Enhancement of the production of TEMPO-mediated oxidation cellulose nanofibrils by kneading

The industrial use of TEMPO-mediated oxidation (TMO) reaction to produce highly fibrillated cellulose nanofibrils has been hindered by high catalyst costs, long reaction times and high reaction volumes. The hypothesis that cellulose concentration during TMO process is key to increase the process of efficiency has been confirmed. The novelty of this research is the proof-of-concept for a significant enhancement of the TMO reaction by kneading the cellulose to work in concentrations above 120 g/L. Results show that the increase of the cellulose concentration in the TMO reaction, from the traditional 10 g/L to 120 g/L, increase not only the production for the same reaction volume (1200 %) but also the pulp recovery (up to 94 %). Moreover, the oxidation time can be reduced from 42 min to only 4 min while properties of both the oxidized pulps and the final nanocellulose are similar. On the other hand, the use of buffers in the TMO reaction allows us to keep the pH constant without using NaOH, and to improve the selectivity of the carboxyl groups production. The proposed process also minimizes the final environmental impact.