Renewable hemicellulose with a unique structure exhibits a wide range of potential applications. However, it has been a formidable challenge to isolate hemicellulose with an intact structure from lignocellulosic materials. In this study, LiBr·3H2O (LBTH) was used as a green solvent for the effective fractionation of hemicellulose from bleached hardwood kraft pulp (BHKP) under mild conditions (25–85 °C). It was found that hemicellulose in BHKP can be dissolved in LBTH with ease and high selectivity owing to the breaking of hydrogen bonds between hemicellulose and cellulose, and the dissolved hemicellulose can be regenerated with a high degree of polymerization (DP) in the range of 240–264 using ethanol precipitation. The highest removal rate of hemicellulose from BHKP was as high as 95.2%, and the corresponding yield of pure hemicellulose reached 84.3%. Moreover, simultaneously obtained undissolved cellulose pulp through LBTH treatment had a high content of α-cellulose (96.7%), high DP (880), and trace levels of Fe (2 ppm), which met the standard requirement for dissolving pulp for the production of lyocell. In addition, LBTH can be easily recycled to guarantee a green and sustainable process. This work provides a new approach for highly selective fractionation of hemicellulose and cellulose from commercial BHKP based on an efficient and environmentally friendly LBTH treatment, which could be very promising for better valorization of hemicellulose and cellulose in many advanced applications.
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