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以强酸性离子交换树脂为催化剂,通过共沸将反应副产物甲醇分离,催化合成了1,3,5-三甲基-2,4,6-三(3,5-二叔丁基-4-羟基苄基)苯(抗氧剂1330)。考察了树脂的类型与用量、反应时间、催化剂重复使用对收率的影响。结果表明:干燥、高交换容量的大孔径强酸性树脂对反应的催化效果较好。最佳工艺条件为n(3,5-二叔丁基-4-羟基苄基甲基醚)∶n(均三甲苯)=3.6∶1,m(树脂)∶m(3,5-二叔丁基-4-羟基苄基甲基醚)=1.03∶1,40℃反应2 h,抗氧剂1330的收率可达85.7%。树脂重复使用6次,抗氧剂1330的平均收率为84.75%。该工艺无废硫酸产生,减少废水产生量约50%~60%。
Strong acid ion exchange resin as a catalyst, by azeotropic reaction by-product methanol separation, catalytic synthesis of 1,3,5-trimethyl-2,4,6-tris (3,5-di-tert-butyl- Hydroxybenzyl) benzene (antioxidant 1330). The effects of the type and amount of resin, the reaction time and the repeated use of catalyst on the yield were investigated. The results showed that the macroporous strong acid resin with high drying capacity and high exchange capacity has a good catalytic effect on the reaction. The optimum conditions were as follows: n (3,5-di-tert-butyl-4-hydroxybenzyl ether) Butyl-4-hydroxybenzyl methyl ether) = 1.03:1, 40 ℃ for 2 h, the yield of antioxidant 1330 can reach 85.7%. The resin was reused 6 times, and the average yield of antioxidant 1330 was 84.75%. The process produces no waste sulfuric acid, reducing the amount of wastewater generated about 50% to 60%.