Utilizing N,N-dimethylbutylammonium hydrogen sulfate for the pretreatment of lignin-rich waste, argan nut shells


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Haykir N. I., GÖKÇE Y., Sar T., Viell J.

Biomass Conversion and Biorefinery, 2025 (SCI-Expanded) identifier

  • Publication Type: Article / Article
  • Publication Date: 2025
  • Doi Number: 10.1007/s13399-025-06678-3
  • Journal Name: Biomass Conversion and Biorefinery
  • Journal Indexes: Science Citation Index Expanded (SCI-EXPANDED), Scopus, Compendex, INSPEC
  • Keywords: Argan nut shells, Fractionation, Lignin, Pretreatment, Protic ionic liquid, Valorization
  • Ankara University Affiliated: Yes

Abstract

Argan nut shells (ANSs), a lignin-rich residue (40 wt-%) from the argan plant, have seen limited use for energy and material-based applications so far. To explore the potential of this industrial crop waste for prospective applications, fractionation of ANS with the protic ionic liquid (PIL), N,N-dimethylbutylammonium hydrogen sulfate ([DMBA][HSO4]) was performed at different operating conditions for enzymatic saccharification of cellulose. At 140 °C for 5 h, [DMBA][HSO4] extracted 73% of the lignin revealing cellulose-enriched biomass with 75% cellulose content. Recovered cellulose-enriched pulp showed morphological and crystallinity changes consistent with its composition, including the emergence of fibrous structures and an increase in the crystallinity index. Cellulose-enriched pulp was enzymatically converted into reducing sugars, achieving approximately 70% saccharification yield. Characterization of lignin precipitates from the pretreatment slurries using FTIR and TGA confirmed the absence of carbohydrates, indicating high-quality lignin. Additionally, humin formation as evident from the spherical forms observed on the recovered pulp following pretreatment at 160 °C for 5 h highlights the importance of the severity of pretreatment conditions. This study helps to understand the interaction between ANS and a PIL and raises the question of whether the cellulose- and lignin-rich fractions obtained after pretreatment can potentially be utilized; however, further evaluation is required to determine their suitability for energy and material generation.