作　　者： ; ; ; ;

机构地区： 上海应用技术学院化学与环境工程学院化学工程系

出　　处： 《石油化工高等学校学报》 2007年第1期5-8,共4页

摘　　要： 分别以氧氯化锆、硅溶胶和氨水为锆源、硅源和沉淀剂,采用共沉淀法制备Zr(OH)4-Si(OH)4,110℃干燥后经硫酸浸渍、干燥和焙烧制得SO42-/ZrO2-SiO2固体超强酸。XRD和比表面积测定结果表明,SiO2的引入对SO42-/ZrO2催化剂的结构产生了重要影响,从而使其比表面积明显增大。以所制备的SO42-/ZrO2-SiO2固体超强酸为催化剂,代替浓硫酸用于丁酸和丁醇的酯化反应,考察了硫酸浸渍液浓度、焙烧温度等制备条件对其催化性能的影响。结果表明,采用硫酸浸渍液浓度为1.0 mol/L,焙烧温度为550℃所制备的SO42-/ZrO2-SiO2催化剂,在丁醇和丁酸的物质的量比为1.2及不添加任何带水剂的条件下,丁酸丁酯的收率高达90%以上,优于SO42-/TiO2-WO3和TiSi W12O40/TiO2催化剂。 A solid superacid catalyst, SO4^2-/ZrO2-SiO2, was prepared by impregnating the Zr（OH）4 -Si（OH）4 coprecipitate with a sulfuric acid solution, then drying and calcinating, in which the Zr（OH）4 -Si（OH）4 coprecipitate was prepared with zirconium oxychloride as zirconia sources, silica solution as silica sources and aqueous ammonia as precipitant, respectively, then drying at 110℃. The results from XRD and surface area measurements indicate that the addition of SiO2 strongly changes the structure of SO4^2-/ZrO2hence greatly increases its surface area. The effect of preparation conditions such as concentration of sulfuric acid and calcination temperature on the catalytic performance of SO4^2-/ZrO2-SiO2 substituted for sulfuric acid for the esterification of n--butanoic acid with n--butyl alcohol was studied. The results show that the yield of butyric butyl using the SO4^2-/ZrO2-SiO2 catalyst prepared with the concentration of H2SO4 by 1.0 mol/L and the calcination temperature of 550 ℃ is higher than 90 % when the molar ratio of butyl alcohol to butanoic acid is 1.2 ： 1 and without addition of entrainer, which is superior to the reported results obtained using SO4^2-/ZrO2-WO3 and TiSiW12 O40/TiO2 catalysts under comparable experiments.

关 键 词： 固体超强酸 丁酸丁酯

领　　域： [理学] [理学]