公开(公告)号：US07767783B2

公开(公告)日：2010-08-03

申请号：US12370201

申请日：2009-02-12

申请人： Hirohito Kawama ,  Mitsuhiro Matsuzaki ,  Michihisa Miyahara ,  Koichi Suzuki ,  Hiroyuki Sato

发明人： Hirohito Kawama ,  Mitsuhiro Matsuzaki ,  Michihisa Miyahara ,  Koichi Suzuki ,  Hiroyuki Sato

IPC分类号： C08G75/14 ,  C08G75/00 ,  C08G75/02

CPC分类号： C08G75/0259

摘要： A dehydration step is conducted by heating a mixture containing an organic amide solvent and a sulfur source including an alkali metal hydrosulfide, and a part of an overall charged amount of an alkali metal hydroxide as needed. The mixture remaining within the system after the dehydration step is mixed with a dihalo-aromatic compound, the resultant mixture is heated to conduct a polymerization reaction, and the alkali metal hydroxide is added to the mixture for polymerization reaction continuously or in portions to control the pH of the mixture for polymerization reaction within a range of from 7 to 12.5 from the beginning to the end of the polymerization reaction. The poly(arylene sulfide) according to the present invention has a nitrogen content of at most 800 ppm.

摘要翻译： 通过根据需要加热包含有机酰胺溶剂和包含碱金属氢硫化物的硫源的混合物和总量的碱金属氢氧化物的一部分来进行脱水步骤。 将脱水步骤后残留在体系内的混合物与二卤代芳族化合物混合，加热所得混合物进行聚合反应，并将碱金属氢氧化物连续地或部分加入到混合物中用于聚合反应，以控制 从聚合反应的开始到结束，聚合反应的混合物的pH在7至12.5的范围内。 本发明的聚（亚芳基硫醚）的氮含量为800ppm以下。

公开(公告)号：US07504476B2

公开(公告)日：2009-03-17

申请号：US10542543

申请日：2004-01-21

申请人： Hirohito Kawama ,  Mitsuhiro Matsuzaki ,  Michihisa Miyahara ,  Koichi Suzuki ,  Hiroyuki Sato

发明人： Hirohito Kawama ,  Mitsuhiro Matsuzaki ,  Michihisa Miyahara ,  Koichi Suzuki ,  Hiroyuki Sato

IPC分类号： C08G75/14 ,  C08G75/00 ,  C08G75/02

CPC分类号： C08G75/0259

摘要： A dehydration step is conducted by heating a mixture containing an organic amide solvent and a sulfur source including an alkali metal hydrosulfide, and a part of an overall charged amount of an alkali metal hydroxide as needed. The mixture remaining within the system after the dehydration step is mixed with a dihalo-aromatic compound, the resultant mixture is heated to conduct a polymerization reaction, and the alkali metal hydroxide is added to the mixture for polymerization reaction continuously or in portions to control the pH of the mixture for polymerization reaction within a range of from 7 to 12.5 from the beginning to the end of the polymerization reaction. The poly(arylene sulfide) according to the present invention has a nitrogen content of at most 800 ppm.

摘要翻译： 通过根据需要加热包含有机酰胺溶剂和包含碱金属氢硫化物的硫源的混合物和总量的碱金属氢氧化物的一部分来进行脱水步骤。 将脱水步骤后残留在体系内的混合物与二卤代芳族化合物混合，加热所得混合物进行聚合反应，并将碱金属氢氧化物连续地或部分加入到混合物中用于聚合反应，以控制 从聚合反应的开始到结束，聚合反应的混合物的pH在7至12.5的范围内。 本发明的聚（亚芳基硫醚）的氮含量为800ppm以下。

公开(公告)号：US20090156780A1

公开(公告)日：2009-06-18

申请号：US12370201

申请日：2009-02-12

申请人： Hirohito Kawama ,  Mitsuhiro Matsuzaki ,  Michihisa Miyahara ,  Koichi Suzuki ,  Hiroyuki Sato

发明人： Hirohito Kawama ,  Mitsuhiro Matsuzaki ,  Michihisa Miyahara ,  Koichi Suzuki ,  Hiroyuki Sato

IPC分类号： C08G75/14

CPC分类号： C08G75/0259

摘要： A dehydration step is conducted by heating a mixture containing an organic amide solvent and a sulfur source including an alkali metal hydrosulfide, and a part of an overall charged amount of an alkali metal hydroxide as needed. The mixture remaining within the system after the dehydration step is mixed with a dihalo-aromatic compound, the resultant mixture is heated to conduct a polymerization reaction, and the alkali metal hydroxide is added to the mixture for polymerization reaction continuously or in portions to control the pH of the mixture for polymerization reaction within a range of from 7 to 12.5 from the beginning to the end of the polymerization reaction. The poly(arylene sulfide) according to the present invention has a nitrogen content of at most 800 ppm.

