: Herein, we report the unique property of MOF as a photo catalyst: ferrocene (Fc) based Co-MOF (probe R1) prepared by a simple method was able to react with H2O2 to achieve high efficiency in photocatalytic Fenton process. In selective heterogeneous Fenton process using Fc based Co-MOF; the results suggest that the combination of Fe2+/Fe3+ cation and H2O2 can significantly improve the photocatalytic proficiency at room temperature. It could completely remove MO azo dye in the presence of a certain amount of H2O2 under visible light within 40 minutes. The activity performed by varying different parameters, such as dye and catalyst concentration, pH, H2O2 dosage. MOF catalyst shows better adsorption at acidic medium. When the quantity of photo catalyst R1 increased, then the decolorization of the azo dyes enhanced. The degradation diminishes with increasing the concentration of dyes as well as pH range. This work reveals that Fc based Co-MOF materials hold countless potential for assertions in the field of radiation-energy exchange into chemical energy. The photo catalyst probe-R1 perceived that was a perfect photo catalyst from the degradation/adsorption of Methyl Orange in the presence of visible radiation.