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A Fenton-like System (Cu(II)/H2O2) for the Preparation of Cellulose Nanocrystals with a Slightly Modified Surface

A preparation process of cellulose nanocrystals using a Fenton-like system was presented. Rod-shaped cellulose nanocrystals were isolated after treatment in the H2O2/acetic acid/2–6 mol % copper acetate system. The morphology and sizes of rod-shaped particles were determined by AFM (atomic force microscopy) and cryo-EM (cryo-electron microscopy). X-ray diffraction proves that the prepared particles have a natural polymorphic modification of cellulose I with a high crystallinity index. Thermogravimetry data indicates a slight decrease in thermal stability of the particles when compared to starting cellulose, correlating with an increase in the number of carbonyl groups determined by chemical analysis. Using pK spectroscopy, active acid–base surface sites (pKi 5.5 and 7.9) were quantitatively determined. The cellulose nanoparticles formed stable hydrosols. Using photometry and dynamic light scattering, it has been established that the critical concentration of coagulation of sols is 76 mM KCl.