The influence of the operating conditions of Miscanthus x Giganteus autohydrolysis on the composition of the solid residues and hydrolysates was examined. Milled wood lignin (MWL) extracted after autohydrolysis treatments performed at the same severity but at different temperatures were studied by (13)C and (31)P NMR in order to obtain a more complete picture of the changes in lignin structure occurring during the autohydrolysis. It was proposed that (1) the lignin homolytical fragmentation route should be enhanced with an increase of the temperature of the autohydrolysis treatment and (2) addition of a catalytic amount of 2-naphthol during the autohydrolysis step not only enhanced the dissolution of lignin but also allowed a better recovery of the hemicellulose sugars. A combined process involving an optimized autohydrolysis step (carried out in presence or not of 2-naphthol) and a low severity ethanol organosolv treatment was described for the separation and recovery of lignin, cellulose and hemicelluloses.
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