The purpose of this paper was analyzing the chemical degradation of Methyl Orange in water via "Photo-Fenton reaction. CuO - Attapulgite nano particles have been used as coating in an internal dike surface of the reactor. The degradation of MO dye has been predestined to be discovered by the catalytic work of CuO- Attapulgite synthesized surface in a turnout of hydrogen peroxide and UV light. Nanoparticles have been described by SEM, EDX, AFM and XRD. MO dye solution with 5 ppm initial concentration was decreased by 100% under the condition of (2.5ml H2O2), (temperature =25°C), (pH= 7) within (3 min). The remaining was observed in the solution via high-performance-liquid chromatography (HPLC). Each overhead state was calculated to reach an optimum working condition for the method (photo - Fenton). The Methyl orange degradation method has pursued first - order reaction basics. Photo - Fenton method caused a more effective oxidation average. The photo - Fenton"degradation was found to be an efficient and economical method via making higher proportion of mineralization and degradation in short time radiation.