AbstractBagasse acetate butyrates were prepared homogeneously in 1-butyl-3-methylimidazolium chloride ([C4mim]Cl) ionic liquid from ball-milled sugarcane bagasse by acylation with acetic anhydride and butyric anhydride. The parameters, including reaction temperature, reaction time, feeding method of adding anhydrides, the dosage of total anhydrides to SCB, and the molar ratio of acetic anhydride to butyric anhydride, were considered, and the extent of acylation was measured by weight percent gain (WPG). The results showed the positive effects of reaction duration and total anhydride dosage on WPG and the negative effects of reaction temperature and molar ratio of AA/BA on WPG. The feeding method of acetylation after butyrylation resulted in the increased WPG compared with acetylation before butyrylation. FT-IR and 1H–13C correlation 2D NMR (HSQC) studies provided evidence for acylation. The bagasse acetate butyrates showed increased thermal stability after acylation. This study provides a new way for high value-added utilization of renewable lignocellulosic biomass.