Influence of mechanical pretreatment to isolate cellulose nanocrystals by sulfuric acid hydrolysis

The mechanical pretreatments intensities on characteristics of cellulose nanocrystals (CNC) prior to acid hydrolysis was evaluated. The cellulose was submitted to mechanical pretreatment as: magnetic stirring (CNCst), blending (CNCbl) or grinding by 20 (CNC20x) and 40 (CNC40x) passages in a super mass colloid mill. Then, all samples were submitted to H2SO4 hydrolysis and the CNC were evaluated by total mass yield (TMY%), rheological behavior, size distribution for width/length (WD), crystallinity index (CI%), OSO3− substitution degree (SD) and zeta potential (ζ). After hydrolysis samples exhibited the same SD (190 ± 5 mMol·kg−1), ζ (−55 ± 3 mV) and CI% (65 ± 2), differing only in TMY% and WD. The CNCst showed TMY% of 85%, WD of 8 ± 5 nm and 100–800 nm, with presence of cellulose nanofibers (CNF), suggesting incomplete hydrolysis. The CNCbl and CNC20x revealed TMY% of 65 ± 1, but differed in WD of 8 ± 5 nm and 300 ± 200 nm and 8 ± 5 nm and 200 ± 170 nm, respectively. The results showed that the grinding mechanical pretreatment is mandatory for CNF isolation, but not for CNC. Stability profile after the hydrolytic procedure, CI%, morphology and similar character generated CNC with adequate features and good yield, by simple mechanical stirring or blending, reducing the production's cost and allowing industrial-scale production.