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Highly ordered cellulose II crystalline regenerated from cellulose hydrolyzed by 1-butyl-3-methylimidazolium chloride

Ahn, Yongjun, Song, Younghan, Kwak, Seung-Yeop, Kim, Hyungsup
Carbohydrate polymers 2016 v.137 pp. 321-327
X-ray diffraction, cellulose, chromatography, crystal structure, crystallization, hydrolysis, ionic liquids, molecular weight, rheological properties
This research focused on the preparation of highly ordered cellulose II crystalline by cellulose hydrolysis in ionic liquid, and the influence of molecular mobility on recrystallization of cellulose. The molar mass of cellulose was controlled by hydrolysis using 1-butyl-3-methylimidazolium chloride (BmimCl). The molecular mobility of cellulose dissolved in BmimCl was characterized by rheological properties. After characterization of cellulose solution and regeneration, change of molar mass and conversion to crystalline were monitored using gel-permeation chromatography and powder X-ray diffraction, respectively. The molar mass of the cellulose in BmimCl was remarkably decreased with an increase in duration time, resulting in better mobility and a lower conformational constraint below critical molar mass. The decrease in molar mass surprisingly increased the crystallinity up to ∼85%, suggesting a recrystallization rate dependence of the mobility. The correlation between the mobility and recrystallization rate represented quit different behavior above and below a critical molar mass, which strongly demonstrated to the effect of mobility on the conversion of amorphous state to crystalline structure.