Isolation of cellulose microfibers and nanofibers by mechanical fibrillation in a water-free solvent

Abstract

Cellulose from vegetable sources is the most abundant biopolymer on earth. In plants, cellulose is a reinforcement element that conforms to a hierarchical structure. Cellulose micro-/nanofibers can be isolated from the cell wall by top-down strategies involving mechanical processes to be used in applications as a reinforcing material. Nonetheless, its use has been limited as its extraction in an aqueous medium is unfavorable when employed in low-hydrophilic matrices. Therefore, this work proposes a novel homogenization route in which cellulose micro-/nanofibers are directly obtained and dispersed in propylene glycol (PG), which generates more possibilities for these (nano) structures in applications that require water-free environments. Moreover, the influence on the cycle numbers in the morphological, chemical, thermal, and rheological properties was researched. Thus, the obtained micro-/nanofibers presented TEM diameters even below 20 nm. XRD analysis evidenced crystalline planes located at 1 1 ¯ 0 , 110, and 200, and crystallinity degree values up to 80%. Also, FTIR spectra bands in 3340 cm−1, 2890 cm−1, 1314 cm−1, and in the fingerprint region corresponded to native cellulose Iβ. FTIR and TGA confirmed no influence of mechanical cycles on cellulose fibers’ chemical and thermal properties. Furthermore, the increase in the cycle number evidenced a shear-thinning rheological behavior of the suspensions. Considering the above results, it was concluded that the proposed high-pressure homogenization within PG is an approach for vegetable nanocellulose homogenization while maintaining high crystallinity, thermal, and chemical features with huge importance for subsequent processes in the development of nanocomposites with hydrophilic matrices for industrial applications. Graphical abstract: [Figure not available: see fulltext.]