Inorganic Sulfur Reactant Contains At Least One Metal Atom Or Contains An Ammonium Ion Patents (Class 528/388)
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Patent number: 5032674Abstract: The invention relates to molding compounds of polyarylene sulfides (PAS), preferably polyphenylene sulfides (PPS), which have a low ion content and delayed crystallization and to their use as an encapsulating compound for active and passive electronic components.Type: GrantFiled: December 4, 1990Date of Patent: July 16, 1991Assignee: Bayer AktiengesellschaftInventors: Karl-Heinz Kohler, Klaus Reinking, Klaus Kraft
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Patent number: 5030672Abstract: An asymmetric membrane formed from a sulphonated polyarylethersulphone has a salt rejection of at least 99%. Alternatively, a membrane has a good salt rejection and an acceptable water flux such that the ratio ##EQU1## has the value of at least 0.7. The membranes can be obtained using barium salts of the sulphonated polyarylethersulphone, with the proportion of barium being controlled to be at least 85%, preferably at least 86%, and not more than 91%, preferably not more than 90% of the barium required to react with the sulphonic acid groups on the sulphonated polymer.Type: GrantFiled: October 1, 1990Date of Patent: July 9, 1991Assignee: Imperial Chemical Industries PLCInventors: Richard A. Hann, David R. Holmes, John W. Smith
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Patent number: 5026824Abstract: A process for preparing a polymer having repeating units corresponding to the structure ##STR1## wherein R is ##STR2## y is in the range of 0.005 to 0.10, x is in the range of 0.01 to 0.50 when R is ##STR3## x is in the range of 0.01 to 0.30 when R is ##STR4## and n is at least 200. The polymer is prepared by reacting a diiodoaromatic compound and elemental sulfur.Type: GrantFiled: May 14, 1990Date of Patent: June 25, 1991Assignee: Eastman Kodak CompanyInventors: Mark Rule, Jerry S. Fauver, David R. Fagerburg, Paul B. Lawrence, Joseph J. Watkins
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Patent number: 5023315Abstract: A process for preparing arylene sulfide polymers which comprises the steps of contacting at least one alkali metal hydroxide, water and at least one lactam to form a first mixture comprising an alkali metal aminoalkanoate, water and lactam, and subsequently contacting said first mixture with at least one sulfur source selected from the group consisting of alkali metal bisulfides, thiolactams, and hydrogen sulfide under reaction conditions of time and temperature sufficient to produce a second mixture comprising a polymerizable complex of an alkali metal aminolkanoate and the sulfur source, lactam, water and metal impurities; separating at least a portion of the metal impurities from the second mixture to form a third mixture; contacting at least one dihaloaromatic compound with the third mixture to produce a polymerization mixture; subjecting the polymerization mixture to polymerization conditions of time and temperature sufficient to produce the arylene sulfide polymer; and recovering the arylene sulfide polType: GrantFiled: April 18, 1990Date of Patent: June 11, 1991Assignees: Phillips Peteroleum Company, Lacey E. ScogginsInventor: Joseph G. Ceurvorst
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Patent number: 5017682Abstract: The invention relates to a process for the production of linear, unbranched polyarylene sulfides from aromatic dichlorine compounds and alkali sulfides in tetra-alkylated, cyclic ureas as the reaction medium.Type: GrantFiled: August 14, 1989Date of Patent: May 21, 1991Assignee: Bayer AktiengesellschaftInventors: Burkhard Kohler, Rolf-Volker Meyer, Ernst-Ulrich Dorf, Wolfgang Russeler, Manfred Schmidt
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Patent number: 5015725Abstract: A process is provided for the production of aromatic sulfide/sulfone polymers which comprises contacting under suitable polymerization reaction conditions: (1) at least one dihaloaromatic sulfone, (2) water, and (3) a complex comprising at least one alkali metal hydrosulfide.Type: GrantFiled: August 31, 1989Date of Patent: May 14, 1991Assignee: Phillips Petroleum CompanyInventors: Lacey E. Scoggins, Kenneth C. Hoover, Wei-Teh Wade Shang
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Patent number: 5013822Abstract: A process for preparing poly(arylene sulfide sulfone) by contacting a dihaloaromatic sulfone, an organic amide, a sulfur-containing compound, water, and an alkali metal carboxylate, wherein the alkali metal carboxylate is prepared in-situ by contacting at least one carboxylic acid with at least one alkali metal hydroxide.Type: GrantFiled: December 7, 1989Date of Patent: May 7, 1991Assignee: Phillips Petroleum CompanyInventor: Charles A. Drake
