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A novel approach was successfully developed for the catalyst Bi-deposited Fe3O4 magnetic nanoparticles, which was used in the degradation of 4-nitrophenol (4-NP). The Bi/Fe3O4 composite was prepared via a one-pot process from ferrous sulfate and bismuth chloride using hydrazine hydrate as a reducing agent. The catalyst was characterized by X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy. In the composite pure Fe3O4 particles were synthesized and bismuth particles were well dispersed. The catalytic performances were investigated for the reduction of 4-NP with sodium borohydride. The catalyst has higher activity when Bi/Fe molar ratio is 1:4 in the composite and the rate constant k is about 0.611 min-1. The catalyst has good reusability which can be used 10 cycles without obvious deactivation. Furthermore, the catalyst can be easily separated by an external magnetic field.