反应精馏法合成氯乙酸乙酯的工艺研究

Synthesis of ethyl chloroacetate by reactive distillation

以氯乙酸和无水乙醇为原料,环己烷为带水剂,采用反应精馏的方法合成氯乙酸乙酯。考察了催化剂种类、催化剂用量、原料配比、环己烷用量以及有效板数对反应的影响。结果表明,较佳的反应条件为:D8099-T强酸性阳离子交换树脂为催化剂,用量为氯乙酸质量的1.00%,n(氯乙酸)∶n(无水乙醇)=1∶3,环己烷用量为80m L/mol氯乙酸,有效板数为14。在该反应条件下,氯乙酸的转化率为100%,氯乙酸乙酯的收率为97.77%。

The synthesis of ethyl chloroacetate from chloroacetic acid and ethyl alcohol by reactive distillation using cyclohexane as water-carrying agent was studied. The effects of catalyst types and dosage, reactants ratio, cyclohexane amount and tray number on reaction were investigated. The results indicate that the optimal reaction conditions are as follows： D8099-T strong- acid cation resin as catalyst, mass ratio of catalyst to chloroacetic acid of 1.0%, molar ratio of chloroacetic acid to ethanol of 1 ： 3, cyclohexane 80 mL per mole chloroacetic acid, and tray number of 14. Under above conditions, the yield of ethyl chloroacetate and conversion of chloroacetic acid reached 97.77% and 100%, respectively.