SO_4^(2-)/ZrO_2-TiO_2的制备、表征及其催化合成丙酸正丁酯  

Preparation and characterization of SO_4^(2-)/ZrO_2-TiO_2 and its catalytic synthesis of n-butyl propionate

作　　者：董成[1] 王刚[1] 侯鑫[1] 徐骏[1] 张立庆[1] 

机构地区：[1]浙江科技学院生物与化学工程学院,杭州310023

出　　处：《浙江科技学院学报》2013年第6期419-424,共6页Journal of Zhejiang University of Science and Technology

基　　金：浙江省自然科学基金资助项目(Y404082);浙江省大学生科技创新活动计划(新苗人才计划)(2011R415025)

摘　　要：采用沉淀-浸渍法制备SO2-4/ZrO2-TiO2催化剂,并应用于催化合成丙酸正丁酯。利用单因素实验得出催化剂最优制备条件:Zr/Ti原子比1∶1、H2SO4浸渍溶液浓度1.0mol/L、焙烧温度600℃。利用正交实验得出SO2-4/ZrO2-TiO2催化合成丙酸正丁酯的最优条件:反应时间2.5h,催化剂用量1.0g,醇酸摩尔比1∶1,收率为77.36%。通过Hammett指示剂法、BET法、IR、TEM及XRD对催化剂进行表征,结果表明,该催化剂H0<-11.93,比表面适中,呈无定形态存在。焙烧过程形成了Zr-O-Ti结构,且SO2-4以螯合双配位式结合,反应前后催化剂形态结构变化较大。The n-butyl propionate was synthesized by SO4^2-/ZrO2-TiO2 prepared by dip-impregnation method. Under the conditions that n（Zr） ： n（Ti）=1： 1, H2SO4 solution was 1.0 mol/L, calcination temperature was 600 ℃, the catalyst had high activity. And the optimum synthesized conditions were reaction time 2.5 h, the amount of catalyst 1.0 g, molar ratio of acid to alcohol 1 ： 1, the yield of ester 77. 36%. Then the catalyst was characterized by methods of Hammett indicator, BET, FT-IR, TEM and XRD. Results showed that the catalyst had suitable specific area and its H0 〈-11. 93. Structure of Zr-O-Ti and chelatingSO4- were formed during cacination and no crystall was found. The surface structure changed obviously after reaction.

关 键 词：丙酸正丁酯 正交实验 催化合成 表征 

分 类 号：TQ225.241[化学工程—有机化工] O643.32[理学—物理化学]