Novel ZnIn2S4/FeUiO-66 (ZFeU) photocatalyst with different proportion of FeUiO-66 has been successfully prepared by a facile one-pot solvothermal reaction. The as-synthesized nanocomposites have been thoroughly characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform-infrared spectroscopy (FT-IR), UV-Vis diffuse reflectance spectroscopy (UV-Vis DRS), Brunauer–Emmett–Teller (BET) characterization, photoluminescence (PL) analysis and electrochemical impedance spectrum (EIS). The photocatalytic performance of ZFeU nanocomposites for the photodegradation of RhB under visible light irradiation was better than that of ZnIn2S4 and FeUiO-66 alone. The experiment results showed the 20% ZFeU nanocomposites had the best photocatalytic properties. At the same time, a probable mechanism was discussed and it was believed that introduction of FeUiO-66 on ZnIn2S4 would minimize the recombination of photogenerated electron-hole pairs, leading to the enhancement of the photocatalytic activity. Novel ZnIn2S4/FeUiO-66 was synthesized by solvothermal reaction. The photocatalytic performance of ZnIn2S4/FeUiO-66 was better than ZnIn2S4 and FeUiO-66 for the photodegradation of RhB under visible light irradiation. The experiment results showed that the 20% ZnIn2S4/FeUiO-66 exhibited the optimal photocatalytic performance. The •O2– and h+ played an important role for the degradation. [ABSTRACT FROM AUTHOR]