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林产化学与工业 ›› 2018, Vol. 38 ›› Issue (5): 107-114.doi: 10.3969/j.issn.0253-2417.2018.05.015

• 研究报告 • 上一篇    下一篇

蔗渣硫酸盐木质素的分级分离与表征

贾转, 万广聪, 李明富, 罗斌, 王双飞, 闵斗勇   

  1. 广西大学 轻工与食品工程学院;广西清洁化制浆造纸与污染控制重点实验室, 广西 南宁 530004
  • 收稿日期:2018-04-23 出版日期:2018-10-25 发布日期:2018-11-06
  • 通讯作者: 闵斗勇,教授,博士生导师,从事木质纤维原料全组分高值化利用基础研究;E-mail:mindouyong@gxu.edu.cn。 E-mail:mindouyong@gxu.edu.cn
  • 作者简介:贾转(1992-),男,河南南阳人,硕士生,主要从事木质纤维原料高值化利用研究
  • 基金资助:
    中国博士后科学基金(2015M570419);华南理工大学制浆造纸工程国家重点实验室开放基金(2015-05-SKLPPE)

Fractionation and Characterization of Sugarcane Bagasse Kraft Lignin

JIA Zhuan, WAN Guangcong, LI Mingfu, LUO Bin, WANG Shuangfei, MIN Douyong   

  1. College of Light Industry and Food Engineering, Guangxi University;Guangxi Key Laboratory of Clean Pulp & Papermaking and Pollution Control, Nanning 530004, China
  • Received:2018-04-23 Online:2018-10-25 Published:2018-11-06

摘要: 从蔗渣制浆黑液中提取纯化硫酸盐木质素(KL),将KL溶解在甲醇/丙酮混合溶液后,通过有机溶剂(乙酸乙酯、乙酸乙酯/石油醚和石油醚)沉降分级分离木质素得到F1、F2、F3和F4这4个组分,再利用红外光谱、元素分析、凝胶渗透色谱、热重和核磁共振波谱等手段对原料以及F1、F2和F3组分进行表征。实验结果表明:F1、F2、F3和F4分别占硫酸盐木质素质量的59.6%、28.4%、10.8%和1.2%;与原料相比,F1相对分子质量(Mr)较高、均一性较好,F2~F4的Mr及分散系数均小于原料;从F1、F2到F3,甲氧基含量、羟基(醇羟基与酚羟基)含量以及结构单元间连接键比例均随木质素Mr的变化而变化,β-O-4'结构比例随Mr降低而减小, β-5'结构比例随Mr降低而增加。

关键词: 蔗渣, 木质素, 分级分离

Abstract: Kraft lignin(KL) of sugarcane bagasse extracted from bagasse pulping black liquor was successively fractionated into four fractions (e.g. F1, F2, F3 and F4) by various organic solvents (ethyl acetate, ethyl acetate/petroleum ether, and petroleum ether) according to their solubility. Kraft lignin and its three fractions(F1, F2 and F3) were comprehensively characterized by elemental composition analysis, gel permeation chromatography, Fourier transform infrared spectroscopy, and nuclear magnetic resonance including 31P, 13C, and 1H-13C HSQC NMR, respectively. The results indicated that F1, F2, F3 and F4 were respectively accounting for 59.6%, 28.4%, 10.8% and 1.2% of kraft lignin. Compared with the original kraft lignin, the molecular weight of F1 was higher and the homogeneity was better. The molecular weight and dispersity of lignin fractions F2 to F4 were smaller than those of original kraft lignin. Furthermore, the contents of methoxyl group, hydroxyl group, and inter-unit linkages, as well as the thermal properties of fractions (F1, F2, and F3), were varied with their molecular weights. The proportion of β-O-4' structure decreases with the decrease of molecular weight, and the proportion of β-5' increases with the decrease of molecular weight.

Key words: sugarcane bagasse, kraft lignin, fractionation

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