This work reports the synthesis of a variety of materials with an ilmenite-type structure MTiO 3 formula, where M= Fe, Co, and Ni, these materials were synthesized by the method of solvo-combustion, a simple and rapid method. These materials were characterized by X-ray Diffraction (XRD), scanning electron microscopy (SEM), FT-IR spectroscopy, thermogravimetric analysis (TGA/DTA), surface area determination by the BET method and analysis of particle size. The photocatalytic activity was measured in the degradation reactions of Rhodamine B (rhB) and tetracycline (TC). The results show that the crystallinity and surface area are factors that influence significantly on the photocatalytic activity of the synthesized titanates.