天然产物研究与开发 ›› 2018, Vol. 30 ›› Issue (10): 1776-1781.doi: 10.16333/j.1001-6880.2018.10.020

• 开发研究 • 上一篇    下一篇

温和酸催化解聚木质素磺酸盐产物的分离与分析

方红霞1*,崔朋1,2,钱晨1,刘京凤1,刘同欢1,李丹丹1,胡小坡1   

  1. 1黄山学院应用化学研究所;2黄山学院分析测试中心,黄山 245041
  • 出版日期:2018-10-31 发布日期:2018-11-01
  • 基金资助:

    安徽省教育厅自然科学项目(KJHS2015B15);黄山学院科研启动项目(2015XKJQ006);安徽省创客实验室项目(2016ckjh190)

Products Separation and Analysis of Depolymerized Lignosulfonate under Mild Acid-catalyzed Conditions

FANG Hong-xia1*,CUI Peng1,2,QIAN Chen1,LIU Jin-feng1,LIU Tong-huan1,LI Dan-dan1,HU Xiao-po1   

  1. 1Applied Chemistry Laboratory of Huangshan University;2Analysis and Test Center of Huangshan University,Huangshan 245041,China
  • Online:2018-10-31 Published:2018-11-01

摘要: 木质素解聚产物是异常复杂的混合物体系,本文以温和酸催化条件下的木质素磺酸盐解聚产物为研究对象,建立分离和分析测试木质素磺酸盐解聚产物和解聚效率的有效方法。采用超高效凝胶渗透色谱对解聚产物实现了高效分离,结果表明木质素磺酸盐高分子获得了高效解聚,解聚获得的产物分子量组成主要分布在三个低聚物区间;采用GC-MS鉴定了主要的木质素基单酚和双酚类官能团化合物9种,约占解聚液的30 wt%,表明解聚产物中含有大量的单体化合物;采用SEM和EDS分析测试木质素解聚后残渣,其结果也进一步证实了在温和酸催化条件下,木质素磺酸盐在解聚过程中还原位脱除了磺酸盐。木质素磺酸盐由于具有特有的Cα-SO3M基团,在酸催化条件下β-O-4键易于断裂,促进了木质素磺酸盐快速解聚,获得了解聚效率达95 wt%以上的解聚产物。

关键词: 木质素磺酸盐, 酸催化解聚, 产物分析, 木质素基酚类化合物

Abstract: Depolymerized lignin products are very complex mixtures.In this paper,based on depolymerization solution of commercially available sodium lignosulfonate under mild conditions,an efficient method for separation and analysis of depolymerized lignin products and evaluation of the yields of reaction products has been developed.The GPC result indicated that lignosulfonate was almost completely converted into small molecules,which mainly dispersed in three oligomer ranges.9 of depolymerized aromatics products accounted for 30 wt% of depolymerized solution are identified by GC-MS.The study also indicated that under these mild conditions lignosulfonate was completely depolymerized,while its sulfonate functional groups were removed easily in situ to form salts,which were confirmed with SEM and EDS energy spectrum.Preliminary studies highlight that the secondary sulfo group (Cα-SO3M) within real lignin help to promote alkyl aryl ether bond (β-O-4) cleavage,thus facilitated the lignin depolymerization reaction.Depolymerized products in high yields of more than 95 wt% were obtained.

Key words: lignosulfonate, acid-catalyzed depolymerization, products analysis, lignin-based aromatic compounds

中图分类号: 

O63