The new microparticles, 2-formylthiophene (FT)/TiO2 and (E)-1,2-bis(5-formyl-2-thienyl) ethylene (EBFTE)/TiO2 were synthesized with a silane coupling agent. The prepared TiO2 composites were characterized using Ultraviolet-Vis absorption (UV-Vis), X-ray diffraction (XRD), scanning electron microscope (SEM) and thermogravimetric analyzer (TGA). Methylene blue was used as a model material to examine the photocatalytic activities of the prepared catalysts under both Ultraviolet-Vis (UV) and visible (Vis) light. The enhanced photocatalytic activities were observed in the presence of (FT)/TiO2 and EBFTE/TiO2 under Vis light. It suggests that FT or EBFTE plays a block or active role in the photodegradation mechanisms under UV and Vis light irradiation, respectively.