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Patent number: 5013823Abstract: A poly(arylene sulfide) sheet excellent in planarity and smoothness is formed of a poly(arylene sulfide) having a melt viscosity, .eta.* of 1,000-25,000 poises as measured at 310.degree. C. and a shear rate of 200 sec.sup.-1, and a melt crystallization temperature, Tc.sub.2 or 170.degree.-240.degree. C., wherein Tc.sub.2 is an exothermic peak temperature of crystallization which appears upon the measurement by a differential scanning calorimeter at a cooling rate of 10.degree. C./min after the polymer is heated from 23.degree. C. to 380.degree. C. at a rate of 10.degree. C./min and then held for 3 minutes at 380.degree. C. It has a surface roughness, Ra of 0.09 .mu.m or less on at least one side thereof and a degree of crystallization of at least 5%. Its number of flexings to break, Y satisfies the following equation (I):log Y.gtoreq.7.11-2.34log t (I)wherein t means a thickness (.mu.m) of the sheet.Type: GrantFiled: November 28, 1989Date of Patent: May 7, 1991Assignee: Kureha Kagaku Kogyo K.K.Inventors: Toshiya Mizuno, Yoshikichi Teramoto, Juichi Wakabayashi, Takeshi Saito
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Patent number: 5010169Abstract: This invention relates to new straight chained and branched copolyarylene sulphides with built-in aromatic or araliphatic comonomers containing phosphine groups and to products obtainable from the phosphine group-containing polyarylene sulphides by a special heat treatment.Type: GrantFiled: November 13, 1989Date of Patent: April 23, 1991Assignee: Bayer AktiengesellschaftInventors: Burkhard Kohler, Rolf-Volker Meyer
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Patent number: 5008370Abstract: Disclosed herein is a process for the preparation of a poly(arylene thioether-ketone) improved in melt stability, which comprises subjecting a poly(arylene thioether-ketone) (PTK) to a heat treatment for 5-5.times.10.sup.3 minutes in a powdery state and a temperature range of 200.degree.-350.degree. C. The PTK has predominant recurring units of the formula ##STR1## and has a melting point, Tm of 310.degree.-380.degree. C., a melt crystallization temperature, Tmc (420.degree. C./10 min) of at least 210.degree. C., a residual melt crystallization enthalpy, .DELTA.Hmc (420.degree. C./10 min) of at least 10 J/g and a reduced viscosity of 0.2-2.0 dl/g. PTKs improved in melt stability and prepared in accordance with the above-described preparation process are also disclosed.Type: GrantFiled: November 3, 1989Date of Patent: April 16, 1991Assignee: Kureha Kagaku Kogyo K.K.Inventors: Ken Kashiwadate, Yoshikatsu Satake, Takashi Kaneko, Masahiro Tada, Takayuki Katto
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Patent number: 5008369Abstract: In a preferred embodiment, poly(4-phenylsulfone) is prepared by self-condensation of sodium 4-fluorophenyl sulfinate. The process is initiated by a small quantity of 4,4'-difluorophenylsulfone. The process is conducted in the presence of a dipolar, aprotic solvent such as dimethylsulfoxide. The reaction is conducted at a mildly elevated temperature, preferably within the range of from about 100.degree. C. to about 200.degree. C.Type: GrantFiled: November 1, 1989Date of Patent: April 16, 1991Assignee: Eastman Kodak CompanyInventors: Douglas R. Robello, Abraham Ulman
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Patent number: 5008368Abstract: A method for producing a poly(arylene sulfide/sulfone) polymer is provided which comprises: contacting reactants comprising a dihalogenated aromatic sulfone, an alkali metal sulfide, a polar organic compound, at least one base, an alkali metal carboxylate, and, optionally water, under suitable conditions to initiate a polymerization reaction; thereafter adding an amount of water while maintaining polymerization conditions; then terminating the reaction; and recovering the polymer.The invention method provides for a polymer product wherein the production of low molecular weight product is minimized and high molecular weight yield is maximized.Type: GrantFiled: August 3, 1989Date of Patent: April 16, 1991Assignee: Phillips Petroleum CompanyInventor: Afif M. Nesheiwat
