摘要
以香茅醇与乙酸酐为原料,以NaHSO4·SiO2为负载型固体催化剂,采用微波辐射的方式绿色合成乙酸香茅酯.分别考察催化剂中NaHSO4的质量分数、反应时间、原料用量比、催化剂用量、反应温度、微波辐射功率等因素对酯收率的影响,并采用傅里叶变换红外光谱(FT-IR)和核磁共振氢谱(1 H NMR)确定产物的结构.结果表明:合成乙酸香茅酯的最佳条件为NaHSO4质量分数为40%,n(酸酐)∶n(醇)=1.4∶1,反应时间为9min,催化剂用量为底物的20%,反应温度为70℃,微波辐射功率为480W,产品收率为98.3%.此外,研究表明NaHSO4·SiO2催化剂循环使用4次,仍然显示出一定的催化活性.
Citronellyl acetate was synthesized from citronellol and acetic anhydride by using NaHSO4 · SiO2 as supported catalyst and under microwave radiation condition. And the optimum reaction conditions such as the loading of NaHSO4 on SiO2, the time of microwave radiation, the ratio of the feeds, the quantity of the catalyst, the reaction temperature and the power of microwave radiation were studied. The results showed that the optimum technological conditions were as following： the loading of NaHSO4 40%, the ration of acetic anhydride and citronellyl 1.4 ： 1, the radiation time 9 minutes, the quantity of catalyst 20%, the reaction temperature 70 ℃, the microwave power 480 W. Under the optimum conditions, the yield of the citronellyl acetate was up to 98. 3 %. The structure of citronellyl acetate was characterized by FT-IR and 1 H NMR spectra. Furthermore, NaHSO4·SiO2 could be recycled and reused at least 4 times and still displayed sat- isfied catalytic activity.
出处
《华侨大学学报（自然科学版）》
CAS
北大核心
2014年第1期47-51,共5页
Journal of Huaqiao University(Natural Science)
基金
福建省教育厅A类科研基金资助项目(JA12007)
华侨大学实验改革与建设基金资助项目(2009年度)
