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Polymer-based solid acid catalyst for the green production of diosgenin
Journal of Applied Polymer Science ( IF 2.7 ) Pub Date : 2021-09-13 , DOI: 10.1002/app.51596 Hui Yuan 1 , Xuejun Yu 2 , Wenxiu Jiang 1 , Bowei Shen 1 , Farong Zhang 1 , Zhiquan Pan 1, 2 , Hong Zhou 1
Journal of Applied Polymer Science ( IF 2.7 ) Pub Date : 2021-09-13 , DOI: 10.1002/app.51596 Hui Yuan 1 , Xuejun Yu 2 , Wenxiu Jiang 1 , Bowei Shen 1 , Farong Zhang 1 , Zhiquan Pan 1, 2 , Hong Zhou 1
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In this study, a novel polymer-based solid acid catalyst was prepared by free radical polymerization of N, N′-methylenebisacrylamide (MBA) and allyl sodium sulfonate (SAS), followed by acidifying of diluted hydrochloric acid. The prepared solid acid was fully characterized by FTIR, solid-state 13C-NMR, TGA, XPS, element analysis, and SEM. In addition, the prepared solid acid poly(MBA-SAA) was used as a catalyst to extract diosgenin from Dioscorea zingiberensis C.H.Wright (DZW) under solvethermal condition using ethanol as a solvent. And the optimal conditions of temperature (104.02°C), alcoholysis time (5.87 h) and solid acid dosage (0.39 g), were obtained by response surface analysis based on the results of single factor experiments. The yield of diosgenin (14.53%) obtained in the alcoholysis is higher than that of the traditional sulfuric acid hydrolysis method. The alcoholysis products were analyzed by high performance liquid chromatography-mass spectrometry (LC–MS) and UV–vis, respectively. The results showed that the solid acid with higher catalytic activity and good reusability can replace sulfuric acid to extract diosgenin, which has a great potential for the clean production of diosgenin in industry.
中文翻译：
用于绿色生产薯蓣皂苷元的聚合物基固体酸催化剂
本研究通过N,N'-亚甲基双丙烯酰胺（MBA）和烯丙基磺酸钠（SAS）的自由基聚合，然后用稀盐酸酸化制备了一种新型聚合物基固体酸催化剂。通过FTIR、固态13 C-NMR、TGA、XPS、元素分析和SEM对制备的固体酸进行了充分表征。此外,以制备的固体酸聚(MBA-SAA)为催化剂从薯蓣中提取薯蓣皂苷元CHWright (DZW) 在溶剂热条件下使用乙醇作为溶剂。并在单因素试验结果的基础上，通过响应面分析得到温度（104.02℃）、醇解时间（5.87 h）和固体酸用量（0.39 g）的最佳条件。醇解得到薯蓣皂苷元的收率（14.53%）高于传统硫酸水解法。醇解产物分别通过高效液相色谱-质谱 (LC-MS) 和紫外-可见光进行分析。结果表明，具有较高催化活性和良好重复利用性的固体酸可替代硫酸提取薯蓣皂甙元，在工业上清洁生产薯蓣皂甙元具有很大潜力。
更新日期：2021-11-01
中文翻译：
用于绿色生产薯蓣皂苷元的聚合物基固体酸催化剂
本研究通过N,N'-亚甲基双丙烯酰胺（MBA）和烯丙基磺酸钠（SAS）的自由基聚合，然后用稀盐酸酸化制备了一种新型聚合物基固体酸催化剂。通过FTIR、固态13 C-NMR、TGA、XPS、元素分析和SEM对制备的固体酸进行了充分表征。此外,以制备的固体酸聚(MBA-SAA)为催化剂从薯蓣中提取薯蓣皂苷元CHWright (DZW) 在溶剂热条件下使用乙醇作为溶剂。并在单因素试验结果的基础上，通过响应面分析得到温度（104.02℃）、醇解时间（5.87 h）和固体酸用量（0.39 g）的最佳条件。醇解得到薯蓣皂苷元的收率（14.53%）高于传统硫酸水解法。醇解产物分别通过高效液相色谱-质谱 (LC-MS) 和紫外-可见光进行分析。结果表明，具有较高催化活性和良好重复利用性的固体酸可替代硫酸提取薯蓣皂甙元，在工业上清洁生产薯蓣皂甙元具有很大潜力。
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