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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 dioxide nanotubes synthesized by hydrothermal method were used as supports, and reacted with 3-mercaptopropyltrimethoxysilane and hydrogen peroxide to prepare functionalized titanium nanotubes (TNTs-SO 3 H) catalyst. XRD, FTIR, TEM , TG, UV-Vis and Hammett indicator method were used to characterize and test the structure and performance of the catalyst. Catalytic synthesis of n-butyl levulinic acid probe reaction, investigated TNTs-SO_3H catalytic properties. The results showed that when the dosage of n (levulinic acid): n (n-butanol) = 1: 5, the amount of TNTs-SO 3 H 3 was 10% of levulinic acid, the reaction temperature was 120 ℃ and the reaction time was 4 h, The yield of butyl ester reached 86.5%. After repeated use of TNTs-SO_3H for 7 times, the yield of n-butyl levulinic ester still reached 81.2%.