In the present work, two novel aminophosphinic acid ligands grafted on poly(styrene-1%divinylbenzene) (St-1%DVB) have been synthesized by reacting polymer precursors bearing primary amino groups with benzaldehyde (or propionaldehyde) and phenylphosphinic acid by the one-pot Kabatachnik-Fields reaction. The resins functionalized with aminophosphinic pendant groups were characterized by means of Fourier transform infrared spectroscopy (FTIR), thermal analysis, energy dispersive X-ray microanalysis (EDX), and Scanning electron microscopy (SEM) imaging. Its adsorption capacity for divalent metal ions such as Cu(II) and Ni(II) were investigated. The adsorption procedure of Cu(II) and Ni(II) ions on polymer-grafted aminophosphinic acid ligands was carried out by batch experiments. The result also shows that the adsorption process was best described by a pseudo-second-order kinetic equation and by the Langmuir adsorption isotherm. The best maximum adsorption capacity was obtained for resin with aminobenzylphosphinic acid groups [1.46 mg Cu(II)/g and 1.36 mg Ni(II)/g]. POLYM. ENG. SCI., 2013. (c) 2012 Society of Plastics Engineers