华南理工大学学报(自然科学版) ›› 2016, Vol. 44 ›› Issue (6): 14-20,26.doi: 10.3969/j.issn.1000-565X.2016.06.003

• 化学化工 • 上一篇    下一篇

新型深度共熔溶剂选择性分离木质素的研究

常杰 刘钧 郭姝君 王曦 付严   

  1. 华南理工大学 化学与化工学院,广东 广州 510640
  • 收稿日期:2015-12-07 修回日期:2016-01-05 出版日期:2016-06-25 发布日期:2016-05-03
  • 通信作者: 常杰(1968-),男,教授,博士生导师,主要从事生物基材料与能源研究. E-mail:changjie@scut.edu.cn
  • 作者简介:常杰(1968-),男,教授,博士生导师,主要从事生物基材料与能源研究.
  • 基金资助:
    国家自然科学基金资助项目(21476090);国家重点基础研究发展计划(973 计划)项目(2013CB228104);华南理工大学中央高校基本科研业务费专项资金资助项目

Investigation into Selective Separation of Lignin in Novel Deep Eutectic Solvent

CHANG Jie LIU Jun GUO Shu-jun WANG Xi FU Yan   

  1. School of Chemistry and Chemical Engineering,South China University of Technology,Guangzhou 510640,Guangdong,China
  • Received:2015-12-07 Revised:2016-01-05 Online:2016-06-25 Published:2016-05-03
  • Contact: 常杰(1968-),男,教授,博士生导师,主要从事生物基材料与能源研究. E-mail:changjie@scut.edu.cn
  • About author:常杰(1968-),男,教授,博士生导师,主要从事生物基材料与能源研究.
  • Supported by:
    Supported by the National Natural Science Foundation of China(21476090)and the National Program on Key Basic Research Project of China(973 Program)(2013CB228104)

摘要: 近年来,以胆碱类为代表的生物基离子液体作为木质素的优良溶剂逐渐受到广泛关注. 文中基于 Hansen 溶解理论,设计出一种分别以乳酸(LA)和氯化胆碱(ChCl)为氢键供受体的新型离子液体———深度共熔溶剂(DES)作为木质素分离的溶剂. 通过实验考察了常压下 ChCl/LA 摩尔比、温度、时间对木质素溶解效果的影响,确定了最佳工艺条件为 ChCl/LA 摩尔比1∶ 9、温度90℃、时间12h,此时木质素的溶解率达90. 1%,再生木质素纯度为 96. 3%.紫外可见光谱(UV)及红外光谱(FT-IR)分析表明木粉中木质素经 DES 处理后被大量脱除;X 射线衍射分析表明经预处理后的木粉中纤维素结构基本未被破坏;核磁共振谱( 13C NMR)分析表明再生木质素由紫丁香基、愈创木基及少量对羟苯基结构单元组成;离子色谱分析结果表明该混合溶液中的综纤维素只有少量发生溶解.

关键词: 木质素, 深度共熔溶剂, 氯化胆碱;乳酸, Hansen 参数

Abstract: In recent years,choline,a novel kind of bio-based ILs (Ionic Liquids) used as a good lignin solvent,has been paid more and more attention to.In this paper,based on Hansen's theory of solubility,a novel ionic liquid analogue named DES (Deep Eutectic Solvent),in which lactic acid (LA) and choline chloride (ChCl) were respectively used as the donor and the acceptor of hydrogen bonds,was designed to separate lignin.Then,the dissolution results of lignin affected by the molar ratio of ChCl to LA,the reaction temperature and the interaction time were investigated by experiments.It was found that the dissolution rate of lignin reached the optimal 90. 1% and the purity of regenerated lignin reached 96. 3% at a ChCl-to-LA molar ratio of 1∶ 9,a reaction temperature 90℃ and a reaction duration of 12 h.The results of UV-Vis spectroscopy and FT-IR spectroscopy show that the lignin in the wood powders is greatly removed after DES treatment.XRD results show that the structure of cellulose in the pretreated wood powders is barely damaged.13C NMR results indicate that the regenerated lignin is mainly composed of syringyl,guaiacyl and a little p-hydroxylphengl.Moreover,ion chromatography results show that only a small amount of holocellulose is dissolved in the mixed solution.

Key words: lignin, deep eutectic solvent, choline chloride, lactic acid, Hansen parameter