四水硫酸铈催化合成乙二醇单乙醚乙酸酯

Synthesis of Ethylene Glycol Monoethyl Ether Acetate with Ceric Sulfate Tetrahydrate as Catalyst

以乙二醇单乙醚和乙酸为主要原料,以四水硫酸铈为催化剂,环己烷为带水剂,合成了乙二醇单乙醚乙酸酯。采用IR、1HNMR等对其结构进行了确证,考察了乙二醇单乙醚和乙酸的摩尔比、催化剂种类和用量、带水剂用量、反应温度、反应时间等因素对反应的影响,得到了适宜的反应条件为:以0.2 mol乙二醇单乙醚为基准,n(乙酸)∶n(乙二醇单乙醚)=1.5∶1,m(四水硫酸铈)∶m(乙二醇单乙醚)=0.05∶1,环己烷9 mL,反应温度130℃,反应时间2.5 h。在该条件下,乙二醇单乙醚乙酸酯收率达97%以上。

Ethylene glycol monoethyl ether acetate was synthesized from ethylene glycol monoethyl ether and acetic acid with ceric sulfate tetrahydrate as catalyst and cyclohexane as water entrainer. Its structure was confirmed by IR, i HNMR. The effects of molar ratio of ethylene glycol monoethyl ether to acetic acid, the variety and dosage of catalyst, the amount of water entrainer, reaction temperature and reaction time on the yield of the product were studied. Based on 0.2 tool ethylene glycol monoethyl ether,such optimum conditions as acetic acid/ethylene glycol monoethyl ether molar ratio of 1.5：1, ceric sulfate tetrahydrate/ethylene glycol monoethyl ether mass ratio of 0. 05 ： 1, amount of cyclohexane （used as water entrainer） of 9 mL, reaction temperature of 130 C, and reaction time of 2.5 h give the highest yield of ethylene glycol monoethyl ether acetate, which is above 97%