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Patent number: 5003042Abstract: A process is provided for preparing a polymeric resin comprising the steps of: (a) preparing a first slurry, wherein the solid component thereof comprises a first particulate resin selected from the group consisting of poly(arlene sulfide ketone)s and poly(arylene sulfide diketone)s, and wherein the liquid component thereof comprises a polar organic compound; (b) substantially liquifying the first particulate resin to form a mixture comprising the substantially liquified first particulate resin and the polar organic compound; and (c) reducing the temperature of the mixture sufficiently to solidify the substantailly liquified resin and form a second slurry, wherein the solid component thereof comprises a second polymeric resin. The filterability of the slurry containing the second polymeric resin is superior to that of the first slurry.Type: GrantFiled: December 29, 1989Date of Patent: March 26, 1991Assignee: Phillips Petroleum CompanyInventor: Afif M. Nesheiwat
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Patent number: 5003033Abstract: A process for preparing a branched, high molecular weight poly(arylene sulfide ketone) by the addition of a polyhaloaromatic compound to a reaction mixture containing a dihaloaromatic ketone, an organic amide, an alkali metal sulfide, and water, and the product produced therefrom.Type: GrantFiled: April 6, 1990Date of Patent: March 26, 1991Assignee: Phillips Petroleum CompanyInventors: Jon F. Geibel, Lacey E. Scoggins, Michael D. Cliffton
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Patent number: 5001220Abstract: This invention relates to new high molecular weight, optionally branched co-polyarylene sulphides prepared by the reaction of halogenated aromatic compounds and dihalogenated phenyl-pyrazole-3-ones in a polar solvent with the addition of 0.2 to 100 mol %, based on the dihalogenated aromatic compound, of an amino acid to the reaction mixture, and to the use of these copolyarylene sulphides as embedding compounds for electronic parts.Type: GrantFiled: March 3, 1989Date of Patent: March 19, 1991Assignee: Bayer AGInventors: Karl-Heinz Kohler, Klaus Reinking
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Patent number: 4988796Abstract: A process for preparing poly(arylene sulfide sulfone) by contacting a dihaloaromatic sulfone, an organic amide, a sulfur-containing compound selected from the group consisting of alkali metal bisulfides, hydrogen sulfide and N-methyl-2-pyrrolidinethione, water, and an alkali metal carboxylate.Type: GrantFiled: February 20, 1990Date of Patent: January 29, 1991Assignee: Phillips Petroleum CompanyInventors: Michael D. Cliffton, Jon F. Geibel
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Patent number: 4983692Abstract: Novel epoxy resins are prepared by dehydrohalogenating the reaction product of an epihalohydrin and a hydroxyalkyl containing polysulfide.Type: GrantFiled: December 12, 1989Date of Patent: January 8, 1991Assignee: The Dow Chemical CompanyInventors: Robert E. Hefner, Jr., Paul L. Wykowski
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Patent number: 4978729Abstract: The invention relates to high molecular weight polyarylene sulfides (PAS), preferably polyphenylene sulfides (PPS), produced from polyarylene sulfides, preferably polyphenylene sulfide and aromatic dihalogen compounds.Type: GrantFiled: August 7, 1989Date of Patent: December 18, 1990Assignee: Bayer AktiengesellschaftInventors: Burkhard Kohler, Hans-Detlef Heinz
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Patent number: 4976825Abstract: A process for recovering N-methylpyrrolidone contained in an N-methylpyrrolidone-containing liquid formed in the process for preparing a polyarylene thioether by the dehalogenosulfidation of a dihalogeno-aromatic compound and an alkali metal sulfide in the presence of N-methylpyrrolidone as the polymerization solvent, which comprises (a) subjecting the N-methylpyrrolidone-containing liquid to distillation to distill and recover the majority of contained N-methylpyrrolidone while recovering a distillation residue having such a flowability that flow transferring of the distillation residue is possible, and (b) supplying the distillation residue to an air-tight mixer for a highly-viscous fluid, which has a vent and is provided with a heater, to treat the distillation residue under the conditions of a temperature in the mixer of 190.degree. to 310.degree. C.Type: GrantFiled: June 23, 1989Date of Patent: December 11, 1990Assignee: Kureha Kagaku Kogyo Kabushiki KaishaInventors: Takao Iwasaki, Katsumi Horikoshi, Yuzo Yoshiji
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Patent number: 4973663Abstract: A novel thermoplastic poly(arylene thioether) copolymer which may be cross-linked is provided. The copolymer may be prepared by reacting a dihalogenobenzonitrile, a dihalogenophenyl sulfone and a thioetherifying agent in a suitable organic solvent.Type: GrantFiled: April 14, 1989Date of Patent: November 27, 1990Assignee: Tosoh CorporationInventors: Tomoji Tamai, Tetsuya Asahi, Yozo Kondo
