Abstract: Based on the current situation of comprehensive utilization of coal slime in China and the urgent need for water pollution control in coal mining areas, this paper uses coal slime(CS)as raw material and CaCl₂ as the activator, different proportions of coal slime-based catalytic materials were prepared under anaerobic calcination, which were characterized by XRD, SEM, BET, FT-IR, XPS, Raman spectroscopy, etc. This study investigated its ability to activate peroxymonosulfate(PMS)for the catalytic degradation of phenol in wastewater. Results show that the catalytic material prepared by CaCl₂-heat treated coal slime can effectively activate PMS to achieve the highly efficient degradation of phenol. In addition, when the mass ratio of coal slime and CaCl₂ reach 4∶3, it shows the optimal degradation performance, whose degradation rate of phenol can reach 100 %. The active species ¹O₂ played a major role in the degradation system. Moreover, the catalytic materials could be applied in a wide pH range(3.0~11.0), and the influence of various anions in water on the degradation of phenol is relatively limited, indicating their good application prospect in wastewater treatment.