TiO2/Zr nano photocatalyst is obtained with various trace amount of Zr by employing the sol-gel method. Several spectroscopic techniques are applied to characterize the structures and properties of nano photocatalyst. It is found that the effect of doping Zr ions to the TiO2 lattice led to improving the surface properties and decreasing the particle size of nano photocatalyst. Therefore, it causes increasing specific surface area and photocatalytic activity as compared with pure TiO2. The photocatalytic activity of the nano photocatalyst is employed for the degradation of Methyl Orange as organic waste in the aqueous solution under UV irradiation in a batch reactor.