This study describes the application of novel chemistry methods for the removal of dye by nano-structured titanium oxide (TiO2) photocatalysts. Such materials can be applied in the development of efficient photocatalytic systems for the treatment of water. Nanocrystalline TiO2 was synthesized by Sol-Gel route using titanium tetraisopropoxide as a metal precursor. The catalysts were characterized by X-ray diffraction (XRD), Transmission Electron Microoscopy (TEM), Fourier-transform infrared spectroscopy (FT-IR). Synthesized TiO2 was related to anatase phase and crystalline structure was characterized by XRD. Cuboidal and uneven shape of TiO2 nanoparticles were observed by TEM images. FTIR reveals the functional groups present in the synthesized TiO2 nanoparticles. Thus synthesized TiO2 nanoparticle was used for photocatalytic degradation of methyl orange. The photodegradation of methyl orange (MO) dye, is examined both under different dye concentration(10,20,30 and 40 ppm) and amounts of TiO2 (5,10,15 and 20 mg / 10 ml).After 15W UV-365 nm irradiation for 3 h, ca. 99.9% of MO was degraded with addition of 20mg TiO2 to solutions containing 40ppmdye. The photodegradationmechanism of the quinonoidal methyl orange using nanoparticles is low cost, ecofriendly and cost effective process in the removal of toxic dyes.