Samples of the bimetallic-based NH2-MIL-125(Ti) at a ratio of Mn+/Ti4+ is 0.15 (Mn+: Ni2+, Co2+ and Fe3+) were first synthesized using the solvothermal method. Their fundamental properties were analyzed by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Raman spectra, scanning electron microscopy (SEM), N2 adsorption–desorption measurements, and UV–Vis diffuse reflectance spectroscopy (UV-Vis DRS). The as-acquired materials were used as high-efficiency heterogeneous photocatalysts to remove Rhodamine B (RhB) dye under visible light. The results verified that 82.4% of the RhB (3 × 10−5 M) was degraded within 120 min by 15% Fe/Ti−MOFs. Furthermore, in the purpose of degrading Rhodamine B (RhB), the rate constant for the 15% Fe/Ti-MOFs was found to be 2.6 times as fast as that of NH2-MIL-125(Ti). Moreover, the 15% Fe/Ti-MOFs photocatalysts remained stable after three consecutive cycles. The trapping test demonstrated that the major active species in the degradation of the RhB process were hydroxyl radicals (HO∙) and holes (h+).
