Abstract: Mixed cobalt and nickel oxides MTiO3/TiO2 (M = Co2+, Ni2+) are synthesized. Organometallic complexes of titanium tetrabutylate Ti(OBu)4 with 1,2-dihydroxybenzene and nitrate hydrates of corresponding metals (M) synthesized under conditions of the modified sol-gel process are used as precursors. The synthesized samples are characterized by field-emission scanning electron microscopy, energy-dispersive X-ray analysis, diffuse reflectance spectroscopy, dispersive X-ray radiation analysis, X-ray diffraction, and low-temperature nitrogen adsorption. The photocatalytic activity of the samples is tested in the ultraviolet spectral range (200 nm < λ < 400 nm) in the photodegradation of 1,2-dihydroxybenzene (catechol) in aqueous solutions. © 2020, Pleiades Publishing, Ltd.