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Patent number: 4968761Abstract: The invention relates to high-molecular polyarylene sulphides (PAS) and a process for producing them.Type: GrantFiled: April 12, 1989Date of Patent: November 6, 1990Assignee: Bayer AktiengesellschaftInventors: Burkhard Kohler, Rolf-Volker Meyer, Hans-Detlef Heinz, Hans-Joachim Traenckner
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Patent number: 4963651Abstract: A method is provided for recovering poly(arylene sulfide) from a liquid reaction mixture, comprising a liquid-phase poly(arylene sulfide) and a polar organic compound which can also function as a solvent for the polymer, and water. The liquid reaction mixture is contacted by an amount of a vaporized phase separation agent at least sufficient to effect or enhance a phase separation of the liquid-phase poly(arylene sulfide) component from the polar organic compound. The poly(arylene sulfide resins recovered according to this invention exhibit greater particle size than those recovered according to prior art methods, and do not tend to adhere to vessel walls during recovery.Type: GrantFiled: May 8, 1989Date of Patent: October 16, 1990Assignee: Phillips Petroleum CompanyInventor: Afif M. Nesheiwat
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Patent number: 4960841Abstract: A process for producing a block copolymer composed of polyphenylene sulfide segments and polyphenylene sulfide sulfone segments comprises reacting a polyphenylene sulfide prepolymer with a mixture of a dihalodiphenyl sulfone and a sulfidization agent, or a polyphenylene sulfide sulfone prepolymer with a mixture of a polyhalogenated aromatic compound and a sulfidization agent.Type: GrantFiled: December 30, 1988Date of Patent: October 2, 1990Assignee: Dainippon Ink and Chemicals, Inc.Inventors: Juheiji Kawabata, Manabu Chiba, Toshinori Sugie, Fumihiro Kobata, Hitoshi Izutsu, Toshio Inoue, Takayuki Mine
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Patent number: 4960861Abstract: A process for producing a polyarylene sulfide polymer, which comprises reacting a polyhaloaromatic compound and a sulfidizing agent in a polar amide solvent in the presence of at least one polymerization additive to form a resinuous liquid consisting of a layer (I) containing a major amount of a polymer having a relatively high molecular weight and a minor amount of a polymer having a relatively low molecular weight and a layer (II) containing a major amount of a polymer having a relatively low molecular weight and a minor amount of a polymer having a relatively high molecular weight, and thereafter fractionating the layer (I) or layer (II) from the resinous liquid.Type: GrantFiled: June 27, 1988Date of Patent: October 2, 1990Assignee: Dainippon Ink and Chemicals, Inc.Inventors: Kohichi Kotera, Toshinori Sugie, Fumihiro Kobata, Juheiji Kawabata, Sugio Hasegawa
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Patent number: 4958003Abstract: A class of amide group-containing aromatic dihalide compounds are sulfidized together with a class of aromatic dihalide compounds to provide a novel class of aromatic sulfideamide polymers increased in crystalline melting point (T.sub.m). The polymers exhibit excellent resistance to high temperatures, resistance to solvents, flame-retardant properties and improved mechanical properties.Type: GrantFiled: December 23, 1988Date of Patent: September 18, 1990Assignee: Tosoh CorporationInventors: Satoshi Tomagou, Toshikazu Kato, Hiroshi Inoue, Kensuke Ogawara
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Patent number: 4958004Abstract: A process is provided for the production of aromatic sulfide/sulfone polymers which involves contacting under suitable polymerization reaction conditions: (1) at least one dihaloaromatic sulfone, (2) at least one organic amide, (3) at least one alkali metal hydrosulfide, (4) water, and (5) at least one member selected from the group consisting of (a) alkali metal carbonates and (b) mixtures of alkali metal carbonates with alkali metal hydroxides wherein said mixtures have at least about 0.5 mole percent alkali metal carbonate.Type: GrantFiled: July 31, 1987Date of Patent: September 18, 1990Assignee: Phillips Petroleum CompanyInventors: Kenneth C. Hoover, Lacey E. Scoggins, Wei-Tech W. Shang, Afif M. Nesheiwat
