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Herein, mesoporous sulfurized CoFe₂O₄ (S-CoFe₂O₄) was developed and applied as a new Fenton catalyst. As a result, the sulfurization for CoFe₂O₄ could significantly improve the Fenton performance, compared with the non-sulfurized CoFe₂O₄. The enhanced removal efficiencies of pollutants in Fenton process catalyzed by S-CoFe₂O₄ was attributed to the elevated specific area and decreased electron transfer resistance of S-CoFe₂O₄. The DFT calculations further confirmed that the increased charge densities of Fesingle bondS bond and Cosingle bondS bond could contribute to the existences of species of Fe and Co in S-CoFe₂O₄ with the low valence, which were more favorable to the H₂O₂ activation. Furthermore, electron paramagnetic resonance (EPR) tests showed that the OH^{radical dot} and O₂^{radical dot−} were the main generated radicals during the H₂O₂ activation process. This work provided a …