硅藻土复合型固体酸的研制及其催化合成异丁酸丁酯.pdfVIP

学兔兔 石 油 化 工 2010年第39卷第2期 PETROCHEMICAL TECHNOL0GY ·157· 硅藻土复合型固体酸的研制及其 催化合成异丁酸丁酯 陈丹云，王树立，何建英 (河南大学 精细化学与工程研究所，河南 开封 475004) [摘要]制备了硅藻土复合型固体酸催化剂，采用XRD和TG方法对催化剂进行了表征；并将该催化剂用于异丁酸与正丁醇进行 酯化反应合成异丁酸丁酯，考察了催化剂制备条件(焙烧温度和浸渍液硫酸浓度)、催化剂用量、n(正丁醇)：n(异丁酸)、反应时 间、带水剂种类等因素对酯化率的影响。实验结果表明，催化剂的适宜制备条件为：m(SnC1 ·5H：O)：rn(硅藻土)=1：3、硫酸 浓度3．0 moVL、焙烧温度550℃、焙烧时间3．5 h。该催化剂催化合成异丁酸丁酯的适宜反应条件为：n(正丁醇)：n(异丁酸)= 1．8、催化剂用量为反应物总质量的1．10％、带水剂环己烷用量10 mL、反应时间2．5 h。在此条件下，酯化率为98．3％。该催化剂 使用8次后，酯化率仍可达到92．7％。 [关键词]硅藻土复合型固体酸催化剂；正丁醇；异丁酸；异丁酸丁酯；酯化 [文章编号]1000—8144(2010)02—0157—05 [中圈分类号]TQ 225．24 [文献标识码]A Composite Diatomite-Solid Acid Catalyst for Synthesis of Butyl-Isobutyrate Chen Danyun，Wang Shuli，He Jianying (Institute of Fine Chemistry and Engineering，Henan University，Kaifeng Henan 475004，China) [Abstract]A composite diatomite—solid acid catalyst was prepared and characterized by means of XRD and TG．Butyl—isobutyrate was synthesized through esterification of isobutyric acid with n-butanol over the prepared catalyst．The effects of the catalyst preparation conditions(calcination temperature and sulfuric acid concentration)，catalyst dosage，mole ratio of n—butanol to isobutyric acid，reaction time and water entrainer type on the esterification rate were investigated．The results indicated that suitable conditions for the catalyst preparation were：mass ratio of SnCI4·5 H2 O to diatomite 1：3， sulfuric acid concentration 3．0 mol／L and calcination at 550 oC for 3 ． 5