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Patent number: 4954554Abstract: Aqueous emulsions of curable silicone compositions provide cured coatings having improved gloss and/or water-repellancy and/or adhesive release if formulated to contain polyvinylachohol having a degree of hydrolysis of 90 mol % or more. The extent of improvement is directly related to the degree of hydrolysis of the PVA. PVA having an average degree of hydrolysis of from 94 to 99 mol % is particularly effective for improving these properties of cured coatings. Conveniently, a mixture of two or more commercially available PVAs having different degrees of hydrolysis can be used to arrive at a PVA having a desired degree of hydrolysis.Type: GrantFiled: February 27, 1989Date of Patent: September 4, 1990Assignee: Dow Corning CorporationInventor: David J. Bunge
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Patent number: 4952671Abstract: A copoly(arylene sulfide) corresponding to the structure ##STR1## wherein A is a divalent substituted or unsubstituted aromatic radical, T is a monovalent aromatic radical, x is n the range of 0.5 t 0.001 and n is at least 100.Type: GrantFiled: July 15, 1988Date of Patent: August 28, 1990Assignee: Eastman Kodak CompanyInventors: David R. Fagerburg, Joseph J. Watkins, Paul B. Lawrence, Mark Rule
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Patent number: 4945155Abstract: A process comprising heating for a sufficient period of time and at a temperature in the range of the glass transition temperature of the polymer to 5 degrees C below the melting point of the polymer, a solid, comminuted, copoly(arylene sulfide) prepared by reacting at a polymer producing temperature a mixture of a diiodoaromatic compound and elemental sulfur which contains less than 0.05 weight percent carbon, the copoly(arylene sulfide) corresponding to the structure[(--A--S--).sub.1--x (--A--S--S--).sub.x ].sub.nwherein A is a divalent substituted or unsubstituted aromatic radical, x is in the range of 0.2 to 0.005 and n is at least 100.Type: GrantFiled: May 11, 1989Date of Patent: July 31, 1990Assignee: Eastman Kodak CompanyInventors: David R. Fagerburg, Mark Rule, Joseph J. Watkins, Paul B. Lawrence
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Patent number: 4939236Abstract: A process for preparing a copoly(arylene sulfide) corresponding to the structure[(--A--S--).sub.1-x (--A--S--S--).sub.x ].sbsb.nwherein x is in the range of 0.5 to 0.001 by reacting a mixture of a diiodoaromatic compound and elemental sulfur which contains less than 0.05 weight percent carbon.Type: GrantFiled: September 8, 1989Date of Patent: July 3, 1990Assignee: Eastman Kodak CompanyInventors: David R. Fagerburg, Joseph J. Watkins, Paul B. Lawrence, Mark Rule
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Patent number: 4935473Abstract: The present invention discloses a composition comprising a mixture containing 100 parts by weight of substantially linear polyphenylene sulfide which is treated with an aqueous solution of an acid or a salt of a strong acid and a weak base and which has not less than 70 mol % of a repeating unit of ##STR1## 0.05 to 5 parts by weight of at least one aminoalkoxysilane compound and, if necessary, 0.01 to 3 parts by weight of a releasing agent, the mixture being kneaded under heating at a temperature higher than the melting point of the polyphenylene sulfide, said composition exhibiting excellent impact strength and weld strength and providing molded product with small amount of flash generated during molding. The invention also discloses a composition which further comprises a fibrous reinforcing material and/or an inorganic powdered or granular filler, according to necessity, as well as disclosing a method of producing said composition.Type: GrantFiled: December 2, 1988Date of Patent: June 19, 1990Assignees: Kureha Kagaku Kogyo Kabushiki Kaisha, Polyplastics Co., Ltd.Inventors: Makoto Fukuda, Yukio Ichikawa, Takayuki Katto, Toshikatsu Nitoh
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Patent number: 4931516Abstract: Disclosed herein is a process for producing a medium- or high-molecular-weight polyarylene sulfide which comprises subjecting an alkali metal sulfide, a dihalo aromatic compound and optionally, small amount of tri- or higher polyhalo aromatic compound to dehalogenation and sulfidation reaction at a temperature of from 240.degree. to 270.degree. C. in the presence of a water in amount of from 0.5 to 5 mol per 1 kg of an aprotic organic polar solvent until the conversion of said dihalo aromatic compound reaches from 70 to 98 mol %, thereby forming a polyarylene sulfide prepolymer having a melt viscosity of from 5 to 300 poise (as measured at 310.degree. C. under a shear rate of 200 sec.sup.-1), adding water to the resultant reaction mixture containing the polyarylene sulfide prepolymer so that from 6 to 15 mol of water is present per 1 kg of said solvent, and then continuing the reaction at a temperature of from 240.degree.-290.degree. C.Type: GrantFiled: January 24, 1989Date of Patent: June 5, 1990Assignee: Kureha Kagaku Kogyo Kabushiki KaishaInventors: Yo Iizuka, Takao Iwasaki, Takayuki Katto, Zenya Shiiki
