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Structural Insights on Recalcitrance during Hydrothermal Hemicellulose Extraction from Wood
KTH, School of Chemical Science and Engineering (CHE), Centres, Wallenberg Wood Science Center. KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology. Wallenberg Wood Science Center. (Wallenberg Wood Science Center)ORCID iD: 0000-0003-4266-0720
KTH, School of Chemical Science and Engineering (CHE), Centres, Wallenberg Wood Science Center. KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology.ORCID iD: 0000-0002-8614-6291
2017 (English)In: ACS Sustainable Chemistry & Engineering, ISSN 2168-0485, Vol. 5, no 6, 5156-5165 p., 10.1021/acssuschemeng.7b00511Article in journal (Refereed) Published
Abstract [en]

Hydrothermal extraction of hemicelluloses from lignocellulosic biomass for conversion to renewable materials or fuels has captured attention. The extraction is however partial and some lignin is codissolved. Herein, we investigated the role of molecular structure in the recalcitrance. Wood meal of Spruce and Birch were subjected to pressurized hydrothermal extraction at 160 °C for 2 h, which extracted 68–75% of the hemicelluloses. 2D heteronuclear single quantum coherence (HSQC) NMR, HSQC-TOCSY, and 13C NMR were applied for structural studies of both extracts and residues. Subsequent to the known partial hydrolysis of native carbon-2 and carbon-3 acetates in hemicellulose, some acetylation of primary alcohols on hemicelluloses and lignin was observed. Lignin carbohydrate complexes (LCC) were detected in both the extracts and residues. In Spruce extracts, only the phenyl glycoside-type of LCC was detected. Birch extracts contained both the phenyl glycoside and benzyl ether-types. In the hydrothermal wood residues of both species, benzyl ether- and gamma (γ)-ester-LCC were present. Structural changes in lignin included decrease in aryl ether (βO4) content and increases in resinol- (ββ) and phenyl coumaran (β5) contents. On the basis of the overall analysis, the mechanisms and contribution of molecular structure to recalcitrance is discussed.

Place, publisher, year, edition, pages
American Chemical Society (ACS), 2017. Vol. 5, no 6, 5156-5165 p., 10.1021/acssuschemeng.7b00511
Keyword [en]
13C NMR; 2D HSQC; Autohydrolysis; HSQC-TOCSY; LCC repolymerization; Lignin carbohydrate complexes (LCC); Recalcitrance; trans-Acetylation
National Category
Wood Science
Research subject
Fibre and Polymer Science
Identifiers
URN: urn:nbn:se:kth:diva-208164DOI: 10.1021/acssuschemeng.7b00511OAI: oai:DiVA.org:kth-208164DiVA: diva2:1104425
Funder
Knut and Alice Wallenberg Foundation, 8107
Note

QC 20170613

Available from: 2017-06-01 Created: 2017-06-01 Last updated: 2017-06-13Bibliographically approved

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Publisher's full texthttp://pubs.acs.org/doi/abs/10.1021/acssuschemeng.7b00511

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