4,4′-二羟基二苯硫醚环氧树脂的合成与表征  

Synthesis and characterization of 4,4′-thiodiphenol epoxy

作　　者：郭雅妮[1] 何俭[1] 刘承美[2] 骆沛尧 

机构地区：[1]武汉工程大学材料科学与工程学院,湖北武汉430074 [2]华中科技大学化学与化工学院,湖北武汉430074

出　　处：《武汉工程大学学报》2014年第10期26-30,共5页Journal of Wuhan Institute of Technology

基　　金：湖北省自然科学基金项目(2012FFC10501);地方高校国家级大学生创新创业训练计划项目(201310490006);武汉工程大学科学研究基金项目(11115032)

摘　　要：以4,4′-二羟基二苯硫醚、环氧氯丙烷为原料,四正丁基溴化铵为催化剂,合成了4,4′-二羟基二苯硫醚环氧树脂,通过核磁共振氢谱、碳谱、傅立叶变换红外光谱表征了产物的结构.利用正交实验法研究了反应温度、醚化时间、闭环时间、原料配比对合成反应的影响,优化后的反应条件为:4,4′-二羟基二苯硫醚与环氧氯丙烷、四正丁基溴化铵的摩尔比为1∶10∶0.02,反应温度90℃,醚化时间4h,闭环时间2h,氢氧化钠与4,4′-二羟基二苯硫醚的摩尔比为1.2∶1.优化反应得到产物的环氧值为4.599mmol/g,产率为87.79%.通过对产物的结构表征,验证了两步法合成工艺路线的可行性.4,4＇-thiodiphenol epoxy was synthesized by using 4,4r-thiodiphenyl and epichlorohydrin as raw materials and using tetrabutylammonium bromide as a catalyst. The chemical structure of the product was confirmed by 1H nuclear magnetic resonance spectra, 13C nuclear magnetic resonance and fourier transform infrared. The effects of reaction temperature, etherification reaction time, ring closure reaction time and molar ratio of raw materials on the yield of the product were studied by an orthogonal experiment method. The optimum reaction conditions were confirmed as follows：the molar ratio of epi- chlorohydrin, tetrabutylammonium bromide and 4,4＇-thiodiphenyl is 10 ： 0.02 ： 1 ,and the molar ratio of sodium hydroxide and 4,4＇-thiodiphenyl is 1.2 ： 1, reaction temperature is 90 ℃, the etherification reaction time and the ring closure reaction time are 4 hours and 2 hours, respectively. Under these conditions, the epoxide value of the product is 4. 599 mmol/g and the yield is 87. 79%. The results of structure characterization show that the two-step preparation process is feasible.

关 键 词：4 4′-二羟基二苯硫醚 环氧树脂 合成 

分 类 号：TQ323.5[化学工程—合成树脂塑料工业]