The construction procedure and structure of Ni2+ macromolecular complexes with series of poly styrene and maleic anhydride (PSt/MA) were studied.Both the copolymers and the complexes (Ni-PSt/MA) were characterized by means of FTIR,elemental analysis, GPC and AAS.A further study using PSt/MA as chelating resins recovering Ni2+ has been performed as well, its adsorption behavior toward Ni2+ and various relating parameters in the separation process were determined.The results indicate that the adsorption capability varies with pH valuables.Adsorption experiments show that the PSt/MA can recovery Ni2+ in higher adsorption rate and higher selectively coefficient from a mixture solution containing light metals such as Ca2+ and Mg2+ as impurities.