NC State
Mishra, S. P., Thirree, J., Manent, A.-S., Chabot, B., and Daneault, C. (2011). "Ultrasound-catalyzed TEMPO-mediated oxidation of native cellulose for the production of nanocellulose: Effect of process variables," BioRes. 6(1), 121-143.


In this study application of ultrasound in oxidizing native cellulose for the production of nanocellulose has been explored for the first time. Bleached hardwood kraft pulp was oxidized with an ultrasound (US) catalyzed 2,2,6,6-tetramethylepiperidin-1-oxyl (TEMPO) system (US-TEMPO-system) at five different temperatures – 5, 15, 25, 35, and 45°C and two pH ranges, 8.5-9.0 and 10.0-10.5 – to obtain the optimum reaction conditions. The reaction pH and temperature have significant effect on the kinetics of the formation of carboxylate in the oxidized pulps and produce depolymerization at temperatures greater than 25°C. Formation of carboxylate on the cellulose chain is directly proportional to the NaBr concentration. The pulp oxidized by the US-TEMPO-system at 25°C had 10-15% more carboxyls and showed a ca. 10% increase in the nanocellulose yield when compared to the TEMPO-system without sono-catalysis.
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