WO_3/MoO_3/SiO_2催化合成柠檬酸三丁酯

Synthesis of Tributy Citrate Catalyzed by WO_3/MoO_3/SiO_2

用正丁醇和柠檬酸为原料,WO3/MoO3/SiO2为催化剂催化合成柠檬酸三丁酯。通过考察醇与酸的物质的量比,反应温度和反应时间,催化剂用量和溶剂用量对酯化反应的影响。确定合成柠檬酸三丁酯的最佳反应条件为n(正丁醇)/n(柠檬酸)=4.5,催化剂用量为反应物柠檬酸质量的6%,反应温度130-140℃,反应时间3.5h,酯化率最高达98.5%,产率最高达94.3%。WO3/MoO3/SiO2催化剂可重复使用,其催化活性基本不变。实验对合成的产品进行了红外光谱分析及折光率的测定,与文献值相符。

Tributyl citrate was synthesized by nbutyl alcohol and citric acid, and WO3/MoO3/SiO2 used as the catalyst. The reactants molar ratio, reaction temperature and time, the effects of dosage of catalyst and solvent were investigated. The optimal reaction condition was as follow： n（n -butyl alcohol）/n（ citric acid） = 4.5：1. catalyst was 6% of the total mass of citric acid, reaction temperature was 130 - 140℃ ,reaction time was 4.5h, the esterifieation was above 98.5% and the yield up to 94.3%. Furthermore, the catalyst in the reaction could be resued again and again . The product was determined from IR and index of refractive.