<p>Choline chloride–based deep eutectic solvents (DES) represent a promising green solution for the processing of renewable lignocellulosic biomass (LCB). In this study, a two-step antisolvent precipitation approach was initially employed to fractionate <i>Picea abies</i> LCB using DES. This method permitted the separation of the cellulose-rich fraction in the residue, as well as the separation of lignin and hemicelluloses using acetone and water as antisolvents. The use of carboxylic acid–based DES resulted in the almost complete (~ 90%) delignification of wood biomass under conditions of prolonged treatment (more than 24&#xa0;h) at elevated temperatures (up to 150&#xa0;°C) and in the presence of water additives (up to 30 wt%). The DES-lignin was then subjected to comprehensive characterization using nuclear magnetic resonance spectroscopy and high-resolution mass spectrometry. The findings indicated that, in the process of lignin isolation, the DES not only act as extraction solvents, but also serve as reaction reagents, thus leading to the chemical modification of the obtained samples. These include a reduction in the quantity of β-O-4 bonds, the formation of carbon–carbon bonds and stilbene structures, an increase in the number of phenolic hydroxyl groups, and a decrease in the quantity of aliphatic hydroxyl groups due to their acylation and interaction with choline chloride.</p> Graphical Abstract <p></p>

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Choline chloride–based deep eutectic solvents in lignocellulose fractionation: two-stage antisolvent precipitation approach

  • Artyom V. Belesov,
  • Daria A. Lvova,
  • Varvara V. Pishchevskaya,
  • Ilya I. Pikovskoi,
  • Anna V. Faleva,
  • Natalya V. Shkaeva,
  • Alexey V. Malkov,
  • Dmitry S. Kosyakov

摘要

Choline chloride–based deep eutectic solvents (DES) represent a promising green solution for the processing of renewable lignocellulosic biomass (LCB). In this study, a two-step antisolvent precipitation approach was initially employed to fractionate Picea abies LCB using DES. This method permitted the separation of the cellulose-rich fraction in the residue, as well as the separation of lignin and hemicelluloses using acetone and water as antisolvents. The use of carboxylic acid–based DES resulted in the almost complete (~ 90%) delignification of wood biomass under conditions of prolonged treatment (more than 24 h) at elevated temperatures (up to 150 °C) and in the presence of water additives (up to 30 wt%). The DES-lignin was then subjected to comprehensive characterization using nuclear magnetic resonance spectroscopy and high-resolution mass spectrometry. The findings indicated that, in the process of lignin isolation, the DES not only act as extraction solvents, but also serve as reaction reagents, thus leading to the chemical modification of the obtained samples. These include a reduction in the quantity of β-O-4 bonds, the formation of carbon–carbon bonds and stilbene structures, an increase in the number of phenolic hydroxyl groups, and a decrease in the quantity of aliphatic hydroxyl groups due to their acylation and interaction with choline chloride.

Graphical Abstract