The influence of acid hydrolysis conditions on cellulose nanowhiskers (CNW) made from moso bamboo (Phyllostachys edulis) was investigated in this study. Procedures with or without an alcohol–toluene extraction were tested using different acid concentrations and hydrolysis durations. The alcohol–toluene extract had no significant effect on the properties of bamboo cellulose nanowhiskers (BCNW). According to the results, a sulfuric acid concentration of 46% with 2 h of hydrolysis and a concentration of 55% with 1 h of hydrolysis were ideal for preparing BCNW because the product had a relatively high crystallinity index. In addition, the surface functional groups of the products obtained from different sulfuric acid hydrolysis conditions were similar. However, groups treated with lower acid concentrations exhibited slightly stronger thermal stability than those treated with higher acid concentrations.
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