In this work, nanocellulose was extracted from bleached corncob residue (CCR), an underutilized lignocellulose waste from furfural industry, using four different methods (i.e. sulfuric acid hydrolysis, formic acid
(FA) hydrolysis, 2,2,6,6-tetramethylpiperidine-1-oxyl (TEMPO)-mediated oxidation, and pulp refining,
respectively). The self-assembled structure, morphology, dimension, crystallinity, chemical structure and
thermal stability of prepared nanocellulose were investigated. FA hydrolysis produced longer cellulose
nanocrystals (CNCs) than the one obtained by sulfuric acid hydrolysis, and resulted in high crystallinity
and thermal stability due to its preferential degradation of amorphous cellulose and lignin. The cellulose
nanofibrils (CNFs) with fine and individualized structure could be isolated by TEMPO-mediated oxidation. In comparison with other nanocellulose products, the intensive pulp refining led to the CNFs with
the longest length and the thickest diameter. This comparative study can help to provide an insight into
the utilization of CCR as a potential source for nanocellulose production.