an post-polymerization of the low molar mass polymer thus obtained in the solid phase; and to compositions and products that contain said copolyamide.Type: GrantFiled: March 29, 2002Date of Patent: June 8, 2004Assignee: DSM IP Assets B.V.Inventors: Rudy Rulkens, Robert C. B. Crombach
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Patent number: 6737499Abstract: A process for using low-molecular weight compounds that are water-extracted from (co)polyamides in the production of polyamide is disclosed. The process entails reacting these compounds with 10 to 15 wt. % water for a period of 3.5 to 6 hours at a temperature of 220° C. to 270° C., and polymerizing the resulting product along with caprolactam.Type: GrantFiled: May 15, 2002Date of Patent: May 18, 2004Assignee: Bayer AktiengesellschaftInventors: Heinrich Haupt, Dieter Göbbels, Konrad Triebeneck, Andreas Gittinger
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Patent number: 6713596Abstract: The invention relates to a novel process for the anionic polymerization of lactams, in which: (a) (i) a catalyst capable of creating a lactamate and (ii) a regulator chosen from the amides of formula R1—NH—CO—R2, in which R1 can be substituted with a radical R3—CO—NH— or R3—0— and in which R1, R2 and R3 denote an aryl, alkyl or cycloalkyl radical, are dissolved in the molten lactam; the temperature of this reaction mixture being between the melting point of the lactam and 15° C. higher in order to ensure its good stability, (b) the solution from step (a) is introduced into a mixing device and is then heated to a temperature which is sufficient to obtain bulk polymerization of the lactam in no more than 15 minutes. (b) is usually a continuous reactor, for example an extruder; however, it can be replaced with a mold.Type: GrantFiled: January 29, 2002Date of Patent: March 30, 2004Assignee: AtofinaInventors: Heike Faulhammer, Michel Biensan, Franck Victorien, Thierry Vivier
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Publication number: 20040054123Abstract: A mixture substantially comprising caprolactam and water is heated for at most 30 minutes to obtain a polyamide prepolymer having an amino end group content of at least 0.1 mmol/g and a cyclic oligomer content of at most 0.6% by weight. An aqueous solution of caprolactam having a water content of from 2 to 20% by weight is heated under pressure at a temperature of from 200 to 330° C. for 1 to 30 minutes to obtain a polyamide prepolymer having an amino group content of at least 0.1 mmol/g and a cyclic oligomer content of at most 0.6% by weight.Type: ApplicationFiled: June 18, 2003Publication date: March 18, 2004Inventors: Yasuto Tachibana, Minoru Noda, Toru Nishimura
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Patent number: 6703475Abstract: A process for continuous production of copolyamides based on a lactam (I), a diamine (II) and a dicarboxylic acid (III) comprises reacting a mixture (IV) comprising a diamine (II), a dicarboxylic acid (III) and water in a first reaction zone at a pressure in the range from 1.3*105 to 2.5*105 Pa in the entry zone of the reaction zone and at a temperature above the melting point of polymer (V) to a conversion, based on the molar amounts of diamine (II) and dicarboxylic acid (III), of at least 80% to form a polymer (V), reacting a mixture (VI) comprising lactam (I) and water in a second reaction zone at a pressure in the range from 5*105 to 40*105 Pa and at a temperature above the melting point of polymer (VII) to a conversion, based on the molar amount of lactam (I), of at least 80% to form a polymer (VII), then reacting polymer (V) and polymer (VII) with each other in a third reaction zone at a pressure in the range from 1*105 to 1.Type: GrantFiled: May 13, 2002Date of Patent: March 9, 2004Assignee: BASF AktiengesellschaftInventors: Jürgen Deininger, Walter Götz, Alfons Ludwig, Gunter Pipper
