Abstract: This invention presents preparation, characterization and evaluation of an efficient heterogeneous Fe (III)-HY catalyst for photo-assisted Fenton reaction. Fe (III) ions are immobilized on HY zeolite using different loadings by impregnation, calcination and the activity of the catalyst is evaluated by the degradation of phenol. The effect of Fe loadings, H2O2 concentration, pH and quenching on photo-Fenton reaction are studied. The results obtained clearly show that Fe (III)-HY is efficient in the degradation of phenol and it is compared with that of a homogeneous photo-Fenton reaction. The increased rate of reaction on Fe (III)-HY highlights the synergistic role of zeolite. Heterogeneous Fe (III)-HY in photo-Fenton reaction allows a wide range of pH for reaction against the narrow pH range in homogeneous system. The system is further subjected to evaluate its stability in solid state. The stability of the catalyst is further established by recycling studies.