A new L-phenylalanine resin (PSAcylPhe) was prepared by chloroacetylated polystyrene (PSAcylCl) instead of merrifield resin (PSCH2Cl) and applied for chelating Ni2+. The effects of pH, chelating time and concentration of Ni2+ on the chelating reaction were investigated for the optimal chelating condition. The results show that under the optimal conditions of Ni2+ concentration 0.1 mol/L, pH 3.5~9.0, and chelating time 1 h, the chelating rate could be up to 40.8%.