To improve the activation efficiency of PMS to efficiently degrade antibiotic sulfadiazine (SD), herein, a Co@MoS2 catalyst was prepared by a one-step hydrothermal process. The unique petal-like structure of MoS2 enables the transition metal Co to achieve high dispersion and avoid agglomeration. Mo(IV) and unsaturated S accelerate the electron transfer between Co2+ and Co3+ to improve the cycling efficiency and thus realize the efficient activation of PMS. The results of active substance quenching experiment and ESR analysis show that the main active substance for the efficient degradation of SD by Co@MoS2 is the non-radical 1O2, while the other three radicals ⋅O−2, ⋅OH and SO∙−4 contribute significantly to the efficient degradation of SD. And after 5 cycles, the degradation could still be as high as 90%. The strong consolidation of Co on the petal-shaped sheet of MoS2 ensures the stability of Co@MoS2 catalyst.