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.