Acid hydrolysis pretreatment of lignocellulosic fibers with ferric chloride hexahydrate (FeCl3·6H2O) enables economical and environmentally friendly production of cellulose nanocrystals (CNCs). Preparation Process · During the treatment of molten FeCl3·6H2O, the degree of polymerization (DP) of cellulose fibers decreased sharply, and at the same time cellulose I transformed into cellulose II microcrystals. · Molten FeCl3·6H2O rapidly hydrolyzes cellulose fibers within 5 minutes at 80°C, resulting in a rapid decrease in polymerization from 922 to 196 and a water-insoluble solid (WIS) retention rate of 80.1%. · CNCs were successfully produced from the mechanical disintegration of the WIS with a low energy input. Hence, the yield of CNCs is consistent with that of the WIS. · Moreover, FeCl3·6H2O was easily recycled from the hydrolysate after hydrolysis, with a high recovery of 94.0-94.5 wt %, using simple concentration and crystallization technologies.
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