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    Process for the preparation of cross-linked polyarylene sulfide
    1.
    发明授权
    Process for the preparation of cross-linked polyarylene sulfide 失效
    制备交联聚芳硫醚的方法

    公开(公告)号：US5268451A

    公开(公告)日：1993-12-07

    申请号：US985156

    申请日：1992-12-03

    申请人： Yo Iizuka ,  Toshio Hosokawa ,  Yoshinobu Itoh ,  Shinji Yamamoto ,  Kazuo Kusida ,  Takayuki Katto

    发明人： Yo Iizuka ,  Toshio Hosokawa ,  Yoshinobu Itoh ,  Shinji Yamamoto ,  Kazuo Kusida ,  Takayuki Katto

    IPC分类号： C08G75/02 ,  C08G75/14 ,  C08G79/04

    CPC分类号： C08G75/0231 ,  C08G75/0254

    摘要： The present invention discloses a process for producing a granular polyarylene sulfide which has a high melt viscosity and a high degree of cross-linkage, becomes gel under melting and is easy to handle in the production and the fabrication thereof.The process disclosed herein comprises (1) a step (A) an initial-stage polymerization step for obtaining a polyarylene sulfide by reacting an alkali metal sulfide, a dihaloaromatic compound and a polyhaloaromatic compound, having three or more halogen substituents in a molecule, in the presence of water in an amount of 0.5 to 2.9 moles per mol of said alkali metal sulfide at a temperature in the range of 180.degree. to 235.degree. C. until the total conversion ratio of said dihalo- and polyhaloaromatic compounds reaches 50 to 98% and the melt viscosity of a polyarylene sulfide obtained at the end of the step becomes 5 to 5,000 poise, measured at 310.degree. C. and a shear rate of 1,200/second; (2) a step (B) a temperature raising step in which while adjusting an amount of water to be 2.5 to 7 moles per mol of fed alkali metal sulfide, a temperature raising condition from the temperature of step (A) to 240.degree. C. is controlled so that the melt viscosity of a polymer obtained at 240.degree. C. reaches 300 to 10,000 poise, measured at 310.degree. C. and a shear rate of 1,200/second and the temperature raising rate between 240.degree. C. and a temperature of the following step (C) is further controlled to be within the range of 10.degree. to 100.degree. C./hour; and (3) a step (C) a second-stage polymerization step for further continuing the reaction at a temperature of 245.degree. to 290.degree. C. until a melt viscosity of the final product reaches not lower than 1.times.10.sup.5 poise, measured at 330.degree. C. and a shear rate of 2/second.The present invention also discloses a granular cross-linked polyarylene sulfide produced by the process described above.

    摘要翻译： 本发明公开了一种具有高熔体粘度和高交联度的粒状聚芳硫醚的制造方法，在熔融时变成凝胶，在制造和制造中易于处理。 本文公开的方法包括（1）步骤（A）初步阶段聚合步骤，用于通过在分子中具有三个或更多个卤素取代基的碱金属硫化物，二卤代芳族化合物和多卤芳族化合物在分子中反应获得聚芳硫醚 在180-235℃的温度范围内，每摩尔所述碱金属硫化物的存在量为0.5-2.9摩尔，直到所述二卤代和多卤芳族化合物的总转化率达到50-98％ 在步骤结束时得到的聚芳硫醚的熔融粘度在310℃下测定为5〜5000泊，剪切速度为1200 /秒; （2）步骤（B）升温步骤，其中当将每一摩尔进料的碱金属硫化物的水量调整为2.5至7摩尔时，将升温条件从步骤（A）的温度升至240℃ 被控制使得在240℃下获得的聚合物的熔体粘度达到300至10,000泊，在310℃和剪切速率为1200 /秒，升温速率在240℃和温度 的下一步骤（C）进一步控制在10℃至100℃/小时的范围内; 和（3）步骤（C）第二阶段聚合步骤，用于在245℃至290℃的温度下进一步继续反应，直到最终产物的熔融粘度达到不低于1×10 5泊，在330℃测量 C.和剪切速率2 /秒。 本发明还公开了通过上述方法制备的粒状交联聚芳硫醚。

