In this paper, molybdenum disulfide was grown on the surface of iron-containing tailings by hydrothermal method, and a series of highly efficient activated persulfate (PMS) iron-based catalysts were successfully prepared. The results show that in the CTM 1-200/PMS system, the additional ratio of tailings and the hydrothermal temperature have important effects on the catalyst. The catalyst prepared under the conditions of CT:MoS2 (molar ratio 1:1) and hydrothermal temperature of 200 °C (CTM 1-200) had the best degradation effect on BPA, and the degradation effect was increased by four times. The reason for the improvement of degradation efficiency is that the introduction of MoS2 accelerates the REDOX cycle between Fe(II)/Fe(III), and the reduction of Fe(III) is mainly related to Mo(IV), while the reduction capacity of S is relatively weak. Molybdenum disulfide/iron tailing composite material provides a way for tailings to solve the problem of water pollution.