Nanofibrillation of alkyl ketene dimer (AKD)-treated cellulose in tetrahydrofuran

A hardwood bleached kraft pulp (HBKP) was reacted with alkyl ketene dimer (AKD) under solvent-free and heterogeneous conditions, and a fibrous chloroform-insoluble fraction with a degree of substitution of AKD β-ketoester groups of 0.75 was obtained at a weight ratio of 95 % of the total reaction product. When this AKD-treated and CHCl₃-insoluble HBKP was mechanically disintegrated in tetrahydrofuran, the suspension turned to a viscous and translucent gel. When an unfibrillated fraction was removed by filtration using a glass filter with 40 μm pore size, the weight recovery ratio of the filter-passed fraction was approximately 30 %. Scanning and transmission electron microphotographs of the glass filter-passed fraction showed that this fraction consisted of cellulose nanofibrils more than several micrometers in length, the surfaces of which probably had AKD β-ketoesters in high densities.