摘要翻译： 通过根据需要加热含有有机酰胺溶剂和包含碱金属氢硫化物的硫源的混合物和总量的碱金属氢氧化物的一部分来进行脱水步骤。 将脱水步骤后残留在体系内的混合物与二卤代芳族化合物混合，加热所得混合物进行聚合反应，并将碱金属氢氧化物连续地或部分加入到混合物中用于聚合反应，以控制 从聚合反应的开始到结束，聚合反应的混合物的pH在7至12.5的范围内。 本发明的聚（亚芳基硫醚）的氮含量为800ppm以下。

公开(公告)号：US20060074219A1

公开(公告)日：2006-04-06

申请号：US10542543

申请日：2004-01-21

申请人： Hirohito Kawama ,  Mitsuhiro Matsuzaki ,  Michihisa Miyahara ,  Koichi Suzuki ,  Hiroyuki Sato

发明人： Hirohito Kawama ,  Mitsuhiro Matsuzaki ,  Michihisa Miyahara ,  Koichi Suzuki ,  Hiroyuki Sato

IPC分类号： C08G75/14

CPC分类号： C08G75/0259

摘要： A dehydration step is conducted by heating a mixture containing an organic amide solvent and a sulfur source including an alkali metal hydrosulfide, and a part of an overall charged amount of an alkali metal hydroxide as needed. The mixture remaining within the system after the dehydration step is mixed with a dihalo-aromatic compound, the resultant mixture is heated to conduct a polymerization reaction, and the alkali metal hydroxide is added to the mixture for polymerization reaction continuously or in portions to control the pH of the mixture for polymerization reaction within a range of from 7 to 12.5 from the beginning to the end of the polymerization reaction. The poly(arylene sulfide) according to the present invention has a nitrogen content of at most 800 ppm.

摘要翻译： 通过根据需要加热包含有机酰胺溶剂和包含碱金属氢硫化物的硫源的混合物和总量的碱金属氢氧化物的一部分来进行脱水步骤。 将脱水步骤后残留在体系内的混合物与二卤代芳族化合物混合，加热所得混合物进行聚合反应，并将碱金属氢氧化物连续地或部分加入到混合物中用于聚合反应，以控制 从聚合反应的开始到结束，聚合反应的混合物的pH在7至12.5的范围内。 本发明的聚（亚芳基硫醚）的氮含量为800ppm以下。

公开(公告)号：US20130068256A1

公开(公告)日：2013-03-21

申请号：US13699143

申请日：2011-04-20

申请人： Masanori Kobayashi ,  Hirohito Kawama ,  Koichi Suzuki ,  Mitsuhiro Matsuzaki

发明人： Masanori Kobayashi ,  Hirohito Kawama ,  Koichi Suzuki ,  Mitsuhiro Matsuzaki

IPC分类号： B08B3/04

CPC分类号： B08B3/041 ,  B01J8/10 ,  B01J19/0066 ,  B01J19/18 ,  B01J2219/00765 ,  B01J2219/00779 ,  C08G75/025

摘要： A longitudinal solid-liquid countercurrent contact method and apparatus are provided in which an aqueous slurry containing solid particles is supplied from an upper part and is caused to pass through a plurality of contact-processing chambers connected in a vertical direction while being caused to proceed downward, a contacting liquid is supplied from a lower part and is caused to pass through the plurality of contact-processing chambers connected in the vertical direction while being caused to proceed upward, and the aqueous slurry and the contacting liquid are caused to be continuously subjected to countercurrent contact, wherein the viscosity of a liquid phase in at least one of the contact-processing chambers is controlled, and especially the viscosity η1 of a liquid phase in a contact-processing chamber positioned at an uppermost part is controlled to fall within a range of 0.9≦η1/η0≦2.0 with respect to the reference viscosity η0 as the viscosity of a predetermined reference composition of a liquid phase at a predetermined temperature.

