Transition of cellulose supramolecular structure during concentrated acid treatment and its implication for cellulose
Lida Xing1, Chuanshuang Hu1, Weiwei Zhang1
1College of Materials and Energy, South China Agricultural University, Guangzhou, 510642, PR China.
Abstract:
Cellulose nanocrystals with cellulose I and II allomorphs (CNC-I and CNC-II) were prepared from eucalyptus cellulose I substrate by controlling the sulfuric acid hydrolysis conditions, including acid concentration (56-64 wt%), reaction temperature (45 or 60 °C) and time (10-120 min). The crystalline structures were verified by XRD and 13C-NMR. CNC-II only appeared at very restricted reaction conditions. The rapid cellulose supramolecular structure transition under sulfuric acid concentration of around 60 wt% resulted in an abrupt change in CNC yield. A maximal CNC yield of 66.7% was obtained at acid concentration of 58 wt% and reaction temperature of 60 °C. CNC-I exhibited spindle-shape, while CNC-II showed a twisted strip structure. The state of order in cellulose during the acid hydrolysis process has been studied using a coagulation method. A tentative model of CNC-I and CNC-II formation was then proposed. This work provided significant knowledge for the production of CNCs with high yield and controllable allomorph.
