The research article discusses a new method for the photocatalyst synthesis based on a mixture of titanium oxide - titanium oxyfluoride. The synthesis was performed by dissolving titanium metal in an acidified solution of ammonium bifluoride, followed by oxidation to the highest oxidation state and hydrolysis with ammonia to obtain metatitanic acid. The decomposition of metatitanic acid was carried out in a muffle furnace at a temperature of 380°C. It was found that during the precipitation of metatitanic acid, the titanium compound with the fluoride ion also passes into the precipitate, which, after calcination, transforms into titanium oxyfluoride. Photocatalytic activity was determined by the oxidation reaction of the methyl orange dye upon irradiation with ultraviolet radiation. The source of ultraviolet radiation was a DRT-125 lamp with a wavelength in the range of 200-400 nm. Suspensions containing 60 mg/L of the dye and various contents of the photocatalyst in the concentration range of 1-7 g/L were subjected to oxidation. The construction of the calibration graph and the determination of the concentrations were carried out on an SF-2000 spectrophotometer at a wavelength of 466.4 nm. The operating wavelength was determined by scanning the solution in the wavelength range of 200-800 nm. It was found that as a result of oxidation, the solution pH shifts to the acidic side to 3.5, which leads to a shift in the wavelength of the maximum absorption; in this regard, the solutions pH was adjusted to the same values.