高效液相色谱对聚芳砜合成反应中芳环氯水解的监测

The Monitoring of Hydrolysis of Chlorine on Aromatic Rings in the Synthesis Reaction of Poly(ethersulfone) s by High Performance Liquid Chromatography

本文用高效液相色谱法,以THF/H_2O为淋洗液,对一些反应中芳环取代氯的水解进行了卓有成效的监测。发现双氯部分水解的同时有缩聚现象存在,并且聚合体最终要水解为双酚或单酚,找到了双氯部分水解制单酚的最佳工艺条件;单酚于乙醇中成钾盐的过程没有苯环氯的水解现象,但有少量的聚合体生成;单酚钾盐于120～200℃的环丁砜中聚合,单酚相转移催化下甲基丙烯酰氯酯化及双酚S、双氯于150℃DMSO中聚合均未发现有明显的端氯水解现象。

In this paper,the hydrolysis of chlorine on aromatic rings was monitored successfully in a series reaction with HPLC. It was found that in some alkaline hydrolysis reactions, along with the chlorine hydrolysis lower polymer was formed also. In the following reactions such as the polymerization of 4-chloro-4-hydroxydiphenylsulfone syevite in sulfalone at 120～200℃,the esterification of 4-chloro-4-hydroxydiphenylsulfone with methacryloyl chloride and the polymerization of 4,4'-dihydroxydiphenylsulfone with 4,4'-dichlorodiphenylsulfone in DMSO,no evident hydrolysis of chlorine is found.