钨钼混配型杂多酸盐催化剂上酯化反应条件的优化研究  

Optimization of the tungsten/molybdenum mixed heteropoly acid salt-catalyzed esterification reaction conditions

作　　者：舒庆[1] 刘宝[1] 宋胜海 张志武[1] 陈培德[1] 

机构地区：[1]江西理工大学冶金与化学工程学院,江西赣州341000

出　　处：《有色金属科学与工程》2014年第6期21-27,共7页Nonferrous Metals Science and Engineering

基　　金：国家自然科学基金资助项目(21206062);江西省教育厅科学基金项目(GJJ13391)

摘　　要：以Na2WO4·2H2O和Na2Mo O4·2H2O为原料,通过硝酸酸化-乙醚萃取法制备了一种钨钼混配型杂多酸盐催化剂(Na4Si Mo W12O40·x H2O).应用X射线荧光光谱对合成的催化剂的元素组成进行了分析;通过红外光谱对其的官能团结构进行了分析;借助热重分析对其的热稳定性进行了研究.并以正丁醇和乙酸为反应物,研究了所制备的钨钼混配型杂多酸盐在催化酯化反应时的活性和稳定性.通过正交试验[L9(3)4]对影响乙酸正丁酯收率的关键影响参数进行了优化,包括催化剂与反应物的质量比、反应时间和温度、以及正丁醇与乙酸的摩尔比.结果表明:当反应时间为120 min,反应温度为90℃,催化剂用量为0.4 g,醇酸摩尔比为2∶1,酯化效果最好,达到93.24 wt%.A tungsten and molybdenum mixed heteropoly acid salt catalyst（Na 4SiMoW12O40·xH2O） is prepared by using Na2WO4·2H2O and Na2MoO4·2H2O as raw materials through the combination of nitric acid acidification and ether extraction technique. The resulting catalyst is characterized by X-ray fluorescence spectrometer （XRF） for the investigation of its elemental composition. The infrared spectroscopy （FTIR） is used to analyze its functional group structure. The thermogravimetric analysis （TGA） is used to study its thermal stability. The catalytic activity and stability of the tungsten and molybdenum mixed heteropoly acid salt catalyst are studied during the process of esterification reaction of butanol and acetic acid. The key reaction parameters that influence the yield of n-butyl acetate are optimized by employing an orthogonal experiment [L 9（3）4], including the mass loading of catalyst, reaction time and reaction temperature, as well as the molar ratio of butanol to acetic acid. Results show that esterification reaction effect of 93.24 wt%is obtained when the reaction time is 120 minutes, reaction temperature is 90 ℃and catalyst loading is 0.4 g with the molar ratio of butanol to acetic acid of being 2：1.

关 键 词：杂多酸盐 酯化反应 催化剂 钨钼 

分 类 号：TF111.52[冶金工程—冶金物理化学] O643.36[理学—物理化学]