Isolation of β-O-4-Rich Lignin From Birch in High Yields Enabled by Continuous-Flow Supercritical Water Treatment

Davide Rigo; Tijana Fechter; Ewellyn A. Capanema; Daryna Diment; Marie Alopaeus; Dmitry Tarasov; Danilo Cantero; Mikhail Yu Balakshin

doi:10.1002/cssc.202401683

Isolation of β-O-4-Rich Lignin From Birch in High Yields Enabled by Continuous-Flow Supercritical Water Treatment

Davide Rigo^*
, Tijana Fechter
, Ewellyn A. Capanema^*
, Daryna Diment
, Marie Alopaeus
, Dmitry Tarasov
, Danilo Cantero
, Mikhail Yu Balakshin

^*Korresponderande författare för detta arbete

Naturmaterialteknik

Forskningsoutput: Tidskriftsbidrag › Artikel › Vetenskaplig › Peer review

8 Citeringar (Scopus)

34 Nedladdningar (Pure)

Sammanfattning

Abstract The continuous flow supercritical water (scH2O) treatment of Birch wood (T=372?382?°C; t=0.3?0.7?s; p=260?bar) followed by alkali extraction of lignin allowed for the isolation of lignin and lignin carbohydrate complexes (LCCs) with a high number of ?-O-4 moieties in the range 29?57/100 Ar (evaluated by quantitative 13C NMR analysis) in yields ranging between 13?19?wt?% with respect to the initial wood. A ?lightning rod effect? of carbohydrates has been claimed to explain the low degradation of ?-O-4 bonds during the process. The structure of the isolated lignin was thoroughly elucidated via comprehensive NMR studies (HSQC, 13C and 31P). A low degree of condensation (DC)

Originalspråk	Engelska
Artikelnummer	e202401683
Tidskrift	ChemSusChem
Volym	18
Nummer	1
DOI	https://doi.org/10.1002/cssc.202401683
Status	Publicerad - 2 jan. 2025
MoE-publikationstyp	A1 Tidskriftsartikel-refererad

Finansiering

This work is dedicated to Prof. of practice Dr. Mikhail Balakshin. Prof. Chunlin Xu is thankfully acknowledged for his help in the data discussion. The authors acknowledge the Agencia Estatal de Investigaci\u00F3n for the financial support given in Project PID2020\u2013119249RA\u2212I00. This work was supported by the Regional Government of Castilla y Le\u00F3n (Spain) and the EU-FEDER program (CLU-2019-04). D.C. is funded by the Spanish Ministry of Science, Innovation and Universities (\u201CBeatriz Galindo\u201D fellowship BEAGAL18/00247). D.R., D.D. and M.B gratefully acknowledge the support from the Research Council of Finland (former Academy of Finland, grant decision number 341586). In addition, this work was a part of the Academy of Finland\u2032s Flagship Programme under Projects No. 318890 and 318891 (Competence Center for Materials Bioeconomy, FinnCERES). This work is dedicated to Prof. of practice Dr. Mikhail Balakshin. Prof. Chunlin Xu is thankfully acknowledged for his help in the data discussion. The authors acknowledge the Agencia Estatal de Investigaci\u00F3n for the financial support given in Project PID2020\u2013119249RA\u2212I00. This work was supported by the Regional Government of Castilla y Le\u00F3n (Spain) and the EU\u2010FEDER program (CLU\u20102019\u201004). D.C. is funded by the Spanish Ministry of Science, Innovation and Universities (\u201CBeatriz Galindo\u201D fellowship BEAGAL18/00247). D.R., D.D. and M.B gratefully acknowledge the support from the Research Council of Finland (former Academy of Finland, grant decision number 341586). In addition, this work was a part of the Academy of Finland\u2032s Flagship Programme under Projects No. 318890 and 318891 (Competence Center for Materials Bioeconomy, FinnCERES).

FN:s SDG:er

Detta resultat bidrar till följande hållbara utvecklingsmål:

SDG 9 – Hållbar industri, innovationer och infrastruktur
SDG 13 – Bekämpa klimatförändringarna

Nyckelord

Lignin
Lignin carbohydrate complexes (LCCs)
NMR
Supercritical water
DSC
GPC

Åtkomst av dokument

10.1002/cssc.202401683

ChemSusChem - 2024 - Rigo - Isolation of ‐O‐4‐Rich Lignin From Birch in High Yields Enabled by Continuous‐Flow-1Slutlig publicerad version, 2,76 MBLicens: CC BY-NC-ND

https://urn.fi/URN:NBN:fi-fe2025040122714

Åbo Akademi Functional Printing Center
Toivakka, M. (PI), Rosenholm, J. (PI), Anttu, N. (PI), Bobacka, J. (PI), Huynh, T. P. (PI), Peltonen, J. (PI), Wang, X. (PI), Wilen, C.-E. (PI), Xu, C. (PI), Zhang, H. (PI) & Österbacka, R. (PI)
Fakulteten för naturvetenskap och teknik
Utrustning/facilitet: Facilitet

