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Miscanthus x giganteus stalks were used to make organosolvent pulp and nanocellulose. The organosolvent miscanthus pulp (OMP) was obtained through thermal treatment in the mixture of glacial acetic acid and hydrogen peroxide at the first stage and the alkaline treatment at the second stage. Hydrolysis of the never-dried OМP was carried out by a solution of sulfuric acid with concentrations of 43% and 50% and followed by ultrasound treatment. Structural changes and the crystallinity index of OMP and nanocellulose were studied by SEM and FTIR methods. X-ray diffraction analysis confirmed an increase in the crystallinity of OMP and nanocellulose as a result of thermochemical treatment. We show that nanocellulose has a density of up to 1.6 g/cm3, transparency up to 82%, and a crystallinity index of 76.5%. The AFM method showed that the particles of nanocellulose have a diameter in the range from 10 to 20 nm. A thermogravimetric analysis confirmed that nanocellulose films have a denser structure and lower mass loss in the temperature range of 320–440°C compared to OMP. The obtained nanocellulose films have high tensile strength up to 195 MPa. The nanocellulose obtained from OMP exhibits the improved properties for the preparation of new nanocomposite materials.

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