Pretreatment with efficient fractionation, eco-friendliness, and low-cost brings high security to future biorefinery systems. Synergistic pretreatment is a compelling blueprint to tackle the compact structure of lignocellulose towards a high-level valorization. Here, a stepwise approach was designed using hydrothermal and deep eutectic solvent (DES) pretreatments to hierarchically extract hemicelluloses and lignin from poplar, while delivering a cellulose-rich substrate that could easily undergo enzymatic hydrolysis to obtain fermentable glucose and residual lignin. The lifetime of recyclable DES showed that the pretreatment efficiency was still largely maintained after the fourth recycling. An enhancement of enzymatic digestibility from 13.9 to 90.4 % was initiated by the deconstruction of amorphous portions and robust cell wall. 23.7 % Xylooligosaccharides (degree of polymerization 2-6), 47.5 % DES-isolated lignin, and 19.2 % cellulose enzymatic lignin were harvested via this coupled process. This study could promote the precise design of sustainable tandem pretreatment that can boost the frontier of highly available biorefinery.
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