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Title: Effect of heat treatment on the chemical structure and thermal properties of softwood-derived glycol lignin
Authors: Nge, Thi, Thi
Tobimatsu, Yuki  kyouindb  KAKEN_id  orcid (unconfirmed)
Yamamura, Masaomi
Takahashi, Shiho
Takata, Eri
Umezawa, Toshiaki  kyouindb  KAKEN_id
Yamada, Tatsuhiko
Author's alias: 飛松, 裕基
梅澤, 俊明
Keywords: glycol lignin
polyethylene glycol (PEG) solvolysis
wood meal size
heat treatment
thermal flow property
Issue Date: Mar-2020
Publisher: MDPI AG
Journal title: Molecules
Volume: 25
Issue: 5
Thesis number: 1167
Abstract: A large-scale glycol lignin (GL) production process (50 kg wood meal per batch) based on acid-catalyzed polyethylene glycol (PEG) solvolysis of Japanese cedar (JC) was developed at the Forestry and Forest Products Research Institute (FFPRI), Tsukuba, Japan. JC wood meal with various particle size distributions (JC-S < JC-M < JC-L) (average meal size, JC-S (0.4 mm) < JC-M (0.8 mm) < JC-L (1.6 mm)) and liquid PEG with various molecular masses are used as starting materials to produce PEG-modified lignin derivatives, namely, GLs, with various physicochemical and thermal properties. Because GLs are considered a potential feedstock for industrial applications, the effect of heat treatment on GL properties is an important issue for GL-based material production. In this study, GLs obtained from PEG400 solvolysis of JC-S, JC-M, and JC-L were subjected to heating in a constant-temperature drying oven at temperatures ranging from 100 to 220 °C for 1 h. All heat-treated GL series were thermally stable, as determined from the Klason lignin content, TMA, and TGA analyses. SEC analysis suggests the possibility of condensation among lignin fragments during heat treatment. ATR-FTIR spectroscopy, thioacidolysis, and 2D HSQC NMR demonstrated that a structural rearrangement occurs in the heat-treated GL400 samples, in which the content of α–PEG-β–O-4 linkages decreases along with the proportional enrichments of β–5 and β–β linkages, particularly at treatment temperatures above 160 °C.
Rights: © 2020 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (
DOI(Published Version): 10.3390/molecules25051167
PubMed ID: 32150921
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