摘要翻译： 提供了一种纵向固液逆流接触方法和装置，其中含有固体颗粒的含水浆料从上部供应并使其通过在垂直方向上连接的多个接触处理室，同时使其向下 从下部供给接触液体，使其在垂直方向上连续通过的多个接触处理室通过，同时使上述水性浆料和接触液体连续地进行 逆流接触，其中控制至少一个接触处理室中的液相的粘度，特别是控制位于最上部的接触处理室中的液相的粘度等于1 相对于参考粘度＆eegr; 0作为p的粘度，范围为0.9＆nlE;＆eegr; 1 / eegr; 0＆nlE; 2.0 在预定温度下液相的重新确定的参考组合物。

公开(公告)号：US08183336B2

公开(公告)日：2012-05-22

申请号：US12789705

申请日：2010-05-28

申请人： Hiroyuki Sato ,  Koichi Suzuki ,  Hirohito Kawama

发明人： Hiroyuki Sato ,  Koichi Suzuki ,  Hirohito Kawama

IPC分类号： C08F6/10 ,  C08F6/12 ,  C08J3/12 ,  C08J3/14 ,  C08G75/10 ,  C08G75/14 ,  C08G75/16 ,  C08L81/00

CPC分类号： C08G75/02 ,  C08G75/0209 ,  C08G75/0213 ,  C08G75/0254 ,  C08G75/0281

摘要： In a process for producing a poly(arylene sulfide) by polymerizing a sulfur source and a dihalo-aromatic compound in the presence of an alkali metal hydroxide in an organic amide solvent, the production process comprises washing a polymer obtained by the polymerization with a hydrophilic organic solvent containing water in a proportion of 1 to 30% by weight, thereby collecting a purified polymer, the content of nitrogen contained in an extract extracted by a mixed solvent containing 40% by weight of acetonitrile and 60% by weight of water from the purified polymer is at most 50 ppm on the basis of the weight of the polymer, and a poly(arylene sulfide), the content of nitrogen contained in an extract extracted by a mixed solvent containing 40% by weight of acetonitrile and 60% by weight of water from the purified polymer is at most 50 ppm on the basis of the weight of the polymer.

摘要翻译： 在有机酰胺溶剂中，在碱金属氢氧化物存在下，通过使硫源和二卤代芳族化合物聚合来制造聚（亚芳基硫醚）的方法中，所述制造方法包括用亲水性 含水比例为1〜30重量％的有机溶剂，由此收集纯化聚合物，将含有40重量％乙腈和60重量％水的混合溶剂萃取提取的氮含量从 纯聚合物基于聚合物的重量为至多50ppm，聚（亚芳基硫醚）包含在通过包含40重量％乙腈和60重量％的混合溶剂萃取的提取物中的氮含量 基于聚合物的重量，来自纯化的聚合物的水的至多50ppm。

公开(公告)号：US20070265425A1

公开(公告)日：2007-11-15

申请号：US11666346

申请日：2005-10-26

申请人： Koichi Suzuki ,  Hiroyuki Sato ,  Nobuo Sato ,  Hirohito Kawama

发明人： Koichi Suzuki ,  Hiroyuki Sato ,  Nobuo Sato ,  Hirohito Kawama

IPC分类号： C08G75/14

CPC分类号： C08G75/025

摘要： A process for producing a poly(arylene sulfide) including a charging step 1 of preparing a charging mixture containing an organic amide solvent, a sulfur source, an alkali metal hydroxide, water and a dihalo-aromatic compound and having a pH of at least 12.5; a first-stage polymerization step 2 of heating the mixture to initiate a polymerization reaction, thereby forming a prepolymer that a conversion of the dihalo-aromatic compound is at least 50%; and a second-stage polymerization step 3 of adding a phase separation agent into the reaction system and adding an alkali metal hydroxide in an amount corresponding to 1 to 10 mol % per mol of the charged sulfur source at a time or in portions, thereby continuing the polymerization reaction.

摘要翻译： 一种制备聚（亚芳基硫醚）的方法，其包括充电步骤1，其制备含有有机酰胺溶剂，硫源，碱金属氢氧化物，水和二卤代芳族化合物并且pH为至少12.5 ; 加热混合物以引发聚合反应的第一阶段聚合步骤2，从而形成二卤代芳族化合物的转化率至少为50％的预聚物; 以及将相分离剂添加到反应体系中并且每次相当于每摩尔加入的硫源1〜10摩尔％的碱金属氢氧化物的时间或部分添加的第二阶段聚合步骤3，从而继续 聚合反应。

公开(公告)号：US20100234559A1

公开(公告)日：2010-09-16

申请号：US12789705

申请日：2010-05-28

申请人： Hiroyuki Sato ,  Koichi Suzuki ,  Hirohito Kawama

发明人： Hiroyuki Sato ,  Koichi Suzuki ,  Hirohito Kawama

IPC分类号： C08G75/14

CPC分类号： C08G75/02 ,  C08G75/0209 ,  C08G75/0213 ,  C08G75/0254 ,  C08G75/0281

摘要： In a process for producing a poly(arylene sulfide) by polymerizing a sulfur source and a dihalo-aromatic compound in the presence of an alkali metal hydroxide in an organic amide solvent, the production process comprises washing a polymer obtained by the polymerization with a hydrophilic organic solvent containing water in a proportion of 1 to 30% by weight, thereby collecting a purified polymer, the content of nitrogen contained in an extract extracted by a mixed solvent containing 40% by weight of acetonitrile and 60% by weight of water from the purified polymer is at most 50 ppm on the basis of the weight of the polymer, and a poly(arylene sulfide), the content of nitrogen contained in an extract extracted by a mixed solvent containing 40% by weight of acetonitrile and 60% by weight of water from the purified polymer is at most 50 ppm on the basis of the weight of the polymer.

