过氧化双(2,4-二氯苯甲酰)的合成工艺研究

Study on Synthesis Process of Bis(2,4-dichlorobenzoyl)peroxide

研究过氧化双(2,4-二氯苯甲酰)(DCBP)的合成工艺。以氢氧化钠、过氧化氢和2,4-二氯苯甲酰氯作为主要原料,以氯仿作为反应的有机溶剂,在一定温度下完全反应,再以甲醇作为产物的惰性溶剂,进行溶析结晶与降温结晶相结合的重结晶过程,可得到高纯度的粉末状DCBP。合成DCBP的优化工艺条件为:氢氧化钠/过氧化氢/2,4-二氯苯甲酰氯物质的量比为2.4/1.2/2,反应温度为5~10℃,氯仿/2,4-二氯苯甲酰氯质量比为4/1,甲醇/2,4-二氯苯甲酰氯质量比为2.5/1,降温结晶温度为-15℃。在优化工艺条件下DCBP的收率为85.83%,纯度为99.78%,粒径小于50μm。

The synthesis process of bis(2,4-dichlorobenzoyl)peroxide(DCBP)was studied.The synthesis reaction was carried out at a certain temperature by using sodium hydroxide,hydrogen peroxide and 2,4-dichlorobenzoyl chloride as the main raw materials,and using chloroform as the solvent.After the reaction was completed,high purity powder DCBP could be obtained through the recrystallization process which included dissolution crystallization and cooling crystallization steps by using methanol as the inert solvent of the product.The optimum process conditions of DCBP synthesis were as follows:the molar ratio of sodium hydroxide/hydrogen peroxide/2,4-dichlorobenzoyl chloride was 2.4/1.2/2,the reaction temperature was 5~10℃,the mass ratio of chloroform/2,4-dichlorobenzoyl chloride was 4/1,the mass ratio of methanol/2,4-dichlorobenzoyl chloride was 2.5/1,and the cooling crystallization temperature was-15℃.Under the optimum process conditions,the yield of DCBP was 85.83%,the purity reached 99.78%,and the particle size was less than 50μm.