Enzymatic hydrolysis of ionic liquid-pretreated celluloses: Contribution of CP-MAS 13C NMR and SEM

The supramolecular structure of four model celluloses was altered prior to their enzymatic saccharification using two ionic liquid pretreatments: one with the commonly used 1-ethyl-3-methylimidazolium acetate ([Emim]+[CH3COO]−) and the other with the newly developed 1-ethyl-3-methylimidazolium methylphosphonate ([Emim]+[MeO(H)PO2]−). The estimation of crystallinity index (CrI) by solid state 13C nuclear magnetic resonance for each untreated/pretreated celluloses was compared with the performances of their enzymatic hydrolysis. For α-cellulose, both pretreatments led to a significant decrease in CrI from 25% to 5% but had no effect on glucose yields. In contrast, The [Emim]+[MeO(H)PO2]− pretreatment on the long fibers of cellulose had no significant effect on the CrI although a conversion yield in glucose of 88% is obtained versus 32% without pretreatment. However, scanning electron microscopy analysis suggested a loss of fiber organization induced by both ionic liquid pretreatments leading to a larger accessibility by cellulases to the cellulose surface.