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Anatase/brookite nanocomposites were fabricated by the classical method of hydrolysis, additionally using hydrothermal treatment of preformed titanium dioxide sol with tetrabutyl orthotitanate. The influence of hydrothermal processing the buffer solution of TiO2 synthesis on the average particle sizes, specific surface area, pore sizes distributions, optical and photocatalytic properties investigated by X-ray diffraction, low-temperature nitrogen adsorption and UV-Vis spectroscopy. It has been determined that the hydrothermal treatment of pre-prepared titania sol as hydrolysis product leads to rutile formation after annealing at 400°C. Respective model of forming anatase/brookite/rutile nanocomposites was proposed. The changes of bang gap energy of TiO2 were observed and explained by effect of change phase composition and particles size of nanocomposite particles. Methylene blue (MB) photo-oxidation reactions using titanium dioxide nanocomposite were analyzed. Maximal photocatalytic activity of MB oxidation was detected for material with the ratio of the titania phases (anatase : brookite : rutile – 2 : 2 : 1). Synergistic effect between crystallinity, phase ratio, morphology of oxide material, band gap and photocatalytic activity in the anatase/brookite nanocomposites was established.