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    Process for producing polyarylene sulfide in titanium vessel with addition of water
    3.
    发明授权
    Process for producing polyarylene sulfide in titanium vessel with addition of water 失效
    添加水在钛合金容器中生产聚芳硫醚的方法

    公开(公告)号：US4931516A

    公开(公告)日：1990-06-05

    申请号：US300938

    申请日：1989-01-24

    申请人： Yo Iizuka ,  Takao Iwasaki ,  Takayuki Katto ,  Zenya Shiiki

    发明人： Yo Iizuka ,  Takao Iwasaki ,  Takayuki Katto ,  Zenya Shiiki

    IPC分类号： C08G75/02 ,  C08G75/06

    CPC分类号： C08G75/0254 ,  C08G75/0231 ,  C08G75/0281

    摘要： 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., in which the reaction comprising said two steps is conducted for from 2 to 6 hours.

    Para-phenylene sulfide block copolymer, process for the production of the same
    4.
    发明授权
    Para-phenylene sulfide block copolymer, process for the production of the same 失效
    对亚苯基硫醚嵌段共聚物，生产过程相同

    公开(公告)号：US4785057A

    公开(公告)日：1988-11-15

    申请号：US858851

    申请日：1986-04-30

    申请人： Zenya Shiiki ,  Takayuki Katto ,  Yo Iizuka ,  Takao Iwasaki ,  Toshitaka Kouyama

    发明人： Zenya Shiiki ,  Takayuki Katto ,  Yo Iizuka ,  Takao Iwasaki ,  Toshitaka Kouyama

    IPC分类号： C08G75/0254 ,  C08G75/0245 ,  H01B3/30 ,  H05K1/03 ,  C08G75/14 ,  C08G75/16

    CPC分类号： H01B3/301 ,  C08G75/0231 ,  C08G75/0245 ,  C08G75/0254 ,  D01F6/765 ,  D01F6/78 ,  H05K1/0333 ,  Y10S428/901 ,  Y10T428/24909 ,  Y10T428/24917 ,  Y10T428/31533

    摘要： A para-phenylene sulfide block copolymer consisting essentially of a recurring unit (A) ##STR1## and a recurring unit (B) ##STR2## said recurring units (A) being present in the form of a block of 20 to 5,000 units of (A) on the average in the molecular chain, the mol fraction of the recurring units (A) being in the range of 0.50 to 0.98, the block copolymer having a melt viscosity (.eta.*) of 50 to 100,000 poise as determined at 310.degree. C. at a shear rate of 200 sec.sup.-1 and having: (a) a glass transition temperature (Tg) of 20.degree. to 80.degree. C., (b) a crystalline melting point (Tm) of 250.degree. to 285.degree. C., and (c) a crystallization index (Ci) of 15 to 45, this value being that of the heat-treated, but not stretch-oriented copolymer, which block copolymer is preferably produced by a process comprising a first step of heating an aprotic polar organic solvent containing a dihaloaromatic compound consisting essentially of a m-dihalobenzene and an alkali metal sulfide to form a reaction liquid (E) containing a m-phenylene sulfide polymer consisting essentially of recurring units (B) ##STR3## and a second step of adding a p-dihalobenzene to the reaction liquid (E) and heating the mixture in the presence of an alkali metal sulfide and an aprotic polar organic solvent to form a block copolymer consisting essentially of the recurring units (B) and recurring units (A) ##STR4##

    摘要翻译： 基本上由重复单元（A）＆lt; IMAGE＆gt;和重复单元（B）＆lt; IMAGE＆gt;组成的对亚苯基硫醚嵌段共聚物表示重复单元（A）以20-5,000单位（ A）平均分子链中，重复单元（A）的摩尔分数在0.50〜0.98范围内，嵌段共聚物的熔体粘度（η）为50〜100,000泊，在310℃下测定 （a）玻璃化转变温度（Tg）为20〜80℃，（b）结晶熔点（Tm）为250〜285℃ ，（c）15〜45的结晶指数（Ci），该值为热处理而不是拉伸取向共聚物的值，该嵌段共聚物优选通过包括加热第 含有主要由间二卤代苯和碱金属硫化物组成的二卤代芳族化合物的非质子极性有机溶剂形成反应液 （E），其包含基本上由重复单元（B）组成的间苯硫醚聚合物，第二步是将对二卤代苯加入到反应液（E）中，并在碱金属硫化物存在下加热混合物 和非质子极性有机溶剂以形成基本上由重复单元（B）和重复单元（A）组成的嵌段共聚物。

    Polyarylene sulfide preparation in titanium reaction vessel with two distinct temperature ranges
    5.
    发明授权
    Polyarylene sulfide preparation in titanium reaction vessel with two distinct temperature ranges 失效
    聚芳硫醚制备在钛反应容器中具有两个不同的温度范围

    公开(公告)号：US4812539A

    公开(公告)日：1989-03-14

    申请号：US79999

    申请日：1987-07-31

    申请人： Yo Iizuka ,  Takao Iwasaki ,  Takayuki Katto ,  Zenya Shiiki

    发明人： Yo Iizuka ,  Takao Iwasaki ,  Takayuki Katto ,  Zenya Shiiki

    IPC分类号： C08G75/02 ,  C08G75/06 ,  C08G75/16

    CPC分类号： C08G75/0254 ,  C08G75/0231 ,  C08G75/0281

    摘要： 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 235.degree. to 280.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., in which the reaction comprising said two steps is conducted for from 1 to 10 hours.

