The use of TiO2 nanoparticles for photocatalysis for the degradation of organic dyes under UV light for wastewater treatment has been widely studied. However, the photocatalytic characteristics of TiO2 nanoparticles are inadequate due to their UV light response and higher band gap. In this work, three nanoparticles were synthesized: (i) TiO2 nanoparticle was synthesized by a sol-gel process. (ii) ZrO2 was prepared using a solution combustion process and (iii) mixed-phase TiO2–ZrO2 nanoparticles were synthesized by a sol-gel process to remove Eosin Yellow (EY) from aqueous solutions in the wastewater. XRD, FTIR, UV-VIS, TEM, and XPS analysis methods were used to examine the properties of the synthesized products. The XRD investigation supported the tetragonal and monoclinic crystal structures of the TiO2 and ZrO2 nanoparticles. TEM studies identified that mixed-phase TiO2–ZrO2 nanoparticles have the same tetragonal structure as pure mixed-phase. The degradation of Eosin Yellow (EY) was examined using TiO2, ZrO2, and mixed-phase TiO2–ZrO2 nanoparticles under visible light. The results confirmed that the mixed-phase TiO2–ZrO2nanoparticles show a higher level of photocatalytic activity, and the process is accomplished at a high degradation rate in lesser time and at a lower power intensity.