超高效聚合物凝胶色谱法快速研究酸催化木质素解聚产物

doi:10.3724/SP.J.1123.2019.02013

色谱 ›› 2019, Vol. 37 ›› Issue (9): 983-989.DOI: 10.3724/SP.J.1123.2019.02013

超高效聚合物凝胶色谱法快速研究酸催化木质素解聚产物

方红霞, 钱晨, 崔朋, 刘京凤, 胡小坡, 何华龙, 孙继影

黄山学院化学化工学院应用化学研究所, 安徽黄山 245041

收稿日期:2019-02-21 出版日期:2019-09-08 发布日期:2015-07-30
通讯作者: 方红霞
基金资助:
安徽省教育厅自然科学项目（KJ2019A0613，KJHS2019B4）；安徽省骨干教师国外访学项目（gxfxZD2016236）；国家级大学生创新创业训练计划（201710375025）；安徽省省级大学生创新创业训练计划（201610375067）；安徽省创客实验室（2016ckjh190）；企业委托研发项目（hxkt20180019）.

A rapid method based on advanced polymer chromatography for analyzing the products of the acid-catalyzed depolymerization of lignosulfonate

FANG Hongxia, QIAN Chen, CUI Peng, LIU Jingfeng, HU Xiaopo, HE Hualong, SUN Jiying

Applied Chemistry Laboratory, School of Chemistry and Chemical Engineering, Huangshan University, Huangshan 245041, China

Received:2019-02-21 Online:2019-09-08 Published:2015-07-30
Supported by:
Natural Science Foundation of the Anhui Higher Education Institutions of China (Nos. KJ2019A0613, KJHS2019B4); Abroad Visiting & Research Program for Young Talents (No. gxfxZD2016236); Undergraduate Innovation and Entrepreneurship Training Program of China (No. 201710375025); Undergraduate Innovation and Entrepreneurship Training Program of Anhui Province (No. 201610375067); Maker Lab Program of Anhui Province (No. 2016ckjh190); Enterprise Entrusted Project (No. hxkt20180019).

摘要/Abstract

摘要： 该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，建立系统分离和分析测试木质素磺酸盐解聚后获得的低分子酚类产物的方法。选用4根油溶性的ACQUITY APC XT小孔径刚性填料色谱柱串联，在高分辨紫外检测器条件下，采用超高效凝胶渗透色谱（APC）对解聚产物实现了高效分离，获得了高灵敏度的木质素基酚类产物的相对分子质量及其分布色谱信息。探讨了反应温度、时间和催化剂浓度等对酸催化木质素磺酸盐解聚行为的影响，结果表明，对于木酚比（木质素：苯酚）为25%（质量分数）的木质素磺酸盐解聚体系，在催化剂和木质素物质的量比为2.334、130℃酸催化反应60 min时，获得了解聚效率高达80%以上的木质素基酚类产物，解聚获得的产物相对峰高分子质量（M_p）组成均分布在720、490和260 Da 3个低聚物区间，均具有很窄的分子质量分布指数（接近1）。由此可以初步推断，木质素磺酸盐在该研究采用的温和酸催化条件下，催化反应机理不受反应时间、温度以及催化剂浓度的影响，具有特定的解聚途径。

关键词: 超高效凝胶渗透色谱, 分离分析, 酚类产物, 木质素磺酸盐, 酸催化解聚

Abstract: In this study, a fast and efficient method for the separation and analysis of the products in the acid-catalyzed depolymerization of commercially available sodium lignosulfonate has been developed. The depolymerized lignosulfonate products were well separated and characterized by advanced polymer chromatography (APC) employing four ACQUITY APC XT columns in series and a ultraviolet detector. The developed method enabled the detection of relative-low-molecular-mass lignin degradation products with peak molecular weights (M_p) of 720, 490, and 260 Da, and an extremely low polydispersity index (PDI) of 1, indicating almost complete conversion of lignosulfonate to smaller molecules. The effects of reaction temperature, time, and catalyst/lignin ratio on the reaction products were systematically investigated. High yields of depolymerization (>80%) could be obtained under the mild acid-catalyzed conditions at 130℃ for 60 min using a catalyst/lignin ratio of 2.334:1. Preliminary studies also indicated that the mild acid-catalytic mechanism is unaffected by the reaction time, temperature, or catalyst concentration, thus suggesting the specificity of the catalytic procedure employed.

Key words: acid-catalyzed depolymerization, advanced polymer chromatography (APC), lignosulfonate, phenolic compounds, separation and analysis

中图分类号:

O658

方红霞, 钱晨, 崔朋, 刘京凤, 胡小坡, 何华龙, 孙继影. 超高效聚合物凝胶色谱法快速研究酸催化木质素解聚产物[J]. 色谱, 2019, 37(9): 983-989.

FANG Hongxia, QIAN Chen, CUI Peng, LIU Jingfeng, HU Xiaopo, HE Hualong, SUN Jiying. A rapid method based on advanced polymer chromatography for analyzing the products of the acid-catalyzed depolymerization of lignosulfonate[J]. Chinese Journal of Chromatography, 2019, 37(9): 983-989.

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超高效聚合物凝胶色谱法快速研究酸催化木质素解聚产物

A rapid method based on advanced polymer chromatography for analyzing the products of the acid-catalyzed depolymerization of lignosulfonate

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