Nowadays there is great empathy from society for products from renewable resources, due to growing awareness of the finiteness of natural resources. A very common residue of agribusiness and generated on a large scale, being largely discarded in landfills, is coconut shell. With the objective of giving a benefit to this residue, this work tried different methods to isolate the nanocellulose derived from coconut fiber and characterized the products of the different stages of the extraction process. The methodology, which achieved the best results, was the one which did the mercerization with NaOH until the remaining liquor does not look like a black liquor anymore. After that, the bleaching was made twice with H2O2 and NaOH and the hydrolysis was carried with sulfuric acid. Subsequent steps aimed to remove the acid from the fibers. The centrifugation was made and supernatant was removed, followed by dialysis until the external medium reached neutral pH. The final dispersion of nanocellulose in aqueous medium was performed using ultrasound. The characterizations of hydrolyzed cellulose and the products of the process steps was performed by TGA analysis; by X-ray diffraction and scanning electron microscopy. The thermal stabilities were determined from the obtained nanocellulose, their respective indices of crystallinity and crystal size achieved and the effects of the different treatments tested. The chemical structure of the generated effluent from the isolation of the nanocellulose black liquor was attested by FTIR.