华南理工大学学报(自然科学版) ›› 2019, Vol. 47 ›› Issue (5): 18-24,31.doi: 10.12141/j.issn.1000-565X.180253

• 化学化工 • 上一篇    下一篇

麦草碱木素在碱性离子液体[Bmim][OH]中的溶解机理

侯轶 张晓 刘超 李友明   

  1. 1. 华南理工大学 制浆造纸工程国家重点实验室,广东 广州 510640
  • 收稿日期:2018-05-31 修回日期:2018-10-22 出版日期:2019-05-25 发布日期:2019-04-01
  • 通信作者: 李友明( 1957-) ,男,教授,博士生导师,主要从事制浆造纸清洁生产技术、造纸化学品等的研究 E-mail:ymli3@scut.edu.cn
  • 作者简介:侯轶( 1973-) ,女,教授,博士生导师,主要从事工业废水处理、烟草薄片生产过程控制、生物质结构分析等的研 究.
  • 基金资助:
    国家重点科技攻关项目( 2017YFB0307901) ; 国家自然科学基金资助项目( 21476091) ; 广东省科技计划项目 ( 2015A020215009) ; 广东省佛山市科技规划项目( 2015AG10011) 

Dissolution Mechanism of Wheat Straw Alkaline Lignin in Alkaline Ionic Liquid [Bmim][OH]

 HOU Yi ZHANG Xiao LIU Chao LI Youming   

  1.  State Key Laboratory of Pulp and Paper Engineering,South China University of Technology,Guangzhou 510640,Guangdong,China
  • Received:2018-05-31 Revised:2018-10-22 Online:2019-05-25 Published:2019-04-01
  • Contact: 李友明( 1957-) ,男,教授,博士生导师,主要从事制浆造纸清洁生产技术、造纸化学品等的研究 E-mail:ymli3@scut.edu.cn
  • About author:侯轶( 1973-) ,女,教授,博士生导师,主要从事工业废水处理、烟草薄片生产过程控制、生物质结构分析等的研 究.
  • Supported by:
     Supported by the National Key Scientific and Technological Project( 2017YFB0307901) ,the National Natural Science Foundation of China( 21476091) and the Science and Technology Planning Project of Guangdong Province( 2015A020215009)

摘要: 对麦草碱木素在强碱性离子液体[Bmim][OH]溶解过程中木质素的结构变化进 行了解析,并对溶解机理进行了探讨. 利用微波加热辅助溶解,实验条件如下: 微波功率 500 W,温度 90 ℃,反应时间 30 min,固液比 1∶ 10. 通过傅里叶变换红外光谱( FT-IR) 、凝 胶渗透色谱( GPC) 、元素分析、二维异质单量子相干核磁共振( 2D HSQC NMR) 、瞬时高温 热解装置 - 气相色谱 - 质谱联用( Py-GC-MS) 等方法进行分析和表征. 研究结果表明: 碱 木素在[Bmim][OH]离子液体溶解过程中其芳香环结构保持稳定,主要发生了侧链取代 或单元连接间含氧基团的脱除,溶解后再生的木质素相对分子质量轻微下降,分子量分布 更加均匀; 同时,再生木质素的不饱和度增大,这是由于溶解过程中发生了脱水反应. 二维 核磁共振光谱与 Py-GC-MS 分析表明,在强碱性离子液体体系中木质素的溶解过程以大 分子中 β-O-4'键的断裂最为明显,β-β、β-5 次之,S /G 比例明显降低. 文中成果为碱木素高 值化应用的相关理论和产品开发提供了基础数据和技术方向.

关键词: 碱木素, 碱性离子液体, 溶解机理

Abstract: This paper deals with the structure variation of wheat straw alkali lignin in alkaline ionic liquid [Bmim] [OH]and the dissolution mechanism of alkali lignin. The dissolution was assisted by microwave heating with a microwave power of 500 W,a temperature of 90 ℃,a reaction period of 30 min and a solid-to-liquid ratio of 1∶10. By using [Bmim] [OH]ionic liquid as a solvent,the lignin dissolution process was characterized and analyzed by means of FT-IR,GPC,elemental analysis,2D HSQC NMR and Py-GC-MS. The results indicate that,during the dissolution of alkali lignin in ionic liquid [Bmim][OH],the aromatic rings remains stable and there mainly occurs the substitution of the side chain or the removal of oxygen-containing groups; and that,after the dissolution,the relative molecular mass of the regenerated lignin slightly decreases,the molecular mass distribution become more uniform and the degree of unsaturation increases due to the dehydration reaction during the dissolution processes. Moreover,2D HSQC NMR and Py-GC-MS results prove that there mainly happens the cleavage of β-O-4' aryl ether linkages during the dissolution of lignin in strongly basic ionic liquid system,followed by β-β and β-5 structures,and the S /G ratio remarkably decreases. This research provides basic data and an approach to the development of relevant theories and the application of high-value alkali lignin

Key words: dissolutionalkaline lignin, alkaline ionic liquid, dissolution mechanism

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