    Process for the preparation of cross-linked polyarylene sulfide
    2.
    发明授权
    Process for the preparation of cross-linked polyarylene sulfide 失效
    制备交联聚芳硫醚的方法

    公开(公告)号：US5200500A

    公开(公告)日：1993-04-06

    申请号：US569766

    申请日：1990-08-22

    申请人： Yo Iizuka ,  Toshio Hosokawa ,  Yoshinobu Itoh ,  Shinji Yamamoto ,  Kazuo Kusida ,  Takayuki Katto

    发明人： Yo Iizuka ,  Toshio Hosokawa ,  Yoshinobu Itoh ,  Shinji Yamamoto ,  Kazuo Kusida ,  Takayuki Katto

    IPC分类号： C08G75/02

    CPC分类号： C08G75/0254 ,  C08G75/0231

    摘要： The present invention discloses a process for producing a granular polyarylene sulfide which has a high melt viscosity and a high degree of cross-linkage, becomes gel under melting and is easy to handle in the production and the fabrication thereof.The process disclosed herein comprises (1) a step (A) an initial-stage polymerization step for obtaining a polyarylene sulfide by reacting an alkali metal sulfide, a dihaloaromatic compound and a polyhaloaromatic compound, having three or more halogen substituents in a molecule, in the presence of water in an amount of 0.5 to 2.9 moles per mol of said alkali metal sulfide at a temperature in the range of 180.degree. to 235.degree. C. until the total conversion ratio of said dihalo- and polyhaloaromatic compounds reaches 50 to 98% and the melt viscosity of a polyarylene sulfide obtained at the end of the step becomes 5 to 5,000 poise, measured at 310.degree. C. and a shear rate of 1,200/second; (2) a step (B) a temperature raising step in which while adjusting an amount of water to be 2.5 to 7 moles per mol of fed alkali metal sulfide, a temperature raising condition from the temperature of step (A) to 240.degree. C. is controlled so that the melt viscosity of a polymer obtained at 240.degree. C. reaches 300 to 10,000 poise, measured at 310.degree. C. and a shear rate of 1,200/second and the temperature raising rate between 240.degree. C. and a temperature of the following step (C) is further controlled to be within the range of 10.degree. to 100.degree. C./hour; and (3) a step (C) a second -stage polymerization step for further continuing the reaction at a temperature of 245.degree. to 290.degree. C. until a melt viscosity of the final product reaches not lower than 1.times.10.sup.5 poise, measured at 330.degree. C. and a shear rate of 2/second.The present invention also discloses a granular cross-linked polyarylene sulfide produced by the process described above.

    摘要翻译： 本发明公开了一种具有高熔体粘度和高交联度的粒状聚芳硫醚的制造方法，在熔融时变成凝胶，在制造和制造中易于处理。 本文公开的方法包括（1）步骤（A）初步阶段聚合步骤，用于通过在分子中具有三个或更多个卤素取代基的碱金属硫化物，二卤代芳族化合物和多卤芳族化合物在分子中反应获得聚芳硫醚 在180-235℃的温度范围内，每摩尔所述碱金属硫化物的存在量为0.5-2.9摩尔，直到所述二卤代和多卤芳族化合物的总转化率达到50-98％ 在步骤结束时得到的聚芳硫醚的熔融粘度在310℃下测定为5〜5000泊，剪切速度为1200 /秒; （2）步骤（B）升温步骤，其中当将每一摩尔进料的碱金属硫化物的水量调整为2.5至7摩尔时，将升温条件从步骤（A）的温度升至240℃ 被控制使得在240℃下获得的聚合物的熔体粘度达到300至10,000泊，在310℃和剪切速率为1200 /秒，升温速率在240℃和温度 的下一步骤（C）进一步控制在10℃至100℃/小时的范围内; 和（3）步骤（C）第二阶段聚合步骤，用于在245℃至290℃的温度下进一步继续反应，直到最终产物的熔体粘度达到不低于1×10 5泊，在330℃测量 C.和剪切速率2 /秒。 本发明还公开了通过上述方法制备的粒状交联聚芳硫醚。