A new method for preparing a novel macro-porous chelating resin that has good adsorption capability for Cu(II) and high selectivity for it with the coexistence of Ni(II) was introduced in this article. First, the animated resin (PS-TETA) was synthesized by the reaction of crosslinked macroporous chloromethylated polystyrene with triethylenetetramine. Subsequently, PS-TETA was coordinated with Cu(II) and then PS-TETA-Cu was obtained. After the crosslinking reaction of PS-TETA-Cu with epoxy chloropropane, the adsorbed Cu(II) was removed by chlorhydric acid, and then the target resin-Cu(II) template triethylenetetramine crosslinked polystyrene resin was obtained. The selectively sorption tests for Cu(II) showed that the sorption capacity was as high as 1.6 mmol/g and the selectivity coefficient alpha(Cu(II)/Ni(II)) could reach to 9.06 with the coexistence of Ni(II). SEM and nitrogen adsorption at 77 K methods were used to characterize the porous structure of the resin. (c) 2006 Wiley Periodicals, Inc.