A novel nanometer-sized chelating resin (NSCR) was prepared via two steps, First step: copolymerization reac- tion of N-methacryloxyphtalimide (NMP) with methylenebisacrylamide (MBA) by suspension polymerization method to give ultrafine poly (NMP-co-MBA). Second step: reaction of triethylenetetra mine (TETA) with poly (NMP-co- MBA) to give NSCR. The prepared NSCR was characterized by Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), Tran smission electron microscopy (TEM), Brunauer-Emmett-Taller (BET) and thermogravimetric analysis (TGA). This study illustrated the capability of NSCR for extraction of Cu(II), Co(II) and Ni(II) from aquatic solu- tions. The pH effect, metal ions concentration, temperature and contact time were elaborated in batch experiments. The results showed that high capacities were 1.3, 1.0 and 0.95 mmol/g resin for Cu(II), Ni(II) and Co(II) ions, respectively. The exper- imental data of adsorption isotherms were convenient for Langmuir isotherm, and the kinetic data illustrated that the removal process was described by pseudo-second order kinetic model. The parameters of Thermo dynamic illustrated that the process of adsorption was endothermic and spontaneous reac- tion. The prepared NSCR was regenerated and used repetitive- ly for five times with small decrease in adsorption capacity