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A Comparative Study of Lignin Recovery Conditions Using GVL-Organosolv and Lignin Characterization

Tanis, Medya H. LU orcid ; Vercoutere, Emilie ; Galbe, Mats LU ; Al-Rudainy, Basel LU and Wallberg, Ola LU orcid (2025) In ACS Sustainable Chemistry & Engineering
Abstract
Delignification is a critical step of the wood fractionation process in a
biorefinery. It directly influences the purity of lignin and aids in
breaking bonds within lignin and lignin–carbohydrate complexes
surrounding cellulose. The recalcitrant nature of lignocellulose poses
challenges in fractionating the material, notably during
delignification. Recent progress in understanding lignin’s physical and
chemical properties has led to the development of numerous value-added
products from lignin sources. This study discusses lignin recovery from
Norway spruce using γ-valerolactone (GVL)-based organosolv. The lignin
recovery was investigated by changing GVL concentration in deionized
water... (More)
Delignification is a critical step of the wood fractionation process in a
biorefinery. It directly influences the purity of lignin and aids in
breaking bonds within lignin and lignin–carbohydrate complexes
surrounding cellulose. The recalcitrant nature of lignocellulose poses
challenges in fractionating the material, notably during
delignification. Recent progress in understanding lignin’s physical and
chemical properties has led to the development of numerous value-added
products from lignin sources. This study discusses lignin recovery from
Norway spruce using γ-valerolactone (GVL)-based organosolv. The lignin
recovery was investigated by changing GVL concentration in deionized
water (60/20 and 80/20 v/v), temperature (140, 160 and 180 °C), and
addition of catalyst (sulfuric acid and phosphoric acid). The highest
delignification and lignin recovery were achieved with 60% GVL at 180 °C
in the presence of phosphoric acid (78% delignification and 66% lignin
recovery) and 80% GVL at 140 °C in the presence of sulfuric acid (67%
delignification and 50% lignin recovery). The lignin samples were
analyzed by FTIR, GPC, Py-GC/MS, and 2D HSQC NMR. FTIR spectra of lignin
showed that they have similar spectra with different intensities in the
fingerprint zone. Additionally, 2D HSQC NMR results show that the
lignin extracted from the 80% GVL at 140 °C in the presence of sulfuric
acid experiment had an abundance of about 47% (per 100 Ar) β-O-4
linkage. The results showed that the GVL-organosolv is a promising
method for lignin recovery, and the GVL-lignin is a good candidate for
high-value applications. (Less)
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author
; ; ; and
organization
publishing date
type
Contribution to journal
publication status
epub
subject
keywords
2D HSQC NMR, lignin recovery, Norway spruce, Py-GC/MS, softwood lignin, γ-valerolactone organosolv
in
ACS Sustainable Chemistry & Engineering
publisher
The American Chemical Society (ACS)
external identifiers
  • scopus:105006732761
ISSN
2168-0485
DOI
10.1021/acssuschemeng.5c03088
language
English
LU publication?
yes
id
98330fdb-6415-4e5b-bb91-01ae64ad7374
date added to LUP
2025-06-02 14:00:22
date last changed
2025-06-11 08:30:05
@article{98330fdb-6415-4e5b-bb91-01ae64ad7374,
  abstract     = {{Delignification is a critical step of the wood fractionation process in a<br>
 biorefinery. It directly influences the purity of lignin and aids in <br>
breaking bonds within lignin and lignin–carbohydrate complexes <br>
surrounding cellulose. The recalcitrant nature of lignocellulose poses <br>
challenges in fractionating the material, notably during <br>
delignification. Recent progress in understanding lignin’s physical and <br>
chemical properties has led to the development of numerous value-added <br>
products from lignin sources. This study discusses lignin recovery from <br>
Norway spruce using γ-valerolactone (GVL)-based organosolv. The lignin <br>
recovery was investigated by changing GVL concentration in deionized <br>
water (60/20 and 80/20 v/v), temperature (140, 160 and 180 °C), and <br>
addition of catalyst (sulfuric acid and phosphoric acid). The highest <br>
delignification and lignin recovery were achieved with 60% GVL at 180 °C<br>
 in the presence of phosphoric acid (78% delignification and 66% lignin <br>
recovery) and 80% GVL at 140 °C in the presence of sulfuric acid (67% <br>
delignification and 50% lignin recovery). The lignin samples were <br>
analyzed by FTIR, GPC, Py-GC/MS, and 2D HSQC NMR. FTIR spectra of lignin<br>
 showed that they have similar spectra with different intensities in the<br>
 fingerprint zone. Additionally, 2D HSQC NMR results show that the <br>
lignin extracted from the 80% GVL at 140 °C in the presence of sulfuric <br>
acid experiment had an abundance of about 47% (per 100 Ar) β-O-4 <br>
linkage. The results showed that the GVL-organosolv is a promising <br>
method for lignin recovery, and the GVL-lignin is a good candidate for <br>
high-value applications.}},
  author       = {{Tanis, Medya H. and Vercoutere, Emilie and Galbe, Mats and Al-Rudainy, Basel and Wallberg, Ola}},
  issn         = {{2168-0485}},
  keywords     = {{2D HSQC NMR; lignin recovery; Norway spruce; Py-GC/MS; softwood lignin; γ-valerolactone organosolv}},
  language     = {{eng}},
  month        = {{05}},
  publisher    = {{The American Chemical Society (ACS)}},
  series       = {{ACS Sustainable Chemistry & Engineering}},
  title        = {{A Comparative Study of Lignin Recovery Conditions Using GVL-Organosolv and Lignin Characterization}},
  url          = {{http://dx.doi.org/10.1021/acssuschemeng.5c03088}},
  doi          = {{10.1021/acssuschemeng.5c03088}},
  year         = {{2025}},
}