公开(公告)号：US10407551B2

公开(公告)日：2019-09-10

申请号：US15872210

申请日：2018-01-16

申请人： Kureha Corporation

发明人： Kenji Suzuki ,  Michihisa Miyahara ,  Hiroshi Sakabe

IPC分类号： C08G75/0209 ,  C08G75/0254 ,  C08G75/0259 ,  C08F28/04 ,  C08F2/06 ,  C08F6/12 ,  C08G75/0281

摘要： To provide a polyarylene sulfide (hereinafter, PAS) manufacturing method and PAS manufacturing device that further eliminates processing costs in manufacturing PAS, by recovering from solid content containing an unreacted sulfur source and alkali metal halide produced as a byproduct the sulfur source and the solid content with a reduced amount of the sulfur source, and then conveniently and easily reusing the unreacted sulfur source without performing a large-scale process. A method of manufacturing PAS according to the present invention comprises: a polymerizing step of producing PAS; an extracting step of bringing an extraction solvent into content with solid content produced in the polymerizing step, and extracting at least a portion of a sulfur source from the solid content; a recovering step of separating and recovering the solid content passing through the extracting step and an extraction liquid produced in the extracting step; and a recycling step of supplying at least a portion of the extraction liquid preferably as at least a portion of PAS produced raw material in the polymerizing step; where the extraction solvent is (1) a protic organic solvent or (2) a mixed solvent containing water and an organic solvent, and the amount of the sulfur source in the solid content recovered in the recovering step is 2 parts by mass or less with regard to 100 parts by mass of the alkali metal halide.

公开(公告)号：US10196486B2

公开(公告)日：2019-02-05

申请号：US15327472

申请日：2015-08-03

申请人： Kureha Corporation

发明人： Michihisa Miyahara ,  Hirohito Kawama ,  Koichi Suzuki

IPC分类号： C08G75/02 ,  C08G75/0204 ,  C08G75/0254 ,  C08G75/14

摘要： The present invention is a production method for producing polyarylene sulfide, wherein an unreacted dihalo aromatic compound is recovered and reused. The present production method includes: (a) a polymerization step; (b) a separation step; and (c) a recovery step of recovering unreacted dihalo aromatic compound from a water-containing mixture of the separated liquid by steam distillation entailing adjusting the reflux ratio of water in the steam distillation column without adding water other than the refluxed water. Alternatively, the production method includes: (a) a polymerization step; (d) a dehydration step; and (c) a recovery step of recovering unreacted dihalo aromatic compound from a water-containing mixture of a water-containing liquid mixture and/or a water-containing steam mixture containing a raw material mixture and/or a polymerization reaction solution by steam distillation entailing adjusting the reflux ratio of water in the steam distillation column without adding water other than the refluxed water in the dehydration step.

公开(公告)号：US20180044483A1

公开(公告)日：2018-02-15

申请号：US15716625

申请日：2017-09-27

申请人： SEOUL NATIONAL UNIVERSITY R&DB FOUNDATION

发明人： Kookheon CHAR ,  Jeewoo LIM ,  Unho JUNG ,  Won Tae JOE

IPC分类号： C08J3/09 ,  C08G75/0254 ,  C08J3/12

CPC分类号： C08J3/097 ,  C08G75/0254 ,  C08J3/096 ,  C08J3/12 ,  C08J2381/02 ,  C08L81/02

摘要： The present disclosure relates to a polysulfide copolymer particle and a method of preparing the polysulfide copolymer particle.

