Characterization of Carboxylated Cellulose Nanocrystals Isolated Through Oxalic Acid Hydrolysis from Solid Residues of Softwood-Derived Glycol Lignin Production

The efficient use of renewable lignocellulosic biomass has attracted wide interest, as it promises to reduce the environmental impact of fossil fuel consumption. A recently developed batch-scale process, which produces glycol lignin (GL) from softwood biomass, generates a considerable amount of cell...

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Main Authors: Thi Thi Nge, Tatsuhiko Yamada
Format: Article
Language:English
Published: MDPI AG 2025-07-01
Series:Molecules
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Online Access:https://www.mdpi.com/1420-3049/30/14/2922
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author Thi Thi Nge
Tatsuhiko Yamada
author_facet Thi Thi Nge
Tatsuhiko Yamada
author_sort Thi Thi Nge
collection DOAJ
description The efficient use of renewable lignocellulosic biomass has attracted wide interest, as it promises to reduce the environmental impact of fossil fuel consumption. A recently developed batch-scale process, which produces glycol lignin (GL) from softwood biomass, generates a considerable amount of cellulose-rich solid residues (SRs) as a byproduct. In this study, usable cellulose was isolated from SRs in the form of carboxylated cellulose nanocrystals (O-CNCs). The properties of O-CNCs were investigated to establish a possible integrated biomass utilization system based on the GL production technology. Three different forms of purified SRs—never-dried (N-Cel), freeze-dried (F-Cel), and vacuum-dried (V-Cel) cellulose—were subjected to oxalic acid (OA) hydrolysis at 95 °C for 4 h. The average length of O-CNCs ranged from 90 to 120 nm and the height ranged from 3 to 6 nm for separate particles and from 8 to 20 nm for aggregates. The carboxyl group content was 0.11–0.23 mmol/g O-CNCs. The overall results indicated that the yields, dimensions, surface charges, and thermal stability of the O-CNCs were largely influenced by the nature of the starting cellulose. In addition, O-CNCs prepared from recycled OA exhibited similar properties to those prepared from fresh OA.
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spelling doaj-art-1e3f3ec4cfd749f7b3c0fa927a7ebc5a2025-08-20T03:32:15ZengMDPI AGMolecules1420-30492025-07-013014292210.3390/molecules30142922Characterization of Carboxylated Cellulose Nanocrystals Isolated Through Oxalic Acid Hydrolysis from Solid Residues of Softwood-Derived Glycol Lignin ProductionThi Thi Nge0Tatsuhiko Yamada1Center for Advanced Materials, Forestry and Forest Products Research Institute (FFPRI), 1 Matsunosato, Tsukuba 305-8687, JapanCenter for Advanced Materials, Forestry and Forest Products Research Institute (FFPRI), 1 Matsunosato, Tsukuba 305-8687, JapanThe efficient use of renewable lignocellulosic biomass has attracted wide interest, as it promises to reduce the environmental impact of fossil fuel consumption. A recently developed batch-scale process, which produces glycol lignin (GL) from softwood biomass, generates a considerable amount of cellulose-rich solid residues (SRs) as a byproduct. In this study, usable cellulose was isolated from SRs in the form of carboxylated cellulose nanocrystals (O-CNCs). The properties of O-CNCs were investigated to establish a possible integrated biomass utilization system based on the GL production technology. Three different forms of purified SRs—never-dried (N-Cel), freeze-dried (F-Cel), and vacuum-dried (V-Cel) cellulose—were subjected to oxalic acid (OA) hydrolysis at 95 °C for 4 h. The average length of O-CNCs ranged from 90 to 120 nm and the height ranged from 3 to 6 nm for separate particles and from 8 to 20 nm for aggregates. The carboxyl group content was 0.11–0.23 mmol/g O-CNCs. The overall results indicated that the yields, dimensions, surface charges, and thermal stability of the O-CNCs were largely influenced by the nature of the starting cellulose. In addition, O-CNCs prepared from recycled OA exhibited similar properties to those prepared from fresh OA.https://www.mdpi.com/1420-3049/30/14/2922carboxylated cellulose nanocrystalsrecyclable oxalic acidsoftwoodsolid residuesglycol lignin
spellingShingle Thi Thi Nge
Tatsuhiko Yamada
Characterization of Carboxylated Cellulose Nanocrystals Isolated Through Oxalic Acid Hydrolysis from Solid Residues of Softwood-Derived Glycol Lignin Production
Molecules
carboxylated cellulose nanocrystals
recyclable oxalic acid
softwood
solid residues
glycol lignin
title Characterization of Carboxylated Cellulose Nanocrystals Isolated Through Oxalic Acid Hydrolysis from Solid Residues of Softwood-Derived Glycol Lignin Production
title_full Characterization of Carboxylated Cellulose Nanocrystals Isolated Through Oxalic Acid Hydrolysis from Solid Residues of Softwood-Derived Glycol Lignin Production
title_fullStr Characterization of Carboxylated Cellulose Nanocrystals Isolated Through Oxalic Acid Hydrolysis from Solid Residues of Softwood-Derived Glycol Lignin Production
title_full_unstemmed Characterization of Carboxylated Cellulose Nanocrystals Isolated Through Oxalic Acid Hydrolysis from Solid Residues of Softwood-Derived Glycol Lignin Production
title_short Characterization of Carboxylated Cellulose Nanocrystals Isolated Through Oxalic Acid Hydrolysis from Solid Residues of Softwood-Derived Glycol Lignin Production
title_sort characterization of carboxylated cellulose nanocrystals isolated through oxalic acid hydrolysis from solid residues of softwood derived glycol lignin production
topic carboxylated cellulose nanocrystals
recyclable oxalic acid
softwood
solid residues
glycol lignin
url https://www.mdpi.com/1420-3049/30/14/2922
work_keys_str_mv AT thithinge characterizationofcarboxylatedcellulosenanocrystalsisolatedthroughoxalicacidhydrolysisfromsolidresiduesofsoftwoodderivedglycolligninproduction
AT tatsuhikoyamada characterizationofcarboxylatedcellulosenanocrystalsisolatedthroughoxalicacidhydrolysisfromsolidresiduesofsoftwoodderivedglycolligninproduction