<p>A novel approach was successfully developed for the catalyst Bi-deposited Fe<sub>3</sub>O<sub>4</sub> magnetic nanoparticles, which was used in the degradation of 4-nitrophenol (4-NP). The Bi/Fe<sub>3</sub>O<sub>4</sub> 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 Fe<sub>3</sub>O<sub>4</sub> 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<sup>-1</sup>. 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. Copyright © 2017 BCREC GROUP. All rights reserved</p><p><em>Received: 11<sup>st</sup> August 2016; Revised: 20<sup>th</sup> December 2016; Accepted: 21<sup>st</sup> December 2016</em></p><p><strong>How to Cite:</strong> Cai, K.Y., Liu, Y.S., Xu, Y., Zhou, H., Zhang, L., Cui., Y. (2017). One-Pot Synthesis of Bi/Fe<sub>3</sub>O<sub>4</sub> and Its Catalytic Performances for 4-Nitrophenol Reduction.<em> Bulletin of Chemical Reaction Engineering & Catalysis</em>, 12 (1): 89-95 (doi:10.9767/bcrec.12.1.621.89-95)</p><p><strong>Permalink/DOI:</strong> http://dx.doi.org/10.9767/bcrec.12.1.621.89-95</p><p> </p>