SO_4^(2-)改性的锆交联黏土固体酸催化合成柠檬酸三丁酯  

Synthesis of Tributyl Citrate Catalyzed by SO_4^(2-) Modified Zirconium Cross-linked Clay Solid Acid

作　　者：付丽华[1] 郭锡坤[1] 林绮纯[1] 李俊[1] 

机构地区：[1]汕头大学化学系,广东汕头515063

出　　处：《精细化工》2002年第1期28-31,共4页Fine Chemicals

基　　金：广东省教育厅自然科学研究资助项目 ( 2 0 0 0 6 4) ;汕头市重点科技计划资助项目 ;汕头大学工业催化"2 11工程"建设资助项目~~

摘　　要：制备了SO4 2 -改性的锆交联黏土固体酸催化剂 (A) ,用于柠檬酸 (B)和正丁醇 (C)的酯化反应 ,与浓硫酸 ,钠基膨润土和锆交联黏土作催化剂的情况相比 ,SO4 2 -改性的锆交联黏土作催化剂时柠檬酸的转化率和产物的纯度更高。同时考察了催化剂用量w(A)、酸醇量比n(B)∶n(C)、反应时间 (t)、反应温度 (θ)对其催化合成柠檬酸三丁酯 (D)的影响 ,并对合成的产物进行红外光谱分析及气相色谱分析。实验结果表明 :SO4 2 -改性的锆交联黏土固体酸催化柠檬酸与正丁醇的酯化反应的最佳反应条件为 :反应温度为 15 0℃ ,n(B)∶n(C) =1∶4,反应时间 3 .5h ,催化剂用量占反应投料总质量的百分比w(A) =1.2 % ,柠檬酸的转化率达 96 .6 0 % ,反应产物柠檬酸三丁酯的质量分数w(D) >99 0 0 %The catalyst of zirconium cross linked clay solid acid modified by SO 4 2- (A) was prepared and applied to the esterification reaction of citric acid (B) and butanol (C). Conversion of citric acid and purity of tributyl citrate catalyzed by A were the highest among those catalyzed by sulfuric acid of high concentation, Na bentonite, zirconium cross linked clay and A. The effect of reaction conditions such as quantity of catalyst w (A), mole ratio n (B)∶ n (C), reaction temperature and reaction time on the conversion of citric acid were studied. The product was analyzed by IR and GC.The experimental results show that in the presence of SO 4 2- modified zirconnium cross linked clay solid acid, the optimum esterification conditions are that the reaction temperature is 150 ℃, the reaction time is 3.5 h, n (B)∶ n (C) is 1∶4,and w (A) is 1.2% based on the total mass of initial materials. Conversion of citric acid amounts to 96.60% and the purity of tributyl citrate is over 99 00%.

关 键 词：锆交联黏土 柠檬酸三丁酯 酯化 固体酸 催化合成 

分 类 号：TQ426.99[化学工程] TQ225.41