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 Antioxidant 1330 via Strong-acidic Cation Exchange Resin

摘要:

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）。考察了树脂类型、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2h，抗氧剂1330的收率 可达85.7%。树脂重复使用6次后，1330的收率 仍可保持在82%以上。该工艺无废硫酸产生，减少废水产生量约50%～60%。

Abstract:

Strong-acid cation exchange resins were employed to catalyze to synthesize 1,3,5-trimethyl-2,4,6-tris(3,5-di-tertbutyl-4-hydroxybenzyl)benzene(antioxidant-1330). During the reaction, a methanol-containing binary azeotrope mixture which was generated as by-product need to be distillated. The effect of type and quantity of resins, reaction time, repeated times of catalyst on the yield were investigated. Results of experiments show that the activity of big bore resins without water was higher than aquiferous ones. The most preferred conditions are as follow: n(3,5-di-tertbutyl-4-hydroxybenzyl methyl ether):n(mesitylene)=3.6:1, m(resin):m(3,5-di-tertbutyl-4-hydroxybenzyl methyl ether)=1.03:1, reaction temperature 40℃ and reaction time 2 h. The yield of UV-1330 is 85.7% which can be kept above 82% after repeat used 6 times. In this new process, there is no waste acid and the effluent can be reduced 50 to 60 percent compared with prior process.