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    Process for preparing polyarylene thioether having thiol/thiolate end group concentration of 10 micro mole/g or less
    1.
    发明授权
    Process for preparing polyarylene thioether having thiol/thiolate end group concentration of 10 micro mole/g or less 失效
    具有硫醇/硫醇基端基浓度为10微摩尔/克以下的聚亚芳基硫醚的方法

    公开(公告)号：US4761468A

    公开(公告)日：1988-08-02

    申请号：US015346

    申请日：1987-02-17

    申请人： Tsuneo Okamoto ,  Takao Iwasaki ,  Yo Iizuka ,  Zenya Shiiki

    发明人： Tsuneo Okamoto ,  Takao Iwasaki ,  Yo Iizuka ,  Zenya Shiiki

    IPC分类号： C08G75/02 ,  C08G75/06 ,  C08G75/14

    CPC分类号： C08G75/0254 ,  C08G75/0245

    摘要： In a process for producing a polyarylene thioether having high stability by dehalogenation/sulfurization reaction of an alkali metal (M) sulfide such as sodium sulfide and a dihaloaromatic compound such as paradichlorobenzene in a polar organic solvent, the haloaromatic compound is used excessively in an appropriate range rather than the alkali metal sulfide and the latter stage of the reaction or all period of the reaction is conducted under a powerful stirring condition to a certain degree to obtain the polyarylene thioether wherein the concentration of --SM or --SH groups of the polymer terminal is lowered. The polyarylene thioether thus obtained suppresses the coloration in the processing with an apparatus made of ferrous material such as extruder.

    摘要翻译： 在通过碱金属（M）硫化物如硫化钠和二卤代芳族化合物如对二氯苯在极性有机溶剂中的脱卤/硫化反应具有高稳定性的聚亚芳基硫醚的制备方法中，卤代芳族化合物过量地用于适当的 范围而不是碱金属硫化物，反应的后期或反应的所有时间段在强力搅拌条件下进行一定程度，得到聚亚芳基硫醚，其中聚合物末端的-SM或-SH基团的浓度 被降低 由此获得的聚亚芳基硫醚通过用诸如挤出机的铁质材料制成的装置抑制加工中的着色。

    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。

    Process for producing polyarylene sulfide in titanium vessel with addition of water
    5.
    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.

    Polyarylene sulfide preparation in titanium reaction vessel with two distinct temperature ranges
    6.
    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
    9.
    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。