Porous magnetic cobalt ferrite nanocrystals (CoFe 2 O 4 NC) are synthesized via a one-step process by using bimetal-organic frameworks (Co/Fe bi-MOFs) as a template for the catalytic degradation of bisphenol A (BPA). The properties of the prepared catalyst are evidenced by a series of characterization techniques. Overall, the unique ferromagnetic nature (34.73 emu/g) make its efficient separation from the liquid phase possible. CoFe 2 O 4 NC activates peroxymonosulfate (PMS) to degrade BPA more efficiently than hydrothermally fabricated CoFe 2 O 4 nanoparticles. The difference in catalytic capacity is attributable to the larger specific surface area (60.4 m 2 g −1 ) and well developed mesoporous structure (0.64 cm 3 g −1 ) of the CoFe 2 O 4 NC. EPR analysis demonstrate the production of HO and SO 4 − radicals in the CoFe 2 O 4 NC/PMS system. The degradation process positively correlates with the increase of initial solution pH, catalysts dosage, and PMS dosage. The degradation rate of 0.112 min −1 is achieved at [PMS]/[BPA] of 10, catalyst dosage of 0.1 g L −1 , temperature of 25 °C, and initial pH of 10.2 in deionized water. The existence of Cl - and HCO 3 − /CO 3 2− show significant positive synergistic effects on the catalytic process. Moreover, simple thermal treatment at 400 °C for 15 min in open air fully regenerates the catalytic capacity of CoFe 2 O 4 NC for reuse. Findings from this work shed light on the rational design of bimetallic oxide catalysts and provide new insight into the development of high-performance magnetic separable catalysts.