氧化法合成四甲基联苯二酚二缩水甘油醚的工艺研究

Synthesis of tetramethyl-diphenyldiglycidyl ether by oxidation method

以3,3′,5,5′-四甲基联苯二酚(TMBP)为原料,通过溴代反应和氧化反应合成了3,3′,5,5′-四甲基联苯二酚二缩水甘油醚,采用红外和核磁对目标化合物结构进行了表征。考察了原料配比,碱盐种类及用量等因素对产物收率的影响,并通过正交实验的方法确定了其它因素的最佳值,经反复实验得出最佳工艺条件为n(碳酸钾)∶n(3-溴丙烯)∶n(TMBP)=2.5∶3∶1,溴代反应温度40℃,氧化反应温度30℃,氧化反应时间30h,n(间氯代过氧化苯甲酸)∶n(TMBP)=1.12∶1,产品产率和纯度分别可达85%和99%以上。

3,3＇, 5,5＇-tetramethyl-diphenyldiglycidyl ether was synthesized from 3,3＇, 5,5＇-tetramethyl- diphenol by bromination and oxidation. The chemical structure of product was characterized by IR and 1 HNMR respectively. The effects of the molar ratio of reactants,the variety and amount of base on the yield of the product were investigated, the other reaction conditions were determined by means of or thogonal experiments, The optimum process was determined and was n （3,3＇, 5,5＇-tetramethyl-diphe- nol） ： n（3-bromopropene） ： n（K2CO3）= 1 ： 3 ： 2.5,the temperature of bromination reaction was 30℃ ,the temperature and time of oxidation were 30 ℃ and 24 h,the yield and purity were above 85%and 99%.