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Nano Fe-BTC/graphene oxide (GO) composites were successfully synthesized by hydrothermal treatment with a microwave-assisted method. Samples were characterized by X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), N2 adsorption–desorption, Scanning electron microscopy (SEM), Energy-dispersive X-ray spectroscopy (EDS), and Ultraviolet–visible diffuse reflection spectroscopy (UV–Vis DRS). SEM image of Fe-BTC/GO-30 showed the particle size of 30–50 nm on the GO surface. From the UV–Vis diffuse reflectance spectra, it revealed that nano Fe-BTC/GO composite absorbed the wavelengths in the visible light region with a low bandgap energy of 2.2–2.45 eV. Fe-BTC/GO nanocomposites were tested for the photocatalytic degradation of reactive yellow 145 (RY-145) in aqueous solution. Fe-BTC/GO composites exhibited high photocatalytic activity. Thus, at pH of 3 and high initial concentration of 100 mg RY-145/L, removal efficiency reached the value of 98.18% after 60 min. of reaction. In comparison with Fe-BTC/GO synthesized by the solvothermal method, nano Fe-BTC/GO showed much higher RY-145 removal efficiency. Moreover, this Fe-BTC/GO-30 showed high catalytic activity stability and could be reused, opening the high potential application of this promising photo-Fenton catalyst in photocatalytic degradation of organic pollutants from aqueous solution. [ABSTRACT FROM AUTHOR]