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

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.