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Patent number: 4923971Abstract: Improved, stronger poly(arylene sulfide) fibers can be produced by treatment of a crystallizable poly(arylene sulfide) fiber with an organic halide, either before or after annealing. Physical properties, such as density and abrasion resistance, can be increased after said treatment.Type: GrantFiled: November 17, 1988Date of Patent: May 8, 1990Assignee: Phillips Petroleum CompanyInventor: Bruce L. Ramsey
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Patent number: 4921935Abstract: This invention relates to a process for the preparation of polyarylene sulphides, preferably polyphenylene sulphide (PPS), whose fusion viscosities can be adjusted to specified values, from alkali metal sulphides and polyhalogenated aromatic compounds in a polar solvent in the presence of a ketone or pinacone. The resulting polyarylene sulphides which have specified fusion viscosities are distinguished by high stability of the melt and low chlorine content. They cause little corrosion in the reaction vessels used for their preparation.Type: GrantFiled: November 3, 1988Date of Patent: May 1, 1990Assignee: Bayer AktiengesellschaftInventors: Ernst-Ulrich Dorf, Franz Alfes, Hans-Joachim Traenckner
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Patent number: 4921758Abstract: The present invention discloses a molded product which is heat-resistant, has a high elongation and is produced by a process including the steps of (1) curing a substantially linear polyarylene thioether having a melt viscosity of about 1,000 to 15,000 poise, thereby forming a polyarylene thioether resin having a melt viscosity of about 5,000 to 16,000 poise and a non-Newtonian coefficient, n, of about 1.5 to 2.1, (2) melt extruding the formed polyarylene thioether resin, (3) taking off the extruded polyarylene thioether resin at an R.sub.1 (ratio of the taking-off speed to the extruding speed at the nozzle of the melt extruded product) of about 10 to 1,000 and (4) crystallizing the taken off polyarylene thioether resin until its crystallization degree is not lower than 20 wt %; and coated electric wires having the above molded product as a coating layer.Type: GrantFiled: January 5, 1988Date of Patent: May 1, 1990Assignee: Kureha Kagaku Kogyo Kabushiki KaishaInventors: Kiyoshi Tagaya, Satoshi Hirose, Takao Iwasaki, Toshitaka Kouyama, Yasuo Sakaguchi
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Patent number: 4920193Abstract: An asymmetric membrane formed from a sulphonated polyarylethersulphone has a salt rejection of at least 99%. Alternatively, a membrane has a good salt rejection and an acceptable water flux such that the ratio ##EQU1## has the value of at least 0.7. The membranes can be obtained using barium salts of the sulphonated polyarylethersulphone, with the proportion of barium being controlled to be at least 85%, preferably at least 86%, and not more than 91%, preferably not more than 90% of the barium required to react with the sulphonic acid groups on the sulphonated polymer.Type: GrantFiled: July 19, 1988Date of Patent: April 24, 1990Assignee: Imperial Chemical Industries PLCInventors: Richard A. Hann, David R. Holmes, John W. Smith
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Patent number: 4919911Abstract: The present invention provides a method of recovering a lithium chloride, which comprises reacting a dihalogenated aromatic compound and an alkali metal sulfide and/or alkali metal hydrogen sulfide in a polar solvent under the pressure of lithium chloride, separating a solvent insoluble component from the resultant reaction mixture to obtain a solution, and calcinating a residue obtained by removing volatile substances from the resultant solution, as well as a method of recovering a lithium chloride, which comprises reacting a dihalogenated aromatic compound and an alkali metal sulfide and/or alkali metal hydrogen sulfide in a polar solvent under the pressure of lithium chloride, separating the granular polymer ingredient from the resultant reaction mixture subjecting the liquid suspension obtained by said separation to solid-liquid separation and calcinating the residue obtained by removing volatile substances from the resultant solution component.Type: GrantFiled: December 16, 1988Date of Patent: April 24, 1990Assignee: Idemitsu Petrochemical Company LimitedInventors: Daigo Shirota, Masao Omori, Hiroyasu Yamato, Norio Ogata
