| Summary: | Due to the natural cellulose encapsulated in both lignin and hemicellulose matrices, as well as in plant cell walls with a compact and complex hierarchy, extracting cellulose nanofibers (CNFs) from lignocellulosic biomass is challenging. In this study, a sustainable high yield strategy with respect to other CNF preparations was developed. The cellulose was liberated from plant cell walls and fibrillated to a 7–22 nm thickness in one bath treatment with H<sub>3</sub>PO<sub>4</sub> and H<sub>2</sub>O<sub>2</sub> under mild conditions. The cellulose underwent swelling, the lignin underwent oxidative degradation, and the hemicellulose and a small amount of cellulose underwent acid hydrolysis. The CNFs’ width was about 12 nm, with high yields (93% and 50% based on cellulose and biomass, respectively), and a 64% crystallinity and good thermal stability were obtained from bagasse. The current work suggests a strategy with simplicity, mild conditions, and cost-effectiveness, which means that this method can contribute to sustainable development for the preparation of CNFs.
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