作　　者： ; ; ; ; ;

机构地区： 南京工业大学化学化工学院

出　　处： 《精细化工》 2010年第4期382-386,共5页

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%.

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

领　　域： [理学] [理学] [一般工业技术]