Abstract: ⁶³Ni is produced by the neutron irradiation of ⁶²Ni in a reactor. After separation and purification, the highly purified ⁶³NiCl₂ solution was obtained. In this paper, using the nickel target which was irradiated in High Flux Engineering Test Reactor (HFETR) for more than 30 years as the research subject, the ZGANR170 nuclear anion resin was used to purify ⁶³Ni from the solution of irradiated nickel target. In the end, the high purity ⁶³NiCl₂ solution products were obtained. In addition, the separation principle, procedures and the optimal separation condition were both introduced in detail. Moreover, the effect of acidity on separation was studied experimentally. The result demonstrated that only when the concentration of HCl is greater than or equal to 9 mol/L, a good separation effect could be obtained. Besides, the decontamination factor of γ radionuclides in the whole process of nickel purification is 2.33×10³. And the nuclear purity of the 63NiCl2 solution is more than 99.9%. After dissolution, system conversion and separation, the recovery rate in the whole process is 86.5%.