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机构地区:[1]齐齐哈尔大学化学与化工学院,黑龙江齐齐哈尔161006
出 处:《化学工业与工程技术》2012年第6期22-26,共5页Journal of Chemical Industry & Engineering
摘 要:采用直接合成法合成K6[MnCu(H2O)W11O39],K5[MnFe(H2O)W11O39],K6[MnCo(H2O)W11O39],K6[MnZnH2(O)W11O39],K6[MnNi(H2O)W11O39],K6[MnCd(H2O)W11O39]等6种过渡金属取代的钨锰杂多酸盐,利用红外光谱、紫外光谱对合成产物的结构进行了表征。结果表明,6种杂多阴离子具有Keggin结构。利用酯化反应考察了所合成催化剂的催化活性,并且确定了最佳催化反应条件:酸醇物质的量比1∶1,催化剂用量占原料总量的1.5%,反应时间4h,反应温度控制在120℃。结果表明,过渡金属取代钨锰三元杂多酸对乙酸正丁酯的催化产率95%以上。Six kinds of transition metal substituted tungstomangaous heteropoly acids with Keggin structure such as K6[MnCu(H2O)W11O39], K5[MnFe(H2O)Wn039], K5[MnCo(H2O)W11039], K6[MnZnH2(O)W11O339], K6[MnNi(H2O)WH039], K6[MnCd(H2O) W11O39]are synthesized by direct synthesis technology and structures are characterized by IR and UV. The results show that the com- pounds have Keggin structure. The catalytic activity is investigated by esterification and the optimum reaction conditions are obtained as following: the molar ratio of acetic acid to n-butanol is 1:1, the dosage of catalyst is 1.5% of the materials gross, the reaction temperature is 120℃ and the reaction time is 4 h. Under the optimum conditions, the yield of n-butyl acetate is more than 95%.
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