Synthesis of ethyl acetate by the esterification process: process optimization
酯化法合成乙酸乙酯：工艺优化

摘要

浓硫酸作为催化剂，通过酯化法高效合成了乙酸乙酯。系统研究表明，醇醋物质的量比、催化剂用量、反应温度、反应物进料速率、洗涤次数等对产物的产率和纯度有关键作用。采用毛细管气相色谱法对合成的乙酸乙酯纯度进行了表征，结果表明仅用5mL浓硫酸，乙酸乙酯产率可达71.05%。为获得较高的理论转化率，控制混合物的滴加速率为1-3s/滴。酯化反应的最佳温度为80-85℃。为了降低粗品中的乙醇含量，需要用饱和氯化钙至少洗涤2次粗品，以获得高纯度的乙酸乙酯产品。本文浓硫酸催化剂的用量远低于其他相关研究。

Abstract

Ethyl acetate was efficiently synthesized by the esterification process, using concentrated sulfuric acid as a catalyst. Systematic studies showed that the molarity ratio of ethanol to acetic acid, dosage of catalyst, reaction temperature, feeding rate of reactants, and washing times played a key role in controlling the productivity and purity of the products. The purity of synthesized ethyl acetate was characterized by the capillary gas chromatograph. It found that with only 5mL of concentrated sulfuric acid the productivity of ethyl acetate reached up to 71.05%. It also revealed that the rate of the addition of the mixture was controlled as 1-3s per drop in order to get high theoretical conversion rates. The optimal temperature of the esterification reaction is 80-85℃. It demonstrated that to reduce the ethanol of the crude product, it is necessary to wash the crude product with saturated calcium chloride at least 2 times to obtain high purity ethyl acetate product. In the paper, the usage of a catalyst of concentrated sulfuric acid was much less than in the other relevant studies.