NMR studies of stock process water and reaction pathways in hydrothermal carbonization of furfural residue

作     者：Fen Yue Christian Marcus Pedersen Xiuyin Yan Yequn Liu Danlei Xiang Caifang Ning Yingxiong Wang Yan Qiao 

作者机构：Institute of Coal Chemistry Chinese Academy of Sciences Institute of Process Engineering Chinese Academy of Sciences Department of Chemistry University of Copenhagen Taiyuan Supervision and Testing Station for Quality of Grain Department of Applied Biology and Chemical Technology The Hong Kong Polytechnic University 

出 版 物：《Green Energy & Environment》 (绿色能源与环境（英文版）)

年 卷 期：2018年第3卷第2期

页      面：163-171页

核心收录：

学科分类：083002[工学-环境工程] 0830[工学-环境科学与工程（可授工学、理学、农学学位）] 08[工学] 

基　　金：Supported by Shanxi Scholarship Council of China (2015-123) the Natural Science Foundation of China (51602322) the Key Research and Development Program of Shanxi Province (International Cooperation) (201703D421041) for financial support 

主　　题：NMR Hydrothermal carbonization Furfural residue Stock process water 

摘      要：Hydrothermal carbonization(HTC) is a valuable approach to convert furfural residue(FR) into carbon material. The prepared biochars are usually characterized comprehensively, while the stock process water still remains to be studied in detail. Herein, a NMR study of the main components in stock process water generated at different HTC reaction conditions was reported. Various qualitative and quantitative NMR techniques(~1H and ^(13)C NMR,~1H-~1H COSY and ~1H-^(13)C HSQC etc.) especially 1D selective gradient total correlation spectroscopy(TOCSY NMR) were strategically applied in the analysis of HTC stock process water. Without separation and purification, it was demonstrated that the main detectable compounds are 5-hydroxymethylfurfural, formic acid, methanol, acetic acid, levulinic acid, glycerol, hydroxyacetone and acetaldehyde in this complicate mixture. Furthermore, the relationship between the concentration of major products and the reaction conditions(180-240 ℃ at 8 h, and 1-24 h at 240 ℃) was established. Finally, reasonable reaction pathways for hydrothermal conversion of FR were proposed based on this result and our previously obtained characteristics of biochars. The routine and challenging NMR methods utilized here would be an alternative other than HPLC or GC for biomass conversion research and can be extended to more studies.