酸化膨润土催化合成草酸二丁酯  

Synthesis of dibutyl oxalate over bentonite activated by acid

作　　者：李春华 丁斌[2] 郝凤岭[2] 

机构地区：[1]中国石油集团工程设计有限责任公司东北分公司,吉林吉林132002 [2]吉林化工学院,吉林吉林132022

出　　处：《工业催化》2008年第7期61-65,共5页Industrial Catalysis

基　　金：中国石油吉林石化资助项目(G-00-学-05)

摘　　要：以酸化膨润土(SO42-/Bentonite)固体酸为催化剂,草酸和正丁醇为原料,合成草酸二丁酯。考察焙烧温度对催化剂活性的影响。结果表明,焙烧温度500℃时催化剂活性较好。考察反应温度、原料配比、催化剂用量和反应时间等因素对酯化反应的影响,通过正交实验得到最佳酯化反应工艺条件:n(正丁醇)∶n(草酸)=3.5∶1,w(SO42-/Bentonite)=1.5%,反应温度130℃,反应时间3 h。最佳酯化反应条件下,草酸的转化率达到95.8%。催化剂重复使用6次后,草酸转化率达到93.6%。Synthesis of dibutyl oxalate from oxalic acid and n-butyl alcohol over bentonite activated by acid （SO4^2-/Bentonite） was studied. Preparation condition for the catalyst, such as calcination temperature,had apparently influence on catalytic behaviors of SO4^2-/Bentonite, with optimum calcination temperature of 500 ℃. Effects of reaction condition, i. e. , reaction temperature, n-butyl-alcohol-tooxalic-acid mole ratio, catalyst dosage and reaction time, was investigated. Optimum reaction condition was obtained by orthogonal experiment as follows： n（ n-butyl alcohol） ： n（oxalic acid） = 3.5： 1, catalyst dosage = 1.5% of the total mass of oxalic acid and n-butyl alcohol, reaction temperature 130 ℃, reaction time 3 h. Oxalic acid conversion of 95.8% was obtained. Activity of the catalyst kept at 93.6% after 6 cycles of use.

关 键 词：精细化学工程 膨润土 酸活化 酯化催化剂 草酸二丁酯 

分 类 号：O643.36[理学—物理化学]