Abstract: In this work, MoS₂ was prepared using a high temperature molten salt electrolysis. In order to improve the adsorption performance of MoS₂ for U(Ⅵ), Mn₂O₃ was blended on molybdenum disulfide substrate. The laminar structure of MoS2 effectively dispersed the agglomeration of Mn₂O₃ and introduced uranophilic oxygen group. Scanning electron microscopy, energy dispersive spectroscopy(SEM & EDS), X-ray diffractometer(XRD) and Zeta potentiometers were used for the characterization of Mn₂O₃@MoS₂. The characterization results show that the high temperature crystallization composite has a complete microstructure and stable crystal structure. By controlling the experimental conditions of variables, the adsorption performance of Mn₂O₃, MoS₂ and Mn₂O₃@MoS₂ on U(Ⅵ) in solution was studied. The results indicate that the adsorption performance of Mn₂O₃@MoS₂ is better than those of Mn₂O₃ and MoS₂, and the adsorption equilibrium time is 90 min at pH=5.5. The adsorption kinetics follows the pseudo-2nd-order kinetic model and the adsorption isotherm curve agrees well with the Langmuir model. The maximum single-layer adsorption capacity of Mn₂O₃@MoS₂ is 117.5 mg/g. Increasing of the temperature from 293.15 K to 318.15 K is beneficial for the adsorption progress.