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Patent number: 6703476Abstract: Polyamides are prepared from aminonitriles and water by (1) reacting the aminonitriles with water at from 180 to 350° C. and such a pressure in the range from 30 to 120 bar that a gaseous phase is present as well as a liquid phase, in a first reaction stage, (2) expanding the reaction mixture obtained in the first reaction stage via an evaporator zone or adiabatically with removal of water and ammonia into a second reaction stage, and (3) postcondensing in the second reaction stage at from 0.1 mbar to 5 bar and from 230 to 320° C.Type: GrantFiled: June 24, 2002Date of Patent: March 9, 2004Assignee: BASF AktiengesellschaftInventors: Ralf Mohrschladt, Helmut Winterling, Dieter Krauss
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Patent number: 6699960Abstract: A polyamide is prepared by reacting at least one dinitrile and at least one diamine with water at a temperature from 90 to 400° C. and a pressure from 0.1 to 50*106 Pa in a molar ratio of at least 1:1 for water to the sum total of dinitrile and diamine in the presence of a heterogeneous catalyst selected from the group consisting of aluminum oxide, tin oxide, silicon oxide, oxides of the second to sixth transition group of the periodic table, oxides of the lanthanides and actinides, sheet-silicates and zeolites.Type: GrantFiled: January 29, 2002Date of Patent: March 2, 2004Assignee: BASF AktiengesellschaftInventors: Frank Ohlbach, Hermann Luyken
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Patent number: 6699962Abstract: A process for removing low molecular weight constituents from polyamide 6 or from copolyamides based on caprolactam (herein (co)polyamide) is disclosed. The process comprise subjecting the (co)polyamide to liquid-extraction at a temperature which is above the boiling point of the liquid at atmospheric pressure said liquid containing water in an amount of at least 80 percent relative to its weight.Type: GrantFiled: May 15, 2002Date of Patent: March 2, 2004Assignee: Bayer AktiengesellschaftInventors: Heinrich Haupt, Dieter Göbbels, Konrad Triebeneck, Andreas Gittinger
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Patent number: 6680364Abstract: The invention describes polyamides having both strongly hydrophilic groups and unsaturated groups, the polyamides consequently being water-dispersible and curable. The hydrophilic groups are distributed along the chain, whereas the unsaturated groups are located at the ends. The polyamides of the invention are useful in many applications, especially in the preparation of intimate blends of polyamides with vinyl, acrylic and/or styrene polymers.Type: GrantFiled: February 22, 2002Date of Patent: January 20, 2004Assignee: AtofinaInventor: Reinhard Linemann
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Publication number: 20030232962Abstract: A polyamide that includes the reaction product of dimer acid (e.g. a dimer acid including at least 98 % by weight dimer), caprolactam, hexamethylene diamine, sebacic acid, and optionally, chain terminating agent.Type: ApplicationFiled: June 14, 2002Publication date: December 18, 2003Inventors: Steven L. Scholl, Sharf U. Ahmed, Andualem W. Emiru
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Patent number: RE39354Abstract: A laser-sinterable powder product has been prepared having unique properties which allow the powder to be sintered in a selective laser sintering machine to form a sintered part which is near-fully dense. For most purposes, the sintered part is indistinguishable from another part having the same dimensions made by isotropically molding the powder. In addition to being freely flowable at a temperature near its softening temperature, a useful powder is disclosed that has a two-tier distribution in which substantially no primary particles have an average diameter greater than 180 ?m, provided further that the number average ratio of particles smaller than 53 ?m is greater than 80%, the remaining larger particles being in the size range from 53 ?m to 180 ?m. A powder with slow recrystallization rates, as evidenced by non-overlapping or slightly overlapping endothermic and exothermic peaks in their differential scanning calorimetry characteristics for scan rates of on the order of 10° C. to 20° C.Type: GrantFiled: October 24, 2002Date of Patent: October 17, 2006Assignee: 3D Systems, Inc.Inventors: Elmer Douglas Dickens, Jr., Biing-Lin Lee, Glenn Alfred Taylor, Angelo Joseph Magistro, Hendra Ng, Kevin P. McAlea, Paul F. Forderhase