公开(公告)号：US09567440B2

公开(公告)日：2017-02-14

申请号：US14655326

申请日：2013-10-29

申请人： ZHEJIANG NHU SPECIAL MATERIALS CO., LTD. ,  ZHEJIANG UNIVERSITY ,  SHANGYU NHU BIOLOGICAL CHEMICAL CO., LTD. ,  ZHEJIANG NHU COMPANY LTD.

发明人： Zhirong Chen ,  Woyuan Li ,  Haoran Li ,  Ming Lian ,  Hong Yin ,  Guiyang Zhou ,  Xinfeng Zheng

IPC分类号： C08G75/16 ,  C08G75/00 ,  C08G75/02

CPC分类号： C08G75/16 ,  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.

摘要翻译： 本发明公开了以二硫化二钠和对二氯苯为原料的纤维级聚苯硫醚树脂的合成方法，将N-甲基吡咯烷酮作为溶剂和通过脱水形成C5-C6脂肪酸和 氢氧化物作为通过聚合合成的聚合添加剂。 白色聚苯硫醚树脂通过反应浆液的酸化和洗涤得到。 鉴于MFR低于125g / 10min，通过GPC测得的重均分子量超过4.2×104，白度超过90，可以满足纤维聚苯硫醚树脂的要求。 根据本发明方法的C5-C6脂肪酸盐在NMP中的溶解度较高，可以更好地促进聚合。 过滤后将其全部转入滤液，然后再用盐酸酸化再转化成游离脂肪酸。 C5-C6脂肪酸可与水共沸，其在水中的溶解度有限。 因此，适用于通过与水共沸从滤液中回收C5-C6脂肪酸，从而解决了可溶于水的添加剂和氯化钠的分离问题。