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Patent number: 4920201Abstract: This invention relates to a process for the preparation of crystalline polyarylenesulphides. Polyarylenesulphides with a high degree of purity, low electrolyte content and low non-uniformity are obtained. The polyarylenesulphides obtained have improved mechanical and electrical properties.Type: GrantFiled: August 18, 1988Date of Patent: April 24, 1990Assignee: Bayer AktiengesellschaftInventors: Wolfgang Jakob, Erhard Tresper, Wolfgang Alewelt
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Patent number: 4912180Abstract: This invention relates to a process for the preparation of polyarylene sulphides by melt condensation, in which the sulphide bridges of the polymer are formed by the splitting off of a compound which is volatile under the reaction conditions.Type: GrantFiled: November 3, 1988Date of Patent: March 27, 1990Assignee: Bayer AktiengesellschaftInventors: Ernst-Ulrich Dorf, Hans-Rudolph Dicke, Volker Eckhardt, Joachim Genz
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Patent number: 4910294Abstract: Disclosed is a process for producing stably a polyarylene sulfide of high purity and high molecular weight by contacting a dihalogeno aromatic compound with an alkali metal sulfide in a polar solvent which comprises, as a first stage, reacting a dihalogeno aromatic compound with an alkali metal sulfide in a polar solvent in the presence of a lithium compound and in the presence of substantially no water at 200.degree.-270.degree. C. with concentration of remaining alkali metal sulfide being 5.5 g/l-polar solvent or less in terms of sulfur; then adding water in an amount of 1.0-10 mols per 1 mol of said alkali metal sulfide; and, thereafter, as a second stage, carrying out the reaction at 220.degree.-280.degree. C. Preferred dihalogeno aromatic compound is p-dichlorobenzene, preferred alkali metal sulfide is sodium sulfide and/or lithium sulfide and preferred lithium compound is lithium chloride and/or lithium sulfide.Type: GrantFiled: June 20, 1988Date of Patent: March 20, 1990Assignee: Idemitsu Petrochemical Company LimitedInventors: Norio Ogata, Hiroyasu Yamato
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Patent number: 4906712Abstract: This invention relates to a process for the preparation of polyarylene sulphides by melt condensation, in which the sulphide bridges of the polymer are formed by the splitting off of a compound which is volatile under the reaction conditions.Type: GrantFiled: November 8, 1988Date of Patent: March 6, 1990Assignee: Bayer AktiengesellschaftInventors: Ernst-Ulrich Dorf, Hans-Rudolph Dicke, Wolfgang Russeler, Volker Eckhardt, Joachim Genz
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Patent number: 4902730Abstract: Improved fiber reinforcement of polyarylene sulphides is achieved by preparing the polyarylene sulphides in the presence of reinforcing fibers pretreated with arylsulphonic acid chlorides at elevated temperatures.Type: GrantFiled: August 15, 1988Date of Patent: February 20, 1990Assignee: Bayer AktiengesellschaftInventors: Karl-Heinz Reichert, Ingo Koschinski
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Patent number: 4900808Abstract: The invention relates to a process for the production of high molecular weight, optionally branched polyarylene sulfides from alkali sulfides and aromatic dihalogen compounds, in which the reaction is carried out in a polar solvent, such as an N-alkyl lactam, containing from 0.5 to 100 mole %, based on the moles of aromatic dihalogen compound, of a lactam.Type: GrantFiled: November 20, 1986Date of Patent: February 13, 1990Assignee: Bayer AktiengesellschaftInventors: Karsten Idel, Edgar Ostlinning, Dieter Freitag
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Patent number: 4895930Abstract: The invention relates to a process for purifying and isolating polyarylene sulphides. In this process polyarylene sulphides are obtained with a particularly low electrolyte content.Type: GrantFiled: June 30, 1988Date of Patent: January 23, 1990Assignee: Bayer AktiengesellschaftInventors: Franz Alfes, Wolfgang Alewelt, Wolfgang Eisermann, Erhard Tresper
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Patent number: 4894434Abstract: A highly heat resistant polymer, polycyanoaryl thioether, of formula: ##STR1## where n is a number of not less than 3 is disclosed. A process for preparing the novel polymer is also disclosed.Type: GrantFiled: May 19, 1988Date of Patent: January 16, 1990Assignee: Tosoh CorporationInventors: Tetsuya Asahi, Yozo Kondo
