柠檬酸三乙酯的新催化合成

New Catalytic Synthesis of Triethyl Citrate

实验首次采用中孔分子筛MCM-41为催化剂,直接用反应物乙醇作带水剂,用乙醇和柠檬酸为原料合成了柠檬酸三乙酯。考察了催化剂用量、反应物物质的量比、反应温度和反应时间对柠檬酸三乙酯收率的影响。通过实验得出该反应最佳的合成条件是:柠檬酸和乙醇的物质的量配比为1∶8,催化剂的量为柠檬酸质量的1.5%,反应时间为6 h,反应在剧烈回流温度下进行。在此条件下,柠檬酸三乙酯的收率可达89.8%,纯度大于99.5%。反应条件温和,操作简单,产物提纯容易,适合工业化生产。

In this paper,triethyl citrate was synthesized from citrate acid and ethanol using mesoporous molecular sieves MCM-41 as catalyst and ethanol as dehydrating for the first time.The factors such as catalyst amount,reactant ratio,reaction temperature and reaction time which affect the yield were investigated.The result showed that the optimum conditions are as follows：the mole ratio of citrate acid to ethanol is 1∶8;the amount of catalyst is 1.5% to citrate acid;the reaction time is 6 h at reflux temperature.The yield is 89.8% and the purity of the product is above 99.5% under the optimum conditions.The reaction conditions were mild,the process was simple,and the product was easily purified and suitable for industrialized production.