Surfactant-assisted ionic liquid fractionation of spruce produces a low molar weight and less condensed lignin

Surfactant-assisted ionoSolv fractionation of spruce sawdust was investigated with the aim of improving the fractionation performance and the quality of the recovered fractions. Anionic surfactants sodium dodecyl sulfate (SDS) and linear alkylbenzenesulfonate (LAS) were added to ionic liquid (IL) water mixtures of N,N -dimethylbutylammonium hydrogen sulphate ([DMBA][HSO 4 ]) containing 20–50 wt% water to process spruce sawdust at 150 and 170 °C for 30–60 min. 1 H NMR spectroscopy established that the processing conditions partly hydrolysed SDS whilst leaving LAS untouched. The use of LAS surfactant decreased the fractionation time but did not encourage the use of a higher water content. IonoSolv fractionation employing 2–10 wt% LAS and 20 wt% water resulted in faster delignification, decreasing the reaction time by 50 % at 150 ºC, with small improvements in cellulose recovery (87.6 % with 2 wt% LAS vs 83.7 % without LAS at 150 ºC). Post-treatment lignin analysis showed that the lignin structure was less condensed when LAS was present during the fractionation. Addition of surfactant had a lightening effect on the colour of the recovered lignin fractions, which is a key feature for its use in applications such as coatings, cosmetics or sunscreen additives. A proportion of LAS surfactant precipitated with the lignin fraction and was found to be mainly physically associated to lignin, although traces of condensed lignin-LAS were also detected. Whilst the extent to which surfactants may assist ionoSolv fractionation was limited, the study highlights the importance of characterising both lignin and cellulose chemical compositions. • Adding surfactants improves the performance of ionoSolv fractionation of biomass. • Addition of surfactants decreased optimal fractionation time by 50 %. • The presence of surfactant protected lignin from degradation and recondensation. • Lignin recovered in the presence of surfactant has lighter color. • Small degree of lignin-surfactant recondensation was detected.

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Publication Details

Journal
Industrial Crops and Products
Published
2025-09-03
DOI
https://doi.org/10.1016/j.indcrop.2025.121815
Primary Topic
Lignin and Wood Chemistry
Type
article
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article

Surfactant-assisted ionic liquid fractionation of spruce produces a low molar weight and less condensed lignin

Jason P. Hallett, Pedro Verdía, Amir Al Ghatta, Giacomo Damilano et al.
Industrial Crops and Products
Lignin and Wood Chemistry
article

Surfactant-assisted ionic liquid fractionation of spruce produces a low molar weight and less condensed lignin

Jason P. Hallett, Pedro Verdía, Amir Al Ghatta, Giacomo Damilano, Agnieszka Brandt‐Talbot, Isabel Fernández Artime, Phuthiphong Ouitrakoon
article en

Abstract

Surfactant-assisted ionoSolv fractionation of spruce sawdust was investigated with the aim of improving the fractionation performance and the quality of the recovered fractions. Anionic surfactants sodium dodecyl sulfate (SDS) and linear alkylbenzenesulfonate (LAS) were added to ionic liquid (IL) water mixtures of N,N -dimethylbutylammonium hydrogen sulphate ([DMBA][HSO 4 ]) containing 20–50 wt% water to process spruce sawdust at 150 and 170 °C for 30–60 min. 1 H NMR spectroscopy established that the processing conditions partly hydrolysed SDS whilst leaving LAS untouched. The use of LAS surfactant decreased the fractionation time but did not encourage the use of a higher water content. IonoSolv fractionation employing 2–10 wt% LAS and 20 wt% water resulted in faster delignification, decreasing the reaction time by 50 % at 150 ºC, with small improvements in cellulose recovery (87.6 % with 2 wt% LAS vs 83.7 % without LAS at 150 ºC). Post-treatment lignin analysis showed that the lignin structure was less condensed when LAS was present during the fractionation. Addition of surfactant had a lightening effect on the colour of the recovered lignin fractions, which is a key feature for its use in applications such as coatings, cosmetics or sunscreen additives. A proportion of LAS surfactant precipitated with the lignin fraction and was found to be mainly physically associated to lignin, although traces of condensed lignin-LAS were also detected. Whilst the extent to which surfactants may assist ionoSolv fractionation was limited, the study highlights the importance of characterising both lignin and cellulose chemical compositions. • Adding surfactants improves the performance of ionoSolv fractionation of biomass. • Addition of surfactants decreased optimal fractionation time by 50 %. • The presence of surfactant protected lignin from degradation and recondensation. • Lignin recovered in the presence of surfactant has lighter color. • Small degree of lignin-surfactant recondensation was detected.

Industrial Crops and ProductsVol. 235
Imperial College London (GB)
Openalex Percentile: Top 78%
Lignin and Wood Chemistry
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