硅藻土负载对甲苯磺酸催化合成乙酸正丁酯  

Study on synthesis of n-butyl acetate catalytic by diatomite load p-toluenesulfonic acid

作　　者：周德志[1] 曹小华[1,2] 占昌朝 林旭嫔[1] 雷艳虹 ZHOU De-zhi;CAO Xiao-hua;ZHAN Chang-chao;LIN Xu-ping;LEI Yan-hong(College of Chemical and Environmental Engineering,Jiujiang University,Jiujiang 332005,Jiangxi Province,China;Jiangxi Provincial Engineering Research Center of Ecological Chemical Industry,Jiujiang 332005,Jiangxi Province,China)

机构地区：[1]九江学院化学与环境工程学院,江西九江332005 [2]江西省生态化工工程技术研究中心,江西九江332005

出　　处：《化学工程》2020年第2期52-56,共5页Chemical Engineering(China)

基　　金：国家自然科学基金资助项目(21864015,51562016);江西省自然科学基金资助项目(20171BAB206015)。

摘　　要：以对甲苯磺酸为活性组分,硅藻土为载体,通过浸渍法制备出硅藻土负载对甲苯磺酸催化剂(p-CH3C6H4SO3H/硅藻土),对催化剂进行FT-IR、XRD、EDS、SEM表征。以p-CH3C6H4SO3H/硅藻土为催化剂,催化乙酸与正丁醇液相合成乙酸正丁酯。采用正交试验考察催化剂用量、醇酸摩尔比、反应温度及反应时间对酯化率的影响。结果表明:硅藻土负载对甲苯磺酸可作为催化合成乙酸正丁酯的有效催化剂。在优化反应条件下,即对甲苯磺酸负载量为20%(占硅藻土的质量比),催化剂用量占反应物质量分数2.1%,醇酸摩尔比为2.5:1,反应温度为120℃,反应时间2.5 h,酯化率可达97.2%。催化剂重复利用5次,酯化率仍保持为84.5%。与传统浓硫酸催化酯化工艺相比,此工艺具有操作简单、绿色环保、重复使用性能好等优点,具有良好的工业开发价值。p-CH3C6H4SO3H/diatomite was prepared by impregnation method with p-CH3C6H4SO3H as active component and diatomite as carrier.The catalyst was characterized by FT-IR,XRD,EDS,SEM and applied in the catalytic synthesis of n-butyl acetate with acetic acid and n-butanol.The amount of p-CH3C6H4SO3H loading,catalyst amount,the molar ratio of n-butyl alcohol to acetic acid,reaction time,reaction temperature and repeated times of catalyst on the yield of n-butyl acetate were investigated.The results show that diatomite supported p-toluene sulfonic acid could be used as catalyst for the synthesis of n-butyl acetate.The highest yield of n-butyl acetate can reach 97.2% under the optimal reaction conditions,i.e.,the mass ratio of p-CH3C6H4SO3H to diatomite 20%,catalyst amount 2.1% of the total mass of reactant,the molar ratio of butanol to acetic acid 2.5,reaction temperature 120℃,and reaction time 2.5 h.The yield of n-butyl acetate remains above 84.5% after 5 cycles.The new technology has the advantages of simple operation,low manufacture cost,less environmental pollution and high quality of the product compared with the traditional sulfuric acid catalytic technology.Therefore it has good industry development value.

关 键 词：对甲苯磺酸 硅藻土 负载型催化剂 乙酸正丁酯 酯化 

分 类 号：TQ426.91[化学工程]