Department of Chemistry, Amirkabir University of Technology, Tehran, Iran Department of Nanomaterials and Nanotechnology, Institute for Color Science and Technology, Tehran, Iran E-mail : gharagozlou@icrc.ac.ir Fa.x : 98-21-22947537 Department of Polymer and Color Engineering, Amirkabir University of Technology, Tehran, Iran Department of Organic Colorants, Institute for Color Science and Technology, Tehran, Iran Manuscript received online 23 April 2012, revised 18 June 2012, accepted 19 June 2012 In this paper, the visible light photocatalytic activity of nanocrystalline TiO2 impregnated with metal-free phthalocyanine pigment (Pc) in aqueous suspension for methyl orange photodegradation has been investigated. For the preparation of the TiO2 impregnated with phthalocyanine, TiO2/(Pc), first TiO2 nanoparticles was prepared by the solgel method and calcined at 400 °C. Then nanocrystalline TiO2/(Pc) was synthesized via the chemical precipitation method and characterized by X-ray diffraction (XRD), diffuse reflectance spectroscopy (DRS), Fourier transformed infrared (FTIR) and transmission electron microscopy (TEM) techniques. Results revealed that the nanocrystalline TiO2/(Pc) possesses the anatase structure with the average particle size of about 20-25 nm. The absorption edge of the synthesized TiO2/ (Pc) has been shifted significantly into the visible region. Our results revealed the photocatalytic activity of TiO2/(Pc) increased efficiently than TiO2 nanoparticles under the visible light. Therefore, synthesized nanocrystalline TiO2/(Pc) is a suitable photocatalyst for use under visible light which make the applicability of TiO2 photocatalysis even more versatile.