摘要
以磷钨钼杂多酸作催化剂,在超声条件下,以正丁醇和冰醋酸为原料,合成乙酸正丁酯。首先制备了催化剂磷钨钼杂多酸,并对其进行了IR和XRD表征,证明了所制备的磷钨钼杂多酸催化剂具有Keggin的结构。进一步较系统地研究了酯化反应中催化剂焙烧温度、催化剂用量、带水剂种类与用量、醇酸摩尔比、反应时间等对酯化率的影响。结果表明,反应的适宜条件为:在20 kHz,1.0 W/cm2的超声条件下,催化剂焙烧温度为400℃,用量为0.6 g,带水剂为甲苯,用量为10 mL,反应温度为120℃,n(正丁醇)∶n(乙酸)=1.5∶1(乙酸用量为0.4mol),反应时间60 min,酯化率可达99.3%。
The synthesis of n-butyl acetate catalyzed by heteropolyacids H3PW6Mo6O40 under ultrasound irradiation was investigated.The catalyst was prepared and characterized by IR and XRD.The results indicate that the catalyst retains the Keggin-type structure.Then the effects of calcination temperature of catalyst,amounts of catalyst,the type and amount of water-carrying agent,molar ratio of n-butanol and acetic acid,and the reaction time on the yield of esterification were discussed systematically.The optimum conditions are as follows：when the conditions of ultrasound are 20 kHz and 0.1 W/cm2,the calcination temperature of catalyst is 400 ℃;the amounts of catalyst is 0.6 g;reaction temperature 120 ℃;n（n-butanol）∶n（acetic acid）=1.5∶1（acetic acid is 0.4 mol）;reaction time 60 min.Under these conditions,the yield of esterification is 99.3%.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2010年第4期382-386,共5页
Fine Chemicals
关键词
乙酸正丁酯
超声
杂多酸催化剂
酯化反应
医药与日化原料
n-butyl acetate
ultrasonic
heteropolyacids catalyst
esterification reaction
drug and cosmetic materials
作者简介
韩越（1985-），女，山东邹城人，硕士研究生，师从吕效平教授，电话：15850588101。
联系人：吕效平，教授，电话：025-83587192，13337724820，E-mail：xplu@njut．edu．cn
