硅锆双组份交联累托土固体酸催化合成水杨酸正丁酯

Synthesis of n-Butyl Salicylate Catalyzed by Mixed SiZr Pillared Rectorite Solid Acid

将自制的SO2-4改性硅锆双组份交联累托土固体酸催化剂(SO2-4/SiZrR)用于水杨酸(C7H6O3)和正丁醇(C4H10O)的酯化反应,与传统酯化反应催化剂以及其他交联剂交联的累托土作酯化反应的催化剂相比,SO2-4/SiZrR催化剂有更好的催化活性。考察了影响酯化反应的诸因素,并对产物进行了折光率测试、红外光谱分析。酯化反应的最佳条件为:酸醇比n(C7H6O3)/n(C4H10O)=1/1 65、催化剂占酸投料质量的百分比为w(SO2-4/SiZrR)=6 5%、反应温度120～135℃、反应时间6h,水杨酸的转化率可达86 85%,产物中水杨酸正丁酯的质量分数w(C11H14O3)>99 9%。

The mixed SiZr pillared rectorite, modified by SO^(2-)_4, was used as solid acid catalyst(SO^(2-)_4/SiZrR) in the preparation of n-butyl salicylate (C_(11)H_(14)O_3) from salicylic acid(C_7H_6O_3) and n-butyl alcohol(C_4H_(10)O). The results showed that SO^(2-)_4/SiZrR exhibited higher activity in the synthesis of C_(11)H_(14)O_3 than the traditional catalyts and the pillared rectorites with other pillaring agents. Over SO^(2-)_4/SiZrR catalyst, the optimized reaction conditions for preparation of C_(11)H_(14)O_3 were as follows: C_7H_6O_3/C_4H_(10)O molar ratio of 1∶1.65, catalyst/ C_7H_6O_3 ratio of 6.5wt%, reaction temperature of 120-135℃, and reaction time of 6h. The conversion of salicylate acid was up to 86.85%, and the content of n-butyl salicylate in product was over 99.9wt% tested by GC analysis.