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Universal fractionation of lignin-carbohydrate complexes (LCCs) from lignocellulosic biomass: an example using spruce wood
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Wood Chemistry and Pulp Technology.
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Wood Chemistry and Pulp Technology.
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Wood Chemistry and Pulp Technology.
2013 (English)In: The Plant Journal, ISSN 0960-7412, E-ISSN 1365-313X, Vol. 74, no 2, 328-338 p.Article in journal (Refereed) Published
Abstract [en]

It is of both theoretical and practical importance to develop a universally applicable approach for the fractionation and sensitive lignin characterization of lignin-carbohydrate complexes (LCCs) from all types of lignocellulosic biomass, both natively and after various types of processing. In the present study, a previously reported fractionation approach that is applicable for eucalyptus (hardwood) and flax (non-wood) was further improved by introducing an additional step of barium hydroxide precipitation to isolate the mannan-enriched LCC (glucomannan-lignin, GML), in order to suit softwood species as well. Spruce wood was used as the softwood sample. As indicated by the recovery yield and composition analysis, all of the lignin was recovered in three LCC fractions: a glucan-enriched fraction (glucan-lignin, GL), a mannan-enriched fraction (GML) and a xylan-enriched fraction (xylan-lignin, XL). All of the LCCs had high molecular masses and were insoluble or barely soluble in a dioxane/water solution. Carbohydrate and lignin signals were observed in H-1 NMR, C-13 CP-MAS NMR and normal- or high-sensitivity 2D HSQC NMR analyses. The carbohydrate and lignin constituents in each LCC fraction are therefore believed to be chemically bonded rather than physically mixed with one another. The three LCC fractions were found to be distinctly different from each other in terms of their lignin structures, as revealed by highly sensitive analyses by thioacidolysis-GC, thioacidolysis-SEC and pyrolysis-GC.

Place, publisher, year, edition, pages
2013. Vol. 74, no 2, 328-338 p.
Keyword [en]
lignin-carbohydrate complex (LCC), universal fractionation approach, spruce, NMR, thioacidolysis, pyrolysis-GC
National Category
Plant Biotechnology
Identifiers
URN: urn:nbn:se:kth:diva-122524DOI: 10.1111/tpj.12124ISI: 000317296200012Scopus ID: 2-s2.0-84876293824OAI: oai:DiVA.org:kth-122524DiVA: diva2:623017
Note

QC 20130524

Available from: 2013-05-24 Created: 2013-05-23 Last updated: 2017-12-06Bibliographically approved
In thesis
1. Deepening the insights of lignin structure: Lignin-carbohydrate complex (LCC) fractionation and characterization and Kraft lignin amination
Open this publication in new window or tab >>Deepening the insights of lignin structure: Lignin-carbohydrate complex (LCC) fractionation and characterization and Kraft lignin amination
2013 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Improvement of kraft pulping delignification efficiency and value-addition of industrial kraft lignin are two attractive topics. The proposal that delignification is deteriorated by the presence of lignin-carbohydrate complex (LCC) is still being debated. Therefore, it is theoretically and practically important to investigate various LCC structures from native wood and their changes during different treatments. Currently, however, there is no effective LCC fractionation method that could quantitatively isolate all LCC fractions and be applicable for all types of lignocellulosic materials. The fractionation should also be followed by comprehensive and reliable structural characterisation. Additionally the Kraft lignin has a heterogeneous structure and poor properties. Structural modification is therefore one possible solution for creating more economical benefits than the presently direct combustion for heat.

In this work, an LCC fractionation method has been developed, which preserves original lignin and lignin-carbohydrate (LC) bonding structures and is nearly quantitative. It is universally applicable for hardwood, softwood or non-wood species. A whole set of subsequent analytical tools for the comprehensive elucidation of the different LCC fractions has also been established and applied. After applying the LCC fractionation and characterisation:

1). spruce wood was found to consist of 49.5% glucan-lignin (GL), 30.9% glucomannan–lignin (GML) and 12.0% xylan–lignin (XL). Although the LC and lignin-lignin (LL) linkage signals could not be directly observed by a 400 MHz NMR instrument, these linkages have been clearly observed by a 600 MHz NMR instrument equipped with a cryogenic probe after enzymatic hydrolysis. The LC bondings include phenyl glycoside, benzyl ether and γ-ester. Based on the LL bond frequencies, GML is less condensed than XL.

2). a general lignin biodegradation mechanism by the laccase-mediator system (LMS) has been proposed, which mainly involves Cα oxidation and Cα-Cβ bond cleavage of the lignin side chain and eventually aromatic ring cleavage. The LMS delignification efficiency depends largely on the species of the applied laccase and mediator. Some LMS has been proven to possess an obvious capacity for hexenuronic acid (HexA) removal. For Kraft pulp bleaching, there are potential benefits of various combinations among biological treatment (by LMS), non-oxidative chemical (by urea treatment, U), and mechanical treatment (by refining, R).

In addition, it has been demonstrated in this work that the structures and properties of industrial softwood Kraft lignin (LignoBoost lignin) could largely be upgraded by amination via the Mannich reaction. With or without a phenolation pretreatment, the aminated lignins obtained are promising polycationic materials, especially in the application as colloidal suspensions. During this investigation of kraft lignin amination, NMR methods have been developed for the quantification of the N content introduced and for the deepened insights of the structural changes of the lignin. 

Place, publisher, year, edition, pages
Stockholm: KTH Royal Institute of Technology, 2013. 65 p.
Series
Trita-CHE-Report, ISSN 1654-1081 ; 2013:30
National Category
Polymer Chemistry
Identifiers
urn:nbn:se:kth:diva-126279 (URN)978-91-7501-818-8 (ISBN)
Public defence
2013-09-10, Sal F3, Lindstedtsvägen 26, KTH, Stockholm, 10:00 (English)
Opponent
Supervisors
Note

QC 20130820

Available from: 2013-08-20 Created: 2013-08-20 Last updated: 2013-08-20Bibliographically approved

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