<p>Cu(I) doped Fe₃O₄ nanoparticles was loaded onto graphene oxide, Cu-Fe₃O₄/GO with binary active sites and accelerated Fe(III)/Fe(II) cycle showed higher tetracycline hydrochloride oxidation efficiency than Fe₃O₄ and Cu-Fe₃O₄, the influences of initial H₂O₂ concentration, reaction pH, catalyst dosage, reaction temperature and radical scavengers on catalytic performance of Cu-Fe₃O₄/GO were investigated. The heterogeneous Fenton reaction over Cu-Fe₃O₄/GO surface contained Fe(III)/Fe(II) and Cu(II)/Cu(I) active sites, Fe species were the dominant active centers. Cu-Fe₃O₄ nanoparticles and GO combined via C–O–Fe bond and formed a stable Cu-Fe₃O₄/GO conductive structure, which promoted electrons transfer between Cu-Fe₃O₄ and H₂O₂, thus accelerating Fe(III)/Fe(II) and Cu(II)/Cu(I) cycles. GO significantly improved specific surface area, Cu-Fe₃O₄ nanoparticles dispersibility, and adsorption performance of catalyst. Furthermore, the strong interaction between GO and Cu-Fe₃O₄ prevented ions from leach, GO captured the soluble Fe(III) which was efficiently reduced to Fe(II)_surf by surrounding H₂O₂ and Cu(I)_surf. The degradation efficiency maintained 80.7% after six cycles, the excellent stability can be ascribed to the strong interaction between Cu-Fe₃O₄ and GO. Reactive oxygen species scavenging results indicated that surface-bound ^•OH_surf played a dominating role, followed by aqueous ^•OH_aq and superoxide radicals (O₂^•−).</p>