Abstract: Visible light responsive MoS₂/Sb₂S₃ composite photocatalyst was successfully designed and constructed by a simple one-step hydrothermal process. XRD, SEM, UV-vis diffuse reflectance spectroscopy (UV-Vis DRS) and XPS were used to characterize its photocatalytic activity. The degradation experiment was conducted with rhodamine B (RhB) as the target pollutant. Compared with the pure Sb₂S₃ and MoS₂, the MoS₂/Sb₂S₃ composite photocatalyst exhibits highly enhanced efficiency in the degradation of RhB, showing excellent adsorption performance and photocatalytic performance. Compared with TiO₂, Bi₂S₃, C₃N₄ and Sb₂S₃, MoS₂/Sb₂S₃ composite photocatalyst is possessed as more excellent photocatalyst under the same experimental conditions. In addition, the photocatalytic degradation mechanism was carried on the exploration. This research expounds the mechanism of photocatalytic reaction, and provides a application for the photocatalyst preparation methods of degradation high concentration organic wastewater, which has certain application value.