AbstractThe objective of this research was to evaluate an all-chemical process to prepare nano-scale to macro-scale cellulosic fibers from kenaf bast fibers, for polymer composite reinforcement. The procedure used in this all-chemical process included alkaline retting to obtain single cellulosic retted fiber, bleaching treatment to obtain delignified bleached fiber, and acidic hydrolysis to obtain both pure-cellulose microfiber and cellulose nanowhisker (CNW). At each step of this chemical process, the resultant fibers were characterized for crystallinity using X-ray diffraction (XRD), for functional groups using the Fourier Transform Infrared spectroscopy (FTIR), and for surface morphology using both the scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The chemical components of the different scale fibers were analyzed. Based on the raw kenaf bast fibers, the yields of retted fibers and bleached fibers were 44.6% and 41.4%. The yield of the pure cellulose microfibers was 26.3%. The yield of CNWs was 10.4%, where about 22.6% α-cellulose had been converted into CNWs. The fiber crystallinity increased as the scale of the fiber decreased, from 49.9% (retted single fibers) to 83.9% (CNWs). The CNWs had fiber lengths of 100 nm to 1400 nm, diameters of 7 to 84 nm, and aspect ratios of 10 to 50. The incorporation of 9% (wt%) CNWs in polyvinyl alcohol (PVA) composites increased the tensile strength by 46%.