聚乙二醇催化合成线型聚苯硫醚树脂工艺优化  

Optimization of Synthesis of Linear Polyphenylene Sulfide Resin Catalyzed by Polyethylene Glycol

作　　者：刘径源 刘肖岍 蔡宇昊 郑潘 蒋文伟[1] LIU Jingyuan;LIU Xiaoqian;CAI Yuhao;ZHENG Pan;JIANG Wenwei(College of Chemistry Engineering,Sichuan University,Chengdu 610065,China)

机构地区：[1]四川大学化学工程学院,四川成都610065

出　　处：《塑料工业》2023年第9期53-59,共7页China Plastics Industry

摘　　要：以硫氢化钠和对二氯苯为原料,采用聚乙二醇(PEG)-400为催化剂,以1,3-二甲基-2-咪唑啉酮(DMI)为溶剂合成了高分子量线型聚苯硫醚(PPS)树脂。考察了DMI溶剂脱水过程的稳定性;考察了反应水硫配比、催化剂用量、反应温度对聚苯硫醚树脂分子量以及收率的影响;通过红外光谱(FTIR)、热重(TG)等表征方法对产品进行了表征。实验结果表明,DMI体系的脱水过程稳定性显著优于N-甲基吡咯烷酮体系;在水硫物质的量比为1.6∶1、PEG用量20 g/(mol硫单体)、第一缩聚段温度200℃的条件下得到了最高的收率和黏均分子量。热分析显示合成的PPS树脂熔点较高,分子量分布较窄,具有良好的热稳定性能。High molecular weight linear polyphenylene sulfide(PPS)resins was synthesized by sodium sulfide and p-dichlorobenzene,using polyethylene glycol(PEG-400)as catalyst and 1,3-dimethyl-2-imidazolidinone(DMI)as solvent.The stability of the dehydration process of DMI solvent system was investigated.The effects of reaction water-sulfur ratios,catalyst amount and reaction temperature on the molecular weight and yield of the polyphenylene sulfide resin products were examined.The products were characterized by Fourier transform infrared spectroscopy(FTIR),thermogravimetry(TG)and other characterization methods.The experimental results show that the stability of the dehydration process of the DMI solvent system is significantly better than that of the N-methylpyrrolidone(NMP)solvent system.The highest yields and viscosity-averaged molecular weights are obtained at water-sulfur molar ratio of 1.6∶1,PEG dosage of 20 g per mole of sulfur,and a first polycondensation section temperature of 200℃.Thermal analysis shows that the synthesized PPS resin has a high melting point,narrow molecular weight distribution and good thermal stability properties.

关 键 词：聚苯硫醚 聚乙二醇 1 3-二甲基-2-咪唑啉酮 工艺优化 

分 类 号：TQ326[化学工程—合成树脂塑料工业]