Cellulose Dissolution in Ionic Liquid under Mild Conditions: Effect of Hydrolysis and Temperature

Abstract

This study investigated the effect of acid hydrolysis of cellulose on its dissolution under mild conditions in ionic liquid, 1-butyl-3-methylimidazolium acetate/N,N-dimethylacetamide (BMIMAc/DMAc). Acid hydrolysis of high molecular weight (MW) cotton cellulose (DP > 4000) was carried out to produce hydrolyzed cotton (HC) samples for dissolution. The HC samples were characterized using gel permeation chromatography (GPC), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and thermogravimetric analysis (TGA), and the dissolution process was monitored using polarized light microscopy (PLM). It was found that the drastic decrease of the MW of cellulose did not result in improvement of its dissolution at room temperature. As compared to original cotton cellulose, the high amount of undissolved fibers in HC solutions led to unstable rheological behavior of HC solutions. Agglomeration and inhomogeneous dispersion of HC, and increased crystallinity, in this case, likely made the diffusion of BMIMAc/DMAc more difficult to the inside of the polymeric network of cellulose at ambient temperature, thereby hindering the dissolution. However, increasing the temperature from room temperature to 35 °C and 55 °C, led to a significant improvement in cellulose dissolution. This phenomenon implies that reducing the MW of cellulose might not be able to improve its dissolution under certain conditions. During the dissolution process, the physical properties of cellulose including fiber aggregation status, solvent diffusivity, and cellulose crystallinity may play a critical role compared to the MW, while the MW may not be an important factor. This finding may help further understand the mechanism of cellulose dissolution and seek better strategies to dissolve cellulose under mild conditions for industrial applications.