磺酸功能化钛纳米管催化合成乙酰丙酸正丁酯  

Sulfonic Acid-Functionalized Titanium Oxide Nanotubes as a Solid Acid Catalyst for Synthesis of n-Butyl Levulinate

作　　者：周硕林[1,2] 刘贤响[2] 徐琼[2] 李家其[1] 蒋达波 丁慧[2] 尹笃林[2] 

机构地区：[1]长沙师范学院基础实验中心,湖南长沙410100 [2]石化新材料与资源精细利用国家地方联合工程实验室湖南师范大学化学化工学院,湖南长沙410081

出　　处：《精细化工》2017年第8期875-879,共5页Fine Chemicals

基　　金：国家自然科学基金(21606082);湖南省自然科学基金(2016JJ6002);湖南省教育厅科学研究项目(14A105;16C0114);长沙师范学院一般项目(XYYB201522)~~

摘　　要：以水热法合成的二氧化钛纳米管为载体,将其与3-巯丙基三甲氧基硅烷、双氧水反应,制备了磺酸功能化钛纳米管催化剂(TNTs-SO_3H),采用XRD、FTIR、TEM、TG、UV-Vis及Hammett指示剂法对催化剂的结构和性能进行了表征与测试。以催化合成乙酰丙酸正丁酯为探针反应,考察了TNTs-SO_3H的催化性能。结果表明:当n(乙酰丙酸)∶n(正丁醇)=1∶5、TNTs-SO_3H用量为乙酰丙酸质量的10%、反应温度120℃、反应时间4 h时,乙酰丙酸正丁酯的收率可达86.5%,TNTs-SO_3H重复使用7次后,乙酰丙酸正丁酯收率仍达81.2%。Titanium oxide nanotubes were prepared by a hydrothermal synthesis method,and then were used as carriers to react with 3-mercaptopropyl trimethoxysilane. Subsequently, the above-prepared intermediate was oxidized with hydrogen peroxide to afford sulfonic acid-functionalized titanium dioxide nanotubes （TNTs-SO3H）. The obtained TNTs-SO3H was characterized by XRD, FTIR, TEM, TG and Hammett analysis techniques. The catalytic performance of TNTs-SO3H was investigated by esterification reaction of levulinic acid with n-butyl alcohol. The experiment results revealed that the TNTs-SO3 H catalyst exhibited high catalytic activity, and the yield of n-butyl levulinate reached 86. 5 % under the following conditions ： n （ levulinic acid） ： n （ n-butyl alcohol） = 1：5, dosage of catalyst was 10% （based on mass of levulinic acid）, at 120 ℃ for 4 h. In addition,the yield of target product still reached 81.2% even if the catalyst was recycled for 7 times.

关 键 词：钛纳米管 固体酸催化剂 磺酸功能化 乙酰丙酸正丁酯 酯化 催化与分离提纯技术 

分 类 号：O643.32[理学—物理化学]