A novel polystyrene modified ethoxycarbonyl thiourea resin(PSETU) was synthesized by polymer grafting of aminated polystyrene and ethoxycarbonyl isothiocyanate. The adsorption capacities of PSETU follow the order: Au(III) > Cu(II) > Zn(II) > Ni(II) > Fe(III) > Ca(II) ≈ Mg(II). The adsorption capacity for Au(III) increases with the increase of contact time, temperature and initial concentration of Au(III). The adsorption data fit Boyd’s diffusion equation of liquid film, Langmuir adsorption isotherm and Freundlich adsorption isotherm. The maximum adsorption capacity of PSETU calculated by Langmuir isotherm equation is 3.485 mmol/g, and the separation factors of PSETU for Au(III)-base metal ions are above 380. According to XPS results, the functional atoms of PSETU coordinate with Au(III) during the adsorption process.