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Article

The Impact of Biomass and Acid Loading on Methanolysis during Two-Step Lignin-First Processing of Birchwood

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Laboratory of Inorganic Materials and Catalysis, Department of Chemical Engineering and Chemistry, Eindhoven University of Technology, P.O. Box 513, 5600 MB Eindhoven, The Netherlands
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Vertoro B.V., Urmonderbaan 22, 6167 RD Geleen, The Netherlands
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Polymer Technology Group Eindhoven (PTG/e) B.V., P.O. Box 6284, 5600 HG Eindhoven, The Netherlands
*
Author to whom correspondence should be addressed.
Academic Editor: Maria Fernanda Neira D’Angelo
Catalysts 2021, 11(6), 750; https://doi.org/10.3390/catal11060750
Received: 19 May 2021 / Revised: 7 June 2021 / Accepted: 9 June 2021 / Published: 19 June 2021
(This article belongs to the Special Issue Catalytic Biomass Upgrading)
We optimized the solvolysis step in methanol for two-step lignin-first upgrading of woody biomass. Birchwood was first converted via sulfuric acid methanolysis to cellulose pulp and a lignin oil intermediate, which comprises a mixture of lignin oligomers and C5 sugars in the methanol solvent. The impact of reaction temperature (140–200 °C), acid loading (0.24–0.81 wt%, dry biomass), methanol/biomass ratio (2.3/1–15.8/1 w/w) and reaction time (2 h and 0.5 h) was investigated. At high biomass loadings (ratio < 6.3/1 w/w), operation at elevated pressure facilitates delignification by keeping methanol in the liquid phase. A high degree of delignification goes together to a large extent with C5 sugar release, mostly in the form of methyl xylosides. Gel permeation chromatography and heteronuclear single quantum coherence NMR of lignin fractions obtained at high acid (0.81 wt%) and low biomass (15.8/1 w/w) loading revealed extensive cleavage of β-O-4′ bonds during acidolysis at 180 °C for 2 h. At an optimized methanol/biomass ratio of 2.3/1 w/w and acid loading (0.24 wt%), more β-O-4′ bonds could be preserved, i.e., about 33% after 2 h and 47% after 0.5 h. The high reactivity of the extracted lignin fragments was confirmed by a second hydrogenolysis step. Reductive treatment with Pd/C under mild conditions led to disappearance of ether linkages and molecular weight reduction in the hydrotreated lignin oil. View Full-Text
Keywords: biomass; lignin first; optimization; lignin oil; β-O-4 content; depolymerization biomass; lignin first; optimization; lignin oil; β-O-4 content; depolymerization
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MDPI and ACS Style

Kouris, P.D.; Huang, X.; Ouyang, X.; van Osch, D.J.G.P.; Cremers, G.J.W.; Boot, M.D.; Hensen, E.J.M. The Impact of Biomass and Acid Loading on Methanolysis during Two-Step Lignin-First Processing of Birchwood. Catalysts 2021, 11, 750. https://doi.org/10.3390/catal11060750

AMA Style

Kouris PD, Huang X, Ouyang X, van Osch DJGP, Cremers GJW, Boot MD, Hensen EJM. The Impact of Biomass and Acid Loading on Methanolysis during Two-Step Lignin-First Processing of Birchwood. Catalysts. 2021; 11(6):750. https://doi.org/10.3390/catal11060750

Chicago/Turabian Style

Kouris, Panos D., Xiaoming Huang, Xianhong Ouyang, Dannie J.G.P. van Osch, Geert J.W. Cremers, Michael D. Boot, and Emiel J.M. Hensen 2021. "The Impact of Biomass and Acid Loading on Methanolysis during Two-Step Lignin-First Processing of Birchwood" Catalysts 11, no. 6: 750. https://doi.org/10.3390/catal11060750

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