Microfibrillated lignocellulose (MFLC) and nanopaper films from unbleached kraft softwood pulp

Microfibrillated cellulose (MFC) is an important industrial nanocellulose product and material component. New MFC grades can widen the materials property range and improve product tailoring. Microfibrillated lignocellulose (MFLC) is investigated, with the hypothesis that there is an optimum in lignin content of unbleached wood pulp fibre with respect to nanofibril yield. A series of kraft fibres with falling Kappa numbers (lower lignin content) was prepared. Fibres were beaten and fibrillated into MFLC by high-pressure microfluidization. Nano-sized fractions of fibrils were separated using centrifugation. Lignin content and carbohydrate analysis, total charge, FE-SEM, TEM microscopy and suspension rheology characterization were carried out. Fibres with Kappa number 65 (11% lignin) combined high lignin content with ease of fibrillation. This confirms an optimum in nanofibril yield as a function of lignin content, and mechanisms are discussed. MFLC from these fibres contained a 40–60 wt% fraction of nano-sized fibrils with widths in the range of 2.5–70 nm. Despite the large size distribution, data for modulus and tensile strength of MFLC films with 11% lignin were as high as 14 GPa and 240 MPa. MFLC films showed improved water contact angle of 84–88°, compared to neat MFC films (< 50°). All MFLC films showed substantial optical transmittance, and the fraction of haze scattering strongly correlated with defect content in the form of coarse fibrils. Graphic abstract

Characterization of Cellulase-Treated Fibers and Resulting Cellulose Nanocrystals Generated through Acid Hydrolysis

Integrating enzymatic treatment and acid hydrolysis potentially improves the economics of cellulose nanocrystal (CNC) production and demonstrates a sustainable cellulosic ethanol co-generation strategy. In this study, the effect of enzymatic treatment on filter paper and wood pulp fibers, and CNCs generated via subsequent acid hydrolysis were assessed. Characterization was performed using a pulp quality monitoring system, scanning and transmission electron microscopies, dynamic light scattering, X-ray diffraction, and thermogravimetric analysis. Enzymatic treatment partially reduced fiber length, but caused swelling, indicating simultaneous fragmentation and layer erosion. Preferential hydrolysis of less ordered cellulose by cellulases slightly improved the crystallinity index of filter paper fiber from 86% to 88%, though no change was observed for wood pulp fibre. All CNC colloids were stable with zeta potential values below −39 mV and hydrodynamic diameters ranging from 205 to 294 nm. Furthermore, the temperature for the peak rate of CNC thermal degradation was generally not affected by enzymatic treatment. These findings demonstrate that CNCs of comparable quality can be produced from an enzymatically-mediated acid hydrolysis biorefining strategy that co-generates fermentable sugars for biofuel production.