Abstract: SbSn intermetallic compound was prepared via mechanical alloying with equal molar ratio of Sb to Sn. The bulk phase structure, micromorphology, melting point and particle size of the SbSn alloy were determined by XRD, SEM, DSC and granulometer respectively. The average diameter of SbSn alloy particle is 10.622μm after 36h ball milling. The SbSn was supported on wire net as working medium, and its desulfurization behavior for four W/O emulsion of crude oil was investigated in an directcurrent field. Under the condition of temparature 30℃, surfactant addition 0.19%, desulfurization efficiency reached 36.8% for W（40）/O（60） when voltage was assigned at 9.62V and processing time was 22h. The desulfurizaition mechanism could be explained by that there are electrochemical reactions between P-polar formed by Sb which is enriched on SbSn surface and the negative polar sulfide on condition of electric current being induced. The electrochemical determination showed that the reaction of sulfur on SbSn surface is reversible.