磺酸功能化离子液体催化制备薯蓣皂苷元研究

Study on Catalytic Preparation of Diosgenin by Sulfonic Acid-Functionalized Ionic Liquid

目的:探索磺酸功能化离子液体1-磺丁基-3-甲基咪唑三氟甲烷磺酸盐([BHSO_(3)MIm]CF3SO_(3))作为催化剂在薯蓣皂苷元制备中的应用。方法:以盾叶薯蓣提取粗皂苷为原料、[BHSO_(3)MIm]CF3SO_(3)为催化剂,水解制备薯蓣皂苷元。通过单因素试验对反应温度、反应时间、离子液体用量、溶剂体积进行考察,采用响应面分析方法进一步优化反应条件,确定最佳反应条件。进行12次循环实验,考察该离子液体循环使用性能。结果:最佳反应条件为反应温度100℃、反应时间5.17 h、离子液体用量2.56 g、水溶剂体积6 mL,在该条件下薯蓣皂苷元产率为12.99%。该离子液体循环6次时,循环效率为82.70%,循环10次时循环效率降至58.12%。结论:在薯蓣皂苷元制备过程中,[BHSO_(3)MIm]CF3SO_(3)作为酸催化剂,表现出了水解效率高、性能稳定、易于回收、循环使用性能良好等优势,具备较强的应用前景。

Objective:To explore the application of the sulfonic acid-functionalized ionic liquid[BHSO_(3)MIm]CF3SO_(3) as a catalyst in the preparation of diosgenin.Methods:Crude saponins extracted from Dioscorea zingiberensis were used as raw materials.With[BHSO_(3)MIm]CF3SO_(3) as a catalyst,diosgenin was prepared by hydrolysis.The reaction temperature,reaction time,amount of ionic liquid,and volume of solvent were investigated by single factor test.The reaction conditions were further optimized by response surface analysis to determine the optimal reaction conditions.The recycling performance of the ionic liquid was investigated by 12 cycles of experiments.Results:The optimal reaction condition was as follows:reaction temperature at 100°C,reaction time of 5.17 h,ionic liquid amount of 2.56 g,and solvent of 6 mL.Under these condition,the yield of diosgenin was 12.99%.When the ionic liquid was tested six times,the cycling efficiency was still as high as 82.70%and decreased to 58.12%when the ionic liquid was tested 10 times.Conclusion:In the preparation process of diosgenin,[BHSO_(3)MIm]CF3SO_(3),as an acid catalyst,has the advantages of high hydrolysis efficiency,stable performance,easy recovery,and good recycling performance,and it has a strong application prospect.