发明授权
- 专利标题: Fiber grade polyphenylene sulfide resin synthesis method
- 专利标题(中): 纤维级聚苯硫醚树脂合成方法
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申请号: US14655326申请日: 2013-10-29
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公开(公告)号: US09567440B2公开(公告)日: 2017-02-14
- 发明人: Zhirong Chen , Woyuan Li , Haoran Li , Ming Lian , Hong Yin , Guiyang Zhou , Xinfeng Zheng
- 申请人: ZHEJIANG NHU SPECIAL MATERIALS CO., LTD. , ZHEJIANG UNIVERSITY , SHANGYU NHU BIOLOGICAL CHEMICAL CO., LTD. , ZHEJIANG NHU COMPANY LTD.
- 申请人地址: CN Shangyu CN Hangzhou CN Shangyu CN Shaoxing
- 专利权人: ZHEJIANG NHU SPECIAL MATERIALS CO., LTD.,ZHEJIANG UNIVERSITY,SHANGYU NHU BIOLOGICAL CHEMICAL CO., LTD.,ZHEJIANG NHU COMPANY LTD.
- 当前专利权人: ZHEJIANG NHU SPECIAL MATERIALS CO., LTD.,ZHEJIANG UNIVERSITY,SHANGYU NHU BIOLOGICAL CHEMICAL CO., LTD.,ZHEJIANG NHU COMPANY LTD.
- 当前专利权人地址: CN Shangyu CN Hangzhou CN Shangyu CN Shaoxing
- 代理商 Jiwen Chen
- 优先权: CN201210576780 20121226
- 国际申请: PCT/CN2013/086096 WO 20131029
- 国际公布: WO2014/101564 WO 20140703
- 主分类号: C08G75/16
- IPC分类号: C08G75/16 ; C08G75/00 ; C08G75/02
摘要:
The present invention discloses a fiber-grade polyphenylene sulfide resin synthesis method, taking sodium bisulfide and p-dichlorobenzene as raw materials, N-methyl pyrrolidone as the solvent and C5-C6 fatty acid salt formed through dehydration to C5-C6 fatty acid and sodium hydroxide as the polymerization additive for synthesis through polymerization. White polyphenylene sulfide resin is obtained through acidification and washing of reaction slurry. In view of the fact that MFR is below 125 g/10 min, weight-average molecular weight as measured by GPC is over 4.2×104, and whiteness is over 90, it can satisfy requirements for fiber polyphenylene sulfide resin. C5-C6 fatty acid salt according to the method of the present invention has a higher solubility in NMP, which can better promote polymerization. It is to be fully diverted into the filtrate after filter prior to conversion into free fatty acid again through acidification with hydrochloric acid. C5-C6 fatty acid is available for azeotropy with water, which has a limited solubility in water. Therefore, it is applicable to recycle C5-C6 fatty acid from the filtrate through azeotropy with water, and thereby solve the problem with separation of additive and sodium chloride that are soluble in water.
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