线性高分子聚苯硫醚的合成及溶助剂循环利用的研究

Study on synthesis of linear poly(p-phenylene sulfide) resin with high molecular weight(HMW PPS) and recycling of solvent and additive

采用均匀设计法研究合成线性高分子聚苯硫醚(PPS)树脂。研究了反应温度、反应时间、原料配比、溶剂用量以及助剂用量等因素对产品得率的影响。实验数据经过多元逐步回归分析,找出其最佳工艺条件:前期反应温度为210.9℃,反应时间为2.8 h;后期反应温度为270℃,反应时间为2.5 h,n(Na2S.9H2O)∶n(对二氯苯)=1.1∶1,V(N-甲基吡咯烷酮)∶n(对二氯苯)=550 mL∶1 mol,m(助剂)∶n(对二氯苯)=20 g∶1 mol。按照此反应条件下反应得到线性高分子聚苯硫醚树脂,其重均相对分子质量接近60 000,平均收率在93.7%以上。不需繁琐的回收工艺,即同时实现了助剂和溶剂的可循环利用,多次循环利用后产品的收率仍高于91.2%。并用热分析、红外分析、元素分析对产品进行了表征。

Uniform design was applied to study the synthesis of linear poly （p-phenylene sulfide） resin with high molecular weight （HMW PPS）. The effects of reaction temperature, reaction time, the molar ratio of reaction monomers, the amoum of solvent and catalyst on the yield of HMW PPS were investigated. The optimal reaction conditions were found by using multiple regression analysis based on the data obtained from uniform design experiments. The optimized conditions are as follows：210. 9~C and 2. 8 hours of reaction temperature and reaction time, respectively, in the early stage,270~C and 2. 5 hours of reaction temperature and reaction time,respectively,in the late stage, 1. 1：1 of molar ratio of N a2 S-9 H20 and para-dichlorobenzene, 550 mL ： 1 tool of ratio of NMP and para-dichlorobenzene, and 20 g ： 1 tool of the additive and para-dichlorobenzene. The molecular weight of the obtained HMW PPS is close to 60 000. The product yield is up to 93.7%. Both the solvent and the catalyst can be reused without complex recovering process. After several times of recycling, the yield of the product is still up to 91.2%. The obtained product is characterized by thermal analysis, IR and element analysis.