抗氧剂330合成工艺研究  

Synthetic process of antioxidant 330

作　　者：张毅 张新军 史建公 Zhang Yi;Zhang Xinjun;Shi Jiangong(Engineering Technology Research Institute of SCC,Beijing 101111,China;SINOPEC Catalyst(Beijing)Co.,Ltd.,Beijing 102400,China)

机构地区：[1]中国石化催化剂有限公司工程技术研究院,北京101111 [2]中石化催化剂(北京)有限公司,北京102400

出　　处：《合成树脂及塑料》2023年第2期27-32,36,共7页China Synthetic Resin and Plastics

摘　　要：研究了以中间体3,5-二叔丁基-4-羟基苄基甲基醚(简称苄醚)与均三甲苯为原料,在硫酸催化剂的作用下合成1,3,5-三甲基-2,4,6-三(3,5-二叔丁基-4-羟基苄基)苯(简称抗氧剂330)的工艺条件,确定了主要杂质的种类和结构,提出了副反应的反应机理,确定了副反应抑制剂的类型和用量。结果表明,合适的反应条件:硫酸含量为94.0%(w),催化剂与苄醚摩尔比1.2∶1.0,促进剂乙酸用量为苄醚质量的20%,反应温度宜控制在-10℃,苄醚与均三甲苯摩尔比(3.2∶1.0)~(3.3∶1.0);确定了影响抗氧剂330透光率和收率的2种主要杂质及其结构,分别为4,4′-双-(2,6-二叔丁基苯酚)甲烷和1,3,5-三甲基-2,4-二(3,5-二叔丁基-4-羟基苄基)苯;在反应体系中添加甲缩醛,可以抑制副反应的发生,合适的用量为苄醚质量的2.5%~5.0%;在优化的工艺条件下合成抗氧剂330,平均收率为87.7%,425,500 nm透光率均超过95%,达到了优级品的要求。The process conditions of synthesizing 1,3,5-trimethyl-2,4,6 tri(3,5-di-tert-butyl-4-hydroxybenzyl)benzene(antioxidant 330)were investigated by reacting intermediate 3,5-di-tert-butyl-hydroxybenzyl ether(benzyl ether)and mesitylene with sulfuric acid as catalyst.The types and structures of the main impurities in the reaction were identified,the reaction mechanism of the side reaction was proposed,and the types and amount of the sub-reactive inhibitor were determined.The results show that the optimum conditions are shown as follows:the concentration of catalyst H 2SO 4 is preferably 94%,the molar ratio of the catalyst to the intermediate benzyl ether is preferably 1.2∶1.0,and acetic acid is used as an accelerator,whose mass fraction in benzylether is 20%;the optimal reaction temperature is generally controlled at-10℃;the molar ratio of benzylether to mesitylene is preferably from 3.2∶1.0 to 3.3∶1.0.Two main impurities affecting the yield and light transmittance of antioxidant 330 are 4,4′-bis-(2,6-di-tert-butylphenol)methane and 1,3,5-trimethyl-2,4,-bis(3,5-di-tert-butyl)-4-hydroxybenzyl)benzene respectively.Methyl acetal in the reaction system can be added to suppress side reactions and whose mass fraction is from 2.5%to 5.0%.The average yield of the antioxidant 330 is 87.7%with the light transmittance of over 95%at both 425 and 500 nm under optimized process conditions,meeting the requirements for the excellent product.

关 键 词：1 3 5-三甲基-2 4 6-三(3 5-二叔丁基-4-羟基苄基)苯 3 5-二叔丁基-4-羟基苄基甲基醚 均三 甲苯 透光率 

分 类 号：TQ031.2[化学工程]