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title = "Isolation of β-O-4-Rich Lignin From Birch in High Yields Enabled by Continuous-Flow Supercritical Water Treatment",

abstract = "The continuous flow supercritical water (scH 2O) treatment of Birch wood (T=372–382 °C; t=0.3–0.7 s; p=260 bar) followed by alkali extraction of lignin allowed for the isolation of lignin and lignin carbohydrate complexes (LCCs) with a high number of β-O-4 moieties in the range 29–57/100 Ar (evaluated by quantitative 13C NMR analysis) in yields ranging between 13–19 wt \% with respect to the initial wood. A “lightning rod effect” of carbohydrates has been claimed to explain the low degradation of β-O-4 bonds during the process. The structure of the isolated lignin was thoroughly elucidated via comprehensive NMR studies (HSQC, 13C and 31P). A low degree of condensation (DC)<5 \% was found for all the lignin samples, which was only slightly dependent on the reaction severity. The number of aliphatic −OH, phenolic −OH, and −COOH groups was in the range 3.37–5.25, 1.41–2.31 and 0.39–0.73 mmol/g, respectively. The number of −COOH groups increased with increased severity, suggesting that oxidation can occur during the scH 2O treatment. Furthermore, by simply varying the reaction severity, it was possible to tune important lignin properties, like the molar mass and the glass transition temperature (T g).",

keywords = "Lignin, Lignin carbohydrate complexes (LCCs), NMR, Supercritical water, DSC, GPC",

author = "Davide Rigo and Tijana Fechter and Capanema, \{Ewellyn A.\} and Daryna Diment and Marie Alopaeus and Dmitry Tarasov and Danilo Cantero and Balakshin, \{Mikhail Yu\}",

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AU - Rigo, Davide

AU - Fechter, Tijana

AU - Capanema, Ewellyn A.

AU - Diment, Daryna

AU - Alopaeus, Marie

AU - Tarasov, Dmitry

AU - Cantero, Danilo

AU - Balakshin, Mikhail Yu

PY - 2025/1/2

Y1 - 2025/1/2

N2 - The continuous flow supercritical water (scH 2O) treatment of Birch wood (T=372–382 °C; t=0.3–0.7 s; p=260 bar) followed by alkali extraction of lignin allowed for the isolation of lignin and lignin carbohydrate complexes (LCCs) with a high number of β-O-4 moieties in the range 29–57/100 Ar (evaluated by quantitative 13C NMR analysis) in yields ranging between 13–19 wt % with respect to the initial wood. A “lightning rod effect” of carbohydrates has been claimed to explain the low degradation of β-O-4 bonds during the process. The structure of the isolated lignin was thoroughly elucidated via comprehensive NMR studies (HSQC, 13C and 31P). A low degree of condensation (DC)<5 % was found for all the lignin samples, which was only slightly dependent on the reaction severity. The number of aliphatic −OH, phenolic −OH, and −COOH groups was in the range 3.37–5.25, 1.41–2.31 and 0.39–0.73 mmol/g, respectively. The number of −COOH groups increased with increased severity, suggesting that oxidation can occur during the scH 2O treatment. Furthermore, by simply varying the reaction severity, it was possible to tune important lignin properties, like the molar mass and the glass transition temperature (T g).

AB - The continuous flow supercritical water (scH 2O) treatment of Birch wood (T=372–382 °C; t=0.3–0.7 s; p=260 bar) followed by alkali extraction of lignin allowed for the isolation of lignin and lignin carbohydrate complexes (LCCs) with a high number of β-O-4 moieties in the range 29–57/100 Ar (evaluated by quantitative 13C NMR analysis) in yields ranging between 13–19 wt % with respect to the initial wood. A “lightning rod effect” of carbohydrates has been claimed to explain the low degradation of β-O-4 bonds during the process. The structure of the isolated lignin was thoroughly elucidated via comprehensive NMR studies (HSQC, 13C and 31P). A low degree of condensation (DC)<5 % was found for all the lignin samples, which was only slightly dependent on the reaction severity. The number of aliphatic −OH, phenolic −OH, and −COOH groups was in the range 3.37–5.25, 1.41–2.31 and 0.39–0.73 mmol/g, respectively. The number of −COOH groups increased with increased severity, suggesting that oxidation can occur during the scH 2O treatment. Furthermore, by simply varying the reaction severity, it was possible to tune important lignin properties, like the molar mass and the glass transition temperature (T g).

KW - Lignin

KW - Lignin carbohydrate complexes (LCCs)

KW - NMR

KW - Supercritical water

KW - DSC

KW - GPC

U2 - 10.1002/cssc.202401683

DO - 10.1002/cssc.202401683

M3 - Article

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JO - ChemSusChem

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ER -

Isolation of β-O-4-Rich Lignin From Birch in High Yields Enabled by Continuous-Flow Supercritical Water Treatment

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Åbo Akademi Functional Printing Center

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