In the present work, degradation of methylene blue (MB) dye in aqueous solution through H₂O ₂and iron doped g-C₃N₄ (Fe-g-C₃N₄) was studied. The hybrid was fabricated by thermal polymerization with iron (III) nitrate nonahydrate and melamine, and it was characterized by X-ray diffraction, Fourier transform infrared, UV-Vis diffuse reflectance spectrum, X-ray photoelectron spectroscopy, transmission electron microscope and Brunner-Emmet-Teller. The various experimental conditions such as doping amount, a dose of the sample, solution pH, the addition of H₂O₂, and concentration of MB on the degradation of MB dye were optimized. The maximum extent of degradation of methylene blue was obtained at pH 5, doping amount of 2.7 wt% and dose of 0.07 g. The molar ratio of Fe:H₂O₂ is 1:1000 showed 99% of MB (30 mg/L) decolorization over 60 min. The hybrid showed good stability and recyclability after three cycles of use. Photo-Fenton reaction exhibited a higher synergetic effect than the combination of Fenton and photocatalytic process.