As pointed above, sulfuric acid hydrolysis leads to reduced thermal stability of acid hydrolyzed CNC compared to that of neat cellulosic feedstock. However, this effect can be diminished by neutralizing the CNCH2SO4 with NaOH solution (~1% NaOH). After neutralization with NaOH, no acid sulfate groups remained, and the thermal stability of neutralized CNCCr(NO3)3 was shifted to a higher temperature. However, the presently used method for isolating the CNCCr(NO3)3 has some restrictions, such as prolonged production time and capital cost in order to remove the free sulfuric acid remaining on the CNCCr(NO3)3 surface after hydrolysis process, for their use in industrial scale. Thus far, the residual sulfuric acid in the cellulosic fiber is usually eliminated by the dialysis process against water until neutral pH is achieved, which is a costly procedure and usually takes a long time (3–7 days) . Some studies reported that the presence of the divalent group (SO42−) or anionic (–OSO2O–) of HSO4 and sulfates on the surface of nanocellulose may significantly reduce the interaction of cellulose fibrils with other polymer and biopolymer materials . Even if the chemical neutralization method is simpler with less processing steps to produce unsulfated CNCH2SO4 than time-consuming dialysis process, the large amount of waste effluents (salts) produced during the neutralization process needs to be further recycled before being discharged into the local waterway or ecological system. In fact, the sulfur content is only able to affect the thermal behavior of the nanocellulose, but maybe not influence or cause a negative effect on the crystallinity of the H2SO4 hydrolyzed CNC . In this study, the thermal degradation pattern of neutralized CNCH2SO4 was similar as native cellulose and CNCCr(NO3)3, in which the low-temperature degradation peak in the DTG curve disappeared completely after neutralization. The neutralized CNCH2SO4 started to degrade at the temperature of ca. 237 °C. As expected, the Tmax value of neutralized CNCH2SO4 profoundly increased to 349 °C, which can be explained by two main reasons. First, the absence of amorphous regions in the treated cellulose matrix and the highly structured crystals segments rendered the higher-temperature degradation. Second, the replacement of hydrogen ions (H+) from acid hydrolysis by alkaline ion (Na+) inhibited the dehydration catalyzed by H2SO4 .