摘要翻译： 在有机酰胺溶剂中，在碱金属氢氧化物存在下，通过使硫源和二卤代芳族化合物聚合来制造聚（亚芳基硫醚）的方法中，所述制造方法包括用亲水性 含水比例为1〜30重量％的有机溶剂，由此收集纯化聚合物，将含有40重量％乙腈和60重量％水的混合溶剂萃取提取的氮含量从 纯聚合物基于聚合物的重量为至多50ppm，聚（亚芳基硫醚）包含在通过包含40重量％乙腈和60重量％的混合溶剂萃取的提取物中的氮含量 基于聚合物的重量，来自纯化的聚合物的水的至多50ppm。

公开(公告)号：US20100113739A1

公开(公告)日：2010-05-06

申请号：US12653623

申请日：2009-12-16

申请人： Hiroyuki Sato ,  Koichi Suzuki ,  Hirohito Kawama

发明人： Hiroyuki Sato ,  Koichi Suzuki ,  Hirohito Kawama

IPC分类号： C08G75/14

CPC分类号： C08G75/0204 ,  C08G75/0213 ,  C08G75/0254 ,  C08G75/0281

摘要： A poly(arylene sulfide) having properties that a melt viscosity is 1 to 3,000 Pa·s as measured under conditions of a temperature of 310° C. and a shear rate of 1,216 sec−1, a pH is 7.0 to 12.0 as measured in a mixed solvent of water/acetone (volume ratio=2/1), a crystallization temperature is at most 220° C. as measured in the course of lowing the temperature of the polymer at a rate of 10° C./min from a molten state, and a whiteness degree is at least 70 as measured in the form of a melt molded or formed product, and a production process thereof.

摘要翻译： 在温度310℃，剪切速度1216秒-1的条件下测定的熔融粘度为1〜3000Pa·s的特性的聚（亚芳基硫醚），pH为7.0〜12.0，如 水/丙酮的混合溶剂（体积比= 2/1），结晶温度为至多220℃，在从聚合物的温度以10℃/ min的速度降低的过程中测量 熔融状态，并且以熔融成型或成形品的形式测量的白度为至少70及其制造方法。

公开(公告)号：US20070161777A1

公开(公告)日：2007-07-12

申请号：US10584629

申请日：2004-12-20

申请人： Hiroyuki Sato ,  Koichi Suzuki ,  Hirohito Kawama

发明人： Hiroyuki Sato ,  Koichi Suzuki ,  Hirohito Kawama

IPC分类号： C08G75/00 ,  C08L81/00

CPC分类号： C08G75/02 ,  C08G75/0209 ,  C08G75/0213 ,  C08G75/0254 ,  C08G75/0281

摘要： In a process for producing a poly(arylene sulfide) by polymerizing a sulfur source and a dihalo-aromatic compound in the presence of an alkali metal hydroxide in an organic amide solvent, the production process comprises washing a polymer obtained by the polymerization with a hydrophilic organic solvent containing water in a proportion of 1 to 30% by weight, thereby collecting a purified polymer, the content of nitrogen contained in an extract extracted by a mixed solvent containing 40% by weight of acetonitrile and 60% by weight of water from the purified polymer is at most 50 ppm on the basis of the weight of the polymer, and a poly(arylene sulfide), the content of nitrogen contained in an extract extracted by a mixed solvent containing 40% by weight of acetonitrile and 60% by weight of water from the purified polymer is at most 50 ppm on the basis of the weight of the polymer.

摘要翻译： 在有机酰胺溶剂中，在碱金属氢氧化物存在下，通过使硫源和二卤代芳族化合物聚合来制造聚（亚芳基硫醚）的方法中，所述制造方法包括用亲水性 含水比例为1〜30重量％的有机溶剂，由此收集纯化聚合物，将含有40重量％乙腈和60重量％水的混合溶剂萃取提取的氮含量从 纯聚合物基于聚合物的重量为至多50ppm，聚（亚芳基硫醚）包含在通过包含40重量％乙腈和60重量％的混合溶剂萃取的提取物中的氮含量 基于聚合物的重量，来自纯化的聚合物的水的至多50ppm。