新型催化剂La_2(SO_4)_3/SiO_2催化合成乙二醇乙醚乙酸酯  

Synthesis of Ethylene Glycol Monoethyl Ether Acetate with Silica-supported Lanthanum Sulfate as Catalyst

作　　者：常小玲[1] 李彬[1] CHANG Xiaoling LI Bin(Patent Examination Cooperation Center of the Patent Office , SIP0 , Henan , Zhengzhou 450002 , Chin)

机构地区：[1]国家知识产权局专利局专利审查协作河南中心,河南郑州450002

出　　处：《河南化工》2017年第4期20-23,共4页Henan Chemical Industry

摘　　要：以La_2O_3为镧源,粗孔硅胶为载体,制备了新型稀土盐催化剂La_2(SO_4)_3/SiO_2。采用上述催化剂,以乙二醇乙醚和乙酸为原料,通过单因素法,考察了乙二醇乙醚与乙酸的物质的量比、催化剂、带水剂用量、反应温度、时间对反应的影响,得到了合成乙二醇乙醚乙酸酯的适宜的条件:以乙二醇乙醚0.2mol计,n(乙二醇乙醚)∶n(酸)=1∶1.5,m(La_2(SO_4)_3/SiO_2)∶m(乙二醇乙醚)=0.045∶1,带水剂环己烷10 m L,加热温度120℃,反应时间2 h,在此适宜条件下乙二醇乙醚乙酸酯收率达到96%以上。采用IR、核磁对产品进行了表征。Using La2O3 as raw material, silochrom as support, a new rare -earth salt catalyst of La2 （ SO4 ） 3/SiO2 is prepared. Ethylene glycol monoethyl ether acetate is synthesized from ethylene glycol mo- noethyl ether and acetic acid with La2 （SO4）3/SiO2 as catalyst and cyclohexane as water entrainer, the effects of molar ratio of ethylene glycol monoethyl etherto acetic acid, dosage of catalyst, amount of water entrainer, reaction temperature and reaction time on the yield of the product are studied. Based on 0.2 mol ethylene glycol monoethylether,such optimum conditions as acetic acid/ethylene glycol monoethyl e- ther molar ratio of 1.5 ： 1, La2 （SO4） 3/SiO2 and ethylene glycol monoethyl ether mass ratio of 0.045 ： 1, mount of cyclohexane（ used as water entrainer ） of 10 mL, reaction temperature of 120 ℃, and reaction time of 2 h, give the highest yield of ethylene glycol monoethyl ether acetate, which is above 96%. Its structure is confirmed by IR, 1HNMR.

关 键 词：氧化镧 粗孔硅胶 乙二醇乙醚乙酸酯 

分 类 号：TQ225.242[化学工程—有机化工] TQ426