公开(公告)号：US20170158820A1

公开(公告)日：2017-06-08

申请号：US15327472

申请日：2015-08-03

申请人： Kureha Corporation

发明人： MICHIHISA MIYAHARA ,  HIROHITO KAWAMA ,  KOICHI SUZUKI

IPC分类号： C08G75/0254 ,  C08G75/0204

CPC分类号： C08G75/0254 ,  C08G75/02 ,  C08G75/0204

摘要： The present invention is a production method for producing polyarylene sulfide, wherein an unreacted dihalo aromatic compound is recovered and reused.The present invention is a production method for producing polyarylene sulfide, the method include: (a) a polymerization step; (b) a separation step; and (c) a recovery step of recovering an unreacted dihalo aromatic compound from a water-containing mixture in the form of a water-containing liquid mixture containing the separated liquid by steam distillation entailing adjusting the reflux ratio of water in the steam distillation column without adding water other than the refluxed water. Alternatively, the present invention is a production method for producing polyarylene sulfide, the method include: (a) a polymerization step; (d) a dehydration step; and (c) a recovery step of recovering an unreacted dihalo aromatic compound from a water-containing mixture in the form of a water-containing liquid mixture and/or a water-containing steam mixture containing a raw material mixture and/or a polymerization reaction solution by steam distillation entailing adjusting the reflux ratio of water in the steam distillation column without adding water other than the refluxed water in the dehydration step.

公开(公告)号：US20170137573A1

公开(公告)日：2017-05-18

申请号：US15300404

申请日：2015-03-27

申请人： Kureha Corporation

发明人： Kenji SUZUKI ,  Ken-Ichi TAKAKI ,  Yasuhiro SUZUKI

IPC分类号： C08G75/0259 ,  C08G75/0213 ,  C08G75/0254

CPC分类号： C08G75/0259 ,  C08G75/02 ,  C08G75/0213 ,  C08G75/0254

摘要： Provided is a method of producing polyarylene sulfide (PAS) that suppresses side reactions and produces PAS with a high purity and a high molecular weight at a high yield.A method of producing PAS in which a sulfur source and a dihalo aromatic compound are polymerized in an organic amide solvent, the method of producing PAS comprising the following steps 1 to 3: step 1: a preparation step of preparing a mixture containing an organic amide solvent, a sulfur source, water, a dihalo aromatic compound, and an alkali metal hydroxide in an amount that is less than an equimolar amount relative to the sulfur source; step 2: a first-stage polymerization step of initiating a polymerization reaction by heating the mixture, and producing a prepolymer having a dihalo aromatic compound conversion rate of 50% or greater; and step 3: a second-stage polymerization step of adding from 0.11 to 0.3 mol of an alkali metal hydroxide per 1 mol of the sulfur source, and continuing the polymerization reaction. A PAS polymerization reaction solution having a low content of byproduct.PAS having an average particle diameter of 10 to 5,000 a melt viscosity (temperature 310° C., shear rate 1,216 sec−1) of 0.1 to 3,000 Pa·s, and a nitrogen content of 750 ppm or less.

公开(公告)号：US5237046A

公开(公告)日：1993-08-17

申请号：US844211

申请日：1992-03-02

申请人： Manfred Schmidt ,  Gabriel Denecker ,  Wolfgang Jakob ,  Wolfgang Arlt

发明人： Manfred Schmidt ,  Gabriel Denecker ,  Wolfgang Jakob ,  Wolfgang Arlt

IPC分类号： C08G75/0254 ,  C08G75/0259 ,  C08G75/06

CPC分类号： C08G75/0254 ,  C08G75/0259

摘要： The invention relates to a process for stabilizing the molecular weight of high molecular weight, optionally branched polyarylene sulfides prepared by reaction of aromatic dihalogen compounds and, optionally, aromatic trihalogen or tetrahalogen compounds and, optionally, polymer-chain-terminating monomers with alkali metal sulfides and/or alkali metal hydrogen sulfides at elevated temperature in aprotic polar solvents, characterized in that, after the desired molecular weight has been reached, alkali metal sulfides and/or alkali metal hydrogen sulfides present in excess are at least partly reacted with acids to form the alkali metal salts of the acids and hydrogen sulfide.

摘要翻译： 本发明涉及通过芳族二卤化合物和任选的芳族三卤素或四卤素化合物和任选的聚合物链终止单体与碱金属硫化物的反应制备的高分子量，任选支化的聚亚芳基硫化物的分子量的稳定化方法 和/或碱金属氢硫化物在高温下在非质子极性溶剂中，其特征在于，在达到所需分子量之后，过量存在的碱金属硫化物和/或碱金属硫化氢至少部分地与酸反应形成 酸和硫化氢的碱金属盐。