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Advanced oxidation (AOPs) utilizing peroxymonosulfate (PMS) are efficient processes for the degradation of organic pollutants. This study aimed to synthesize and characterize cobalt ferrite (CoFe2O4), graphene oxide (GO), MIL-101(Fe), and their composite structures. The nanomaterials were applied as catalysts by PMS for triclosan (TCS) decomposition. The maximum removal rates of TCS were 49.29, 66.13, 84.04, 89.73, and 100% for PMS alone, CoFe2O4, GO, MIL-101(Fe), and CoFe2O4/MIL-101(Fe)/GO with PMS, respectively. Metal ions leaching declined in CoFe2O4/MIL-101(Fe)/GO/PMS compared with others. Hence, the composite nanomaterials appear to be effective catalysts for the degradation of organic pollutants by PMS activation.