Impact of mechanical and enzymatic pretreatments on softwood pulp fiber wall structure studied with NMR spectroscopy and X-ray scattering
2015
Virtanen, Tommi | Penttilä, Paavo A. | Maloney, Thaddeus C. | Grönqvist, Stina | Kamppuri, Taina | Vehviläinen, Marianna | Serimaa, Ritva | Maunu, Sirkka Liisa
Dissolution of wood pulp can be enhanced by applying certain pretreatments before exposing the fibers to solvents. We have analyzed effect of mechanical and enzymatic pretreatments on softwood fiber wall structure using nuclear magnetic resonance (NMR) spectroscopic methods, small and wide angle X-ray scattering (SAXS, WAXS). NMR diffusometry was used to estimate the effect of pretreatments on average pore sizes at micrometer size scale and for the connectivity of the porous network. A proton NMR experiment was used to quantify the nonfreezing water content inside the fiber wall, and solid state NMR 13C cross polarization (CP) magic angle spinning (MAS) spectroscopy was used to observe the effect of pretreatments on crystallinity and lateral fibril dimensions of cellulose fibrils, and in combination with fiber saturation point measurement to calculate the average pore size at nanometer size scale. Both WAXS and CP–MAS NMR experiments confirmed that there were no changes in crystallinity nor in fibril lateral dimensions due to pretreatments. The pretreatments caused an increase in the amount of nonfreezing water, suggesting an opening of the pore system. According to diffusion experiments there are only minor changes in micrometer scale pore network due to pretreatments. SAXS results indicated that enzymatic treatment increased the microfibrillar distance, and there was also an increase in cross relaxation rate of magnetization from water to cellulose protons as observed by NMR. These were interpreted to be due to opening of microfibrillar bundles, leading to an increased accessibility of water.
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