Nanosized iron phosphide (Fe2P) was successfully synthesized under mild solvothermal conditions with environmental-friendly raw materials. The key synthetic parameters including the molar ratios of Fe/P in initial mixture, the solvothermal treatment temperature, and duration were systematically investigated, and the samples were characterized using X-ray diffraction, energy dispersive spectroscopy, and transmission electron microscopy. These measurements indicated that the nanoparticles are pure Fe2P with an average particle size of about 20 nm. Furthermore, the catalytic performance of the as-synthesized Fe2P/ZSM-5 in thiophene hydrodesulfurization was tested. The results showed that the desulfurization efficiency of thiophene can reach up to 88 % after 3 h with a stable catalytic activity during the whole examination process.