新型抗氧剂KY-1330合成的研究

采用两步法合成抗氧剂1,3,5-三甲基-2,4,6-三(3,5-二叔丁基-4-羟基苄基)苯(KY-1330),先以2,6-二叔丁基苯酚和多聚甲醛为原料,醚化合成3,5-二叔丁基-4-羟基苄基甲基醚,再与均三甲苯进行缩合反应得到抗氧剂KY-1330。通过正交实验优化了反应条件,醚化条件为:2,6-二叔丁基苯酚15.0 g,多聚甲醛3.5 g,催化剂二甲胺用量1.5 mL,反应温度100℃,反应时间为190 min,搅拌速度100 r/min,产率为87.2%;缩合条件为:3,5-二叔丁基-4-羟基苄基甲基醚与均三甲苯的摩尔比为4∶1,反应温度为5℃,反应时间为120 min,硫酸质量分数为80%,产率为81.5%。

Studies on the synthesis of new antioxidant KY-1330

The two-step method was used in synthesis of antioxidant 1,3,5-trimethyl-2,4,6-tris(3,5-di-tert-butyl-4-hydroxybenzyl)benzene(KY-1330).The first step,2,6-di-tert-butyl-4-(methoxymethyl)phenol were synthesized from 2,6-di-tert-butyl phenol and paraformaldehyd;the second step,2,6-di-tert-butyl-4-(methoxymethyl)phenol reacted with mesitylene to produce KY-1330.The reaction conditions were optimized by using the orthogonal experiment.The etherification reaction conditions were 2,6-di-tert-butyl phenol 15 g,paraformaldehyde 3.5 g,catalyst dimethylamine 1.5 mL,reaction temperature 100 ℃,reaction time 190 min,stirring speed 100 r/min,yield 87.2%;the condensation conditions were molar ratio of 2,6-di-tert-butyl-4-(methoxymethyl)phenol to mesitylene 4 ∶1,reaction temperatrure 5 ℃,reaction time 120 min,mass fraction of sulfuric acid 80%,yield 81.5%.