    Polyarylene sulfide preparation in titanium reaction vessel with two distinct temperature ranges
    7.
    发明授权
    Polyarylene sulfide preparation in titanium reaction vessel with two distinct temperature ranges 失效
    聚芳硫醚制备在钛反应容器中具有两个不同的温度范围

    公开(公告)号：US4745167A

    公开(公告)日：1988-05-17

    申请号：US941209

    申请日：1986-12-12

    申请人： Yo Iizuka ,  Takao Iwasaki ,  Takayuki Katto ,  Zenya Shiiki

    发明人： Yo Iizuka ,  Takao Iwasaki ,  Takayuki Katto ,  Zenya Shiiki

    IPC分类号： C08G75/02 ,  C08G75/06 ,  C08G75/16

    CPC分类号： C08G75/0254

    摘要： A process for the preparation of a high-molecular-weight polyarylene sulfide, which comprises subjecting an alkali metal sulfide such as sodium sulfide and a dihalo aromatic compound such as dichlorobenzene to dehalogenation sulfidation reaction in an organic amide solvent, wherein at least a part of the reaction is carried out in a reaction vessel in which at least the portion which the reaction liquid contacts is made of titanium, through at least the following two steps: (1) the step of carrying out the reaction at a temperature of 180.degree. to 235.degree. C. in the presence of water in an amount of 2.4 to 10 moles per mole of the alkali metal sulfide so that the conversion of the dihalo aromatic compound is at least 50% and the melt viscosity of the formed polyarylene sulfide does not exceed 500 P, and (2) the step of elevating the temperature to 245.degree. to 290.degree. C. in the presence of water in an amount of 2.5 to 10 moles per mole of the alkali metal sulfide with or without the addition of water to the reaction system and carrying out the reaction. The titanium reaction vessel is used for at least the step (1) and, preferably, for both the steps (1) and (2). The two-step reaction is advantageous in producing high molecular weight polyarylene sulfide.

    摘要翻译： 一种高分子量聚芳硫醚的制备方法，其特征在于，在有机酰胺类溶剂中，使硫化钠等碱金属硫化物和二氯苯等二卤化芳香族化合物进行脱卤硫化反应，其中，将至少一部分 反应在反应容器中进行，其中至少反应液体接触的部分由钛制成，至少通过以下两个步骤：（1）在180℃〜 235℃，每摩尔碱金属硫化物为2.4〜10摩尔的水存在下，二卤代芳族化合物的转化率为至少50％，形成的聚芳硫醚的熔融粘度不超过 500P，和（2）在水存在下将温度升至245℃至290℃的步骤，每摩尔碱金属硫化物的添加量为2.5至10摩尔 n的水转化为反应体系并进行反应。 所述钛反应容器至少用于步骤（1），优选用于步骤（1）和（2）。 两步反应在制备高分子量聚芳硫醚中是有利的。

    Polyarylenesulfide complexes, processes for production and uses thereof
    10.
    发明授权
    Polyarylenesulfide complexes, processes for production and uses thereof 失效
    聚芳硫醚络合物，其制备方法和用途

    公开(公告)号：US4613654A

    公开(公告)日：1986-09-23

    申请号：US734321

    申请日：1985-05-15

    申请人： Takayuki Katto ,  Toshitaka Kouyama ,  Takao Iwasaki ,  Zenya Shiiki

    发明人： Takayuki Katto ,  Toshitaka Kouyama ,  Takao Iwasaki ,  Zenya Shiiki

    IPC分类号： D01F6/76 ,  C08G75/02 ,  C08G75/06 ,  C08J5/18 ,  C08F283/00

    CPC分类号： C08G75/0295

    摘要： Novel polyarylenesulfide complexes are obtained by reacting a polyarylenesulfide with 0.05 to 20 mols of at least one strongly basic metal compound per 100 mols of arylenesulfide groups contained in the polyarylenesulfide under a uniformly dispersed condition, and have the properties defined in the following (A) through (C):(A) .eta.*/.eta..sub.0 *=3 to 100, wherein the .eta.* and .eta..sub.0 * stand for melt viscosities of the complex and the starting polyarylenesulfide, respectively;(B) .DELTA.T.sub.c2 =(T.sub.c2).sub.0 -T.sub.c2 =10 to 100.degree. C., wherein T.sub.c2 and (T.sub.c2).sub.0 stand for crystallization temperaturs of the complex and the starting polyarylenesulfide, respectively, observed when the polyarylenesulfide is cooled from its moten state; and(C) .DELTA.(.DELTA.E)=.DELTA.E-(.DELTA.E).sub.0 =5 to 75 kcal/mol, wherein .DELTA.E and (.DELTA.E).sub.0 stand for apparent flow activation energies of the complex and the starting polyarylenesulfide, respectively.The polyarylenesulfide complexes have higher melt viscosity with improved flow characteristics.

    摘要翻译： 通过在均匀分散的条件下使多芳基硫化物与包含在聚芳基硫醚中的每100摩尔芳基硫化物基团中的至少一种强碱性金属化合物与0.05至20摩尔的至少一种强碱性金属化合物反应获得新颖的聚芳硫醚络合物，并具有以下（A）至 （C）：（A）eta * / eta 0 * = 3至100，其中eta *和eta 0 *分别表示络合物和起始多芳基硫化物的熔体粘度; （B）DELTA Tc2 =（Tc2）0-Tc2 = 10〜100℃，其中Tc2和（Tc2）0分别代表复合物和起始多芳基硫化物的结晶温度，当聚芳基硫醚从其燃烧 州; 和（C）DELTA（DELTA E）= DELTA E-（DELTA E）0 = 5至75kcal / mol，其中DELTA E和（DELTA E）0分别表示络合物和起始聚芳基硫醚的表观流动活化能 。 聚芳硫醚配合物具有较高的熔体粘度和改善的流动特性。