强酸性阳离子树脂催化合成受阻酚类抗氧剂1330

Synthetic Process of Hindered Phenolic Evernox 1330 via Strong-acidic Cation Ion Exchange Resins

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 cation ion exchange resins were employed to synthesize 1,3,5-trimethyl-2,4,6-tris（ 3,5-di-tert-butyl-4-hydroxybenzyl） benzene（ Evernox 1330）. And by-product methanol was separated by azeotrope reaction. The effect of different type of resins,dosage of resins,reaction time,reused times of the catalyst on the yield of Evernox 1330 were investigated. The results of experiments showed that the dry resins with a high cation exchange capacity and a large aperture showed higher catalytic activity. The optimum processing conditions were obtained as follows： n（ 3,5-di-tert-butyl-4-hydroxy benzyl methyl ether） ∶ n（ mesitylene） = 3. 6∶1,m（ resin） ∶ m（ 3,5-di-tert-butyl-4-hydroxy benzyl methyl ether） = 1. 03∶1,reaction temperature 40 ℃,and reaction time 2 h. The yield of Evernox 1330 could reach 85. 7% under the optimum processing condition,and the average yield is 84. 75% after the resins was reused six times. This new process for synthesis of Evernox 1330 does not generate waste sulfuric acid,which will reduce about 50% ~ 60% of the waste water emissions compared with the prior process.