Jia Zhuan, Li Mingfu, Wan Guangcong, Luo Bin, Guo Chenyan, Wang Shuangfei, Min Douyong
College of Light Industry and Food Engineering, Guangxi University Nanning 530004 PR China
Guangxi Key Laboratory of Clean Pulp & Papermaking and Pollution Control Nanning 530004 PR China.
RSC Adv. 2018 Dec 19;8(74):42269-42279. doi: 10.1039/c8ra08595a.
The heterogeneous features of lignin, especially the wide distribution of its molecular weight, limit its high value-added application. To improve the homogeneity of lignin, sugarcane bagasse kraft lignin (KL) dissolved in methanol/acetone (7 : 3, v/v) was successively fractionated into four fractions (., 1, 2, 3, and 4) with various organic solvents of decreasing dissolving capacity (., ethyl acetate, ethyl acetate/petroleum ether 1 : 1 v/v, and petroleum ether). The yields of the four fractions (1, 2, 3, and 4) were 59.6, 28.4, 10.8, and 1.2% that of KL, respectively. Gel permeation chromatography (GPC) analysis indicated the molecular weight of each fraction decreased from 1 to 4. All fractions had a lower polydispersity than KL. KL and the fractions were comprehensively characterized by chemical composition analysis, elemental composition analysis (EA), methoxyl group analysis, Fourier transform infrared spectroscopy (FT-IR), nitrobenzene oxidation analysis (NBO), and nuclear magnetic resonance (NMR) including P and H-C HSQC NMR. The results showed that the methoxyl group, hydroxyl group, interunit linkages, and thermal properties of the fractions varied with the molecular weight. The homogeneity of lignin was improved through solvent fractionation.
木质素的异质性特征,尤其是其分子量的广泛分布,限制了其高附加值应用。为了提高木质素的均匀性,将溶解于甲醇/丙酮(7∶3,v/v)的甘蔗渣硫酸盐木质素(KL)先后用溶解能力逐渐降低的各种有机溶剂(如乙酸乙酯、乙酸乙酯/石油醚1∶1 v/v和石油醚)分级为四个级分(即1、2、3和4)。四个级分(1、2、3和4)的产率分别为KL产率的59.6%、28.4%、10.8%和1.2%。凝胶渗透色谱(GPC)分析表明,每个级分的分子量从1到4逐渐降低。所有级分的多分散性均低于KL。通过化学成分分析、元素组成分析(EA)、甲氧基分析、傅里叶变换红外光谱(FT-IR)、硝基苯氧化分析(NBO)以及包括磷和氢-碳异核单量子相干核磁共振(H-C HSQC NMR)在内的核磁共振(NMR)对KL和各个级分进行了全面表征。结果表明,级分的甲氧基、羟基、单元间连接以及热性能随分子量而变化。通过溶剂分级提高了木质素的均匀性。