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Ethanol organosolv fractionation combined with ball milling was conducted on three major agricultural residues: Rice husk (RH), rice straw (RS), and barley straw (BS). The highest lignin extraction yields of RH, RS, and BS were 55.2%, 53.1%, and 59.4% and the purity of lignin recovered was 99.5% for RH and RS, and 96.8% for BS, with similar chemical characteristics, i.e., low molecular weight distributions (1453–1817 g/mol) and poly dispersity index (1.15–1.28). However, considering the simultaneous production of hemicellulose-derived sugars, distinctive fractionation behaviors were shown for the three agricultural residues. The highest hemicellulose-derived sugar yield was 73.8% when RH was fractionated at 170 °C for 30 min. Meanwhile, very low sugar yields of 31.9% and 35.7% were obtained from RS and BS, respectively. The highest glucan-to-glucose conversion yield from enzymatic hydrolysis of fractionated RH reached 85.2%. Meanwhile, the enzymatic digestibility of the fractionated RS and BS was 60.0% and 70.5%, respectively. Consequently, the fractionation efficiency for RH can be improved with fine refinement. For the case of RS, other fractionation process should be applied to achieve effective fractionation performance.

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Extraction Behaviors of Lignin and Hemicellulose-Derived Sugars During Organosolv Fractionation of Agricultural Residues Using a Bench-Scale Ball Milling Reactor