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This study aimed to determine the photocatalytic activity of photo-Fenton reagent in the photodegradation of 4-Nitrophenol. For this purpose, Fe(III) tetraphenyl porphyrin encapsulated NaY zeolite (FeTPP/NaY) was successfully synthesised via the zeolite synthesis method. The effects of catalyst amount, H2O2 and UV illumination, concentration of 4-Nitrophenol and pH value on the photodegradation process were examined. Ultraviolet–Visible spectroscopy studies revealed that catechol, benzoquinone, and nitrate as the key intermediate species for photodegradation of 4-Nitrophenol. The chemical oxygen demand analysis indicated mineralisation of pollutant which exhibits 85% conversion of 4-Nitrophenol after 120 min irradiation.