抗氧剂4,4′-二(苯基异丙基)二苯胺制备工艺开发

Preparation Process Research & Development on Antioxidant Bis[4-(2-phenyl-2-propyl)phenyl]amine

实验首先以二苯胺为原料,α-甲基苯乙烯为烷基化试剂,催化小试合成4,4′-二（苯基异丙基）二苯胺。考查了工艺条件对反应的影响。实验表明,适宜的反应条件是在氯化锌催化下,反应温度90℃,α-甲基苯乙烯和二苯胺的摩尔比为2.4∶1,催化剂的量为二苯胺摩尔量的7%,反应6个小时,收率可以达到87%。产品结构用核磁进行了表征,产品熔点为100.1~100.5℃。中试实验表明该工艺适合于工业化生产。

Bis[4-（2-phenyl-2-propyl）phenyl]amine was prepared using diphenylamine as raw material and α-methylstyrene as alkylation reagent through F-C alkylation reaction. The effect of reaction conditions on the yield of the product was investigated. It has been shown that the optimum conditions of the reaction is that the reaction temperature is 90 ℃, reaction time 6 h, the molar ratio ofα-methylstyrene to diphenylamine being 2.4∶1, using zinc chloride as catalyst. The yield of the product can be 87.0 %. Product was characterized by NMR. The melting point of product is 100.1~100.5 ℃. Pilot process experiment indicates that the process is suitable for industrial production.