In this study, biomass carbon supported with iron and cobalt bimetal (FeCo/BC) was synthesized by a one-pot calcination method to activate peroxymonosulfate (PMS) and peroxydisulfate (PDS) for bisphenol A (BPA) degradation. Characterization with X-ray diffraction, X-ray photoelectron spectroscopy and high resolution transmission electron microscopy showed that Fe 0 , Fe 3 O 4 , Co 0 and CoO nanocrystals were included in FeCo/BC materials. The degradation results showed Fe 0.6 Co 0.4 /BC had excellent catalytic activation performance for PMS or PDS. The Fe 0.6 Co 0.4 /BC (0.0050 g) combined with 0.25 g·L −1 of PMS could completely degrade 20 mg·L −1 BPA within 8 min, and the same amount of BPA could be removed with 0.020 g Fe 0.6 Co 0.4 /BC in the presence of 0.25 g·L −1 PDS within 20 min. The corresponding total organic carbon removal rates reached 83.49% and 77.5% respectively after 2 h. The Fe 0.6 Co 0.4 /BC also had good adaptability to solution pH and practical water body. After five cycles, the degradation rates of BPA in the two systems were all over 90%, and excellent magnetism was beneficial to the reuse of catalysts. Electron paramagnetic resonance and free radical quenching tests indicated that SO 4 •- , •OH, and 1 O 2 were the main active species involved in the BPA degradation. This work not only provided a promising catalyst for the degradation of organic pollutants, but also elucidated the synergistic effect between Fe-Co bimetal alloys during PMS and PDS activation, which would facilitate the design, synthesis, and application of catalytic materials with high efficiency. • The FeCo/C material was prepared through one-pot calcination method. • The FeCo/C exhibited high efficiency and feasibility for bisphenol A degradation by activating persulfate. • The synergistic effect between Fe and Co redox cycles played an important role for persulfate activation. • Electron paramagnetic resonance determination indicated that SO 4 •- , · OH, and 1 O 2 were the main active species.