In this study, a new 3D Co -base MOF ([Co 3 (NTB) 2 (DPP) 2 ] & sdot;2CH 3 OH & sdot;5H 2 O), named CUST-562 , was successfully synthesized from Co(NO 3 ) 2 center dot 6H 2 O, 4,4 ' ,4 ' '-nitrilotribenzoic acid (NTB) and 1,3 -di (4-pyridyl) propane (DPP), and applied to activate peroxymonosulfate (PMS) for degrading dyes in aquatic environments. Because of the continuous cycle of Co 2 + /Co 3 + , CUST-562 exhibited excellent PMS activation performance for the degradation of Rhodamine B (RhB) and Acid Orange 7 (AO7), achieving removal rates of 99.23 % and 93.46 %, respectively. Furthermore, the experimental parameters such as CUST-562 dosage, PMS concentration, dye concentration, reaction temperature, environmental pH, and co-existing anions on dye degradation were explored in detail. Based on the results of radical quenching experiments, it was revealed that 1 O 2 played the predominant role in the CUST-562 /PMS system, and the generation paths of 1 O 2 were explained elaborately. The practical applicability of the CUST-562 activated PMS for dye decontamination was also assessed.