有机化学 ›› 2016, Vol. 36 ›› Issue (6): 1438-1443.DOI: 10.6023/cjoc201511015 上一篇    下一篇

研究简报

微波辅助SnCl4/H2SO4二元体系催化纤维素醇解制备乙酰丙酸甲酯

黄耀兵, 杨涛, 刘安凤, 周新成, 潘晖   

  1. 南京林业大学化学与工程学院南京 210037
  • 收稿日期:2015-11-09 修回日期:2015-12-28 发布日期:2016-02-01
  • 通讯作者: 黄耀兵, 潘晖 E-mail:hyb@njfu.edu.cn;hpan@njfu.edu.cn
  • 基金资助:

    国家自然科学基金(No.21502095)、江苏省自然科学基金(No.BK20150872)和江苏省生物质绿色燃料和化学品重点实验室开放基金(No.14003)资助项目.

Microwave-Assisted Alcoholysis of Cellulose to Methyl Levulinate Catalyzed by SnCl4/H2SO4

Huang Yaobing, Yang Tao, Liu Anfeng, Zhou Xincheng, Pan Hui   

  1. College of Chemical and Engineering, Nanjing Forestry University, Nanjing 210037
  • Received:2015-11-09 Revised:2015-12-28 Published:2016-02-01
  • Supported by:

    Project supported by the National Natural Science Foundation of China (No. 21502095), the Natural Science Foundation of Jiangsu Province (No. BK20150872) and the Opening Fund from Jiangsu Key Laboratory of Biomass-based Green Fuels and Chemicals (No. 14003).

主要研究了在微波条件下, 金属盐-酸混合二元体系催化纤维素醇解制备乙酰丙酸甲酯的反应. 在SnCl4和H2SO4的协同作用下, 纤维素被高效转化, 获得了61.5%的乙酰丙酸甲酯的产率. 考察了催化剂比例、反应时间和反应温度等参数对反应产率和选择性的影响, 研究了水的加入对于反应的促进作用. 同时, 将该体系应用到多种生物质原料(如蔗糖、淀粉和菊粉等)转化为乙酰丙酸甲酯的反应中, 取得了48%~60%的产率. 催化剂经过5次的连续回收和重复使用, 依然保持了良好的催化活性.

关键词: 纤维素, 乙酰丙酸甲酯, 微波辐射, 醇解反应

Microwave irradiation technology was used to assist the conversion of cellulose to methyl levulinate (ML) in methanol solution in the presence of mixed catalysts. The reactions were carried out in a microwave reactor and cellulose was rapidly converted into ML with a highest yield of 61.5% by the use of SnCl4/H2SO4 as catalyst. The catalysts ratios, reaction time and reaction temperature were optimized and found to have great influences on both the ML product yield and the selectivity. Besides, an appropriate amount of water, which may participate the breakage of the glucosidic bond of cellulose, is highly desirable for the full conversion of cellulose. Several other biomass derived carbohydrates such as starch, sucrose and inulin were also tested in the optimized system and 48%~60% ML yields were achieved. Finally, the mixed catalysts can be recycled and reused for at least five times without much decrease in catalytic activity.

Key words: cellulose, methyl levulinate, microwave irradiation, alcoholysis