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Patent number: 4892929Abstract: Melt stable polymeric resins are provided by process which comprises heating a first particulate resin selected from the group consisting of poly(arylene sulfide ketone) and poly(arylene sulfide diketone), while in the presence of a gaseous oxidizing atmosphere, to a temperature at least about 150.degree. C. (302.degree. F.) but below the melting point of the first particulate resins, for time sufficient to produce a second particulate resin. The thermal stability of the second particulate resin is superior to that of its respective first particulate resin is superior to that of its respective first particulate resin. Moreover, the molecular weight of the second particulate resin is greater than that of its respective first particulate resin.Type: GrantFiled: November 16, 1988Date of Patent: January 9, 1990Assignee: Phillips Petroleum CompanyInventors: Jon F. Geibel, Roger G. Gaughan, Michael D. Cliffton
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Patent number: 4892930Abstract: The melt crystallization temperature (T.sub.mc) of an arylene sulfide polymer is reduced by incorporating therein an effective amount of an organic phosphite.Type: GrantFiled: July 29, 1988Date of Patent: January 9, 1990Assignee: Phillips Petroleum CompanyInventor: Yeon F. Liang
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Patent number: 4882418Abstract: A process is provided for removing solid and liquid impurities from a particulate arylene sulfide polymer recovered from a polymerization reaction mixture slurry, without significantly discoloring the resulting washed polymer. The process of this invention comprises the steps of: (a) preparing a first slurry, wherein the solid component thereof comprises a particulate arylene sulfide polymer recovered from a reaction mixture slurry, and wherein the liquid component thereof comprises a mixture of water and a reducing agent; (b) heating the first slurry to a temperature of at least about 185.degree. C. (365.degree. F.) but below the melting point of the particulate polymer, to wash the polymer contained therein; (c) cooling the first slurry to a temperature below about 100.degree. C. (212.degree. F.), to form a second slurry, wherein the solid component thereof comprises a washed particulate arylene sulfide polymer; and (d) recovering the washed particulate arylene sulfide polymer from the second slurry.Type: GrantFiled: December 13, 1988Date of Patent: November 21, 1989Assignee: Phillips Petroleum CompanyInventors: Guy Senatore, Afif M. Nesheiwat, Fred T. Sherk
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Patent number: 4882416Abstract: Arylene sulfide polymers which can be linear, branched or modified are prepared by a process which comprises the steps of: (a) admixing a sulfur source and a cyclic organic amide in the presence of water to form an aqueous admixture wherein the molar ratio of the sulfur source to the cyclic organic amide is at least about 0.6:1 to about 1:1; (b) dehydrating said aqueous admixture to form a dehydrated admixture; (c) admixing with said dehydrated admixture at least one polymerizable halo-substituted aromatic compound to form a polymerization mixture; (d) subjecting the polymerization mixture to polymerization conditions effective to produce the arylene sulfide polymer; and (3) recovering the arylene sulfide polymer.Type: GrantFiled: June 20, 1988Date of Patent: November 21, 1989Assignee: Phillips Petroleum CompanyInventors: Guy Senatore, Wei-Teh W. Shang, Kenneth D. Goetz
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Patent number: 4880901Abstract: A process for the production of an arylene sulfide terpolymer is provided comprising reacting at least one alkali metal sulfide, at least one p-dihalo unsubstituted benzene, at least one polyhalo aromatic compound having more than two halogen substituents per molecule, at least one p-dihalo alkyl substituted benzene, and at least one N-alkyl lactam. Another process is provided comprising first reacting an at least one alkali metal sulfide in hydrated form or in an aqueous mixture with at least one N-alkyl lactam to form a reaction product, thereafter heating the reaction product to form a dehydrated composition, then reacting the dehydrated composition with a mixture consisting essentially of at least one p-dihalo unsubstituted benzene, at least one polyhalo aromatic compound having more than 2 halogen atoms per molecule, at least one p-dihalo alkyl subsituted benzene, and at least one member selected from the group consisting of (a) water in an amount of about 0.2 mole to about 2.Type: GrantFiled: May 30, 1986Date of Patent: November 14, 1989Assignee: Phillips Petroleum CompanyInventor: James W. Cleary