Abstract:We focused on preparing cellulose nanofibrils by purification, separation, and mechanical treatment of Kombucha membranes (KM) resulted as secondary product from beverage production by fermentation of tea broth with symbiotic culture of bacteria and yeast (SCOBY). We purified KM using two alkaline solutions, 1 and 4 M NaOH, which afterwards were subjected to various mechanical treatments. Transmission electron microscopy (TEM), scanning electron microscopy (SEM), dynamic light scattering (DLS), X-ray diffraction (XRD), X-ray fluorescence (XRF), Fourier-transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA) were employed to evaluate the purification degree, the size and aspect of cellulose fibrils after each treatment step, the physical-chemical properties of intermediary and final product, and for comparison with micro-crystalline cellulose from wooden sources. We determined that 1 M NaOH solution leads to approx. 85% purification, while a higher concentration assures almost 97% impurities removal. XRD analysis evidenced an increase in crystallinity from 37% to 87% after purification, the characteristic diffractograms of Iα and Iβ cellulose allomorphs, and a further decrease in crystallinity to 46% after microfluidization, fact correlated with a drastically decrease in fibrils' size. FTIR analysis evidenced the appearance of new chain ends by specific transmission bands at 2941 and 2843 cm −1 .