低熔点线形高分子量聚苯硫醚的制备  

Preparation of Low Melting Point Linear High Molecular Weight Polyphenylene Sulfide

作　　者：时盼盼[1] 王明明[1] 姜一男 齐彩亚[1] 安会勇[1] 

机构地区：[1]辽宁石油化工大学,辽宁抚顺113001

出　　处：《当代化工》2016年第10期2277-2279,2287,共4页Contemporary Chemical Industry

基　　金：国家自然科学基金青年项目;项目号:201304042

摘　　要：采用硫磺溶液法,以硫磺和对二氯苯为原料,氯化锂和磷酸钠作为混合催化剂,在六甲基磷酰三胺溶剂中通过自缩聚反应制备聚苯硫醚。以聚苯硫醚的产率为目标参数,通过正交试验优化合成路线,制备低熔点线形高分子量聚苯硫醚。结果表明,最佳反应条件是催化剂用量0.9 g·mol^(-1),加水量为1.5 m L·mol^(-1),溶剂用量为600 m L·mol^(-1),反应温度为210℃,物料配比为1.1:1。此反应条件下PPS的产率为92.62%。由红外光谱分析和元素分析确定产物为线形结构;由DSC测定其熔点为240℃;采用粘度法测定其分子量为6.04×10~4。Polyphenylene sulfide was prepared from sulfur and p-dichlorobenzene by self-polycondensation with lithium chloride and sodium phosphate as catalysts, hexamethylphosphoramide as solvent. The optimum reaction conditions of low-melting point and high molecular weight linear polyphenylene sulfide were determined by orthogonal experiments as follows： the catalyst amount 0.9 g·mol^-1, the water amount 1.5 g·mol^-1, the solvent amount 600 m L·mol^-1, the reaction temperature 210 ℃, the material ratio 1.1：1. Under above conditions, the yield of polyphenylene sulfide can reach to 92.62%. The linear structure of product was determined by infrared spectroscopy and elemental analysis. The melting point was measured by DSC. Molecular weight was measured by viscosity method.

关 键 词：聚苯硫醚 低熔点 硫磺溶液法 正交试验 

分 类 号：TQ325[化学工程—合成树脂塑料工业]