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采用ZrOCl2.8H2O和La(NO3)3.9H2O共沉淀法制备固体超强酸SO42-/ZrO2-La2O3催化剂。固体超强酸SO24-/ZrO2-La2O3制备条件为nZr/nLa为6∶1,-15℃陈化24 h,120℃干燥12 h,浸渍液硫酸浓度为0.5 mol/L,浸渍4 h,120℃干燥1 h,600℃焙烧4 h。将此固体超强酸用于邻苯二甲酸酐和正丁醇合成邻苯二甲酸二丁酯的酯化反应,考察了正丁醇和邻苯二甲酸酐的物质的量比、催化剂用量、反应时间、反应温度对酯化反应的影响。结果表明,醇酐的物质的量比为3.5∶1,催化剂用量为所用邻苯二甲酸酐的2.7%,反应时间3 h,反应温度160℃条件下酯化收率达91.6%。
The solid superacid SO42- / ZrO2-La2O3 catalyst was prepared by coprecipitation of ZrOCl2.8H2O and La (NO3) 3.9H2O. Solid superacid SO24- / ZrO2-La2O3 was prepared under the conditions of nZr / nLa of 6:1, aged at -15 ℃ for 24 h and dried at 120 ℃ for 12 h. The concentration of sulfuric acid in the impregnation solution was 0.5 mol / L, Dry 1 h, calcined at 600 ℃ for 4 h. This solid superacid was used for the esterification of dibutyl phthalate with phthalic anhydride and n-butanol. The effects of the molar ratio of n-butanol to phthalic anhydride, the amount of catalyst, the reaction time, Effect of reaction temperature on esterification reaction. The results showed that the molar ratio of alcohol to anhydride was 3.5:1, the amount of catalyst was 2.7% of the phthalic anhydride used, the reaction time was 3 h, and the esterification yield was 91.6% at 160 ℃.