Preparation of cellulose I nanowhiskers with a mildly acidic aqueous ionic liquid: reaction efficiency and whiskers attributes

Cellulose I nanowhiskers were prepared in relatively high yield (48 ± 2 %) by single-stage hydrolysis of microcrystalline cellulose with an aqueous solution of 1-butyl-3-methylimidazolium hydrogen sulfate ([Bmim]HSO₄). This reaction occurred under mildly acidic reaction conditions with an [H⁺]/[AGU] ratio of 0.24 mol/mol, i.e., 2 orders of magnitude lower than with concentrated sulfuric acid. The nanowhiskers exhibited small width and width distribution and also smaller length than nanowhiskers obtained with concentrated acid. With a relatively low content of sulfur they also exhibited higher thermal stability than whiskers obtained with concentrated sulfuric acid. The lower solvating power of the aqueous ionic liquid compared to that of concentrated sulfuric acid likely contributes to the greater hydrolysis efficiency in the present system.