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The acid washing solution of copper smelting flue gas was adsorbed by D296 anion exchange resin, and then Sb was desorbed by ammonia, Bi was desorbed by NaOH and tartaric acid mixed solution, and Re was desorbed by NH₄SCN solution. The step-by-step desorption of Re/Sb/Bi was realized and rhenium enrichment solution was obtained. The results show that the potential of acid washing solution has no significant effect on the adsorption rates of Re, Sb and Bi. The appropriate concentration of H₂SO₄ in acid washing solution is about 43 g.L^_-1, and the adsorption rates of Re, Sb and Bi are 100%, 6.55% and 89.05%, respectively. The breakthrough capacity and saturation capacity of D296 resin for adsorption of Re are 1.308 g.L^_-1 and 1.773 g.L^_-1, respectively, and the utilization rate of resin is 73.77%. Firstly, 12.5% ammonia is used to desorb sb, and 16% NaOH + 140 g.L^_-1 tartaric acid mixed solution is used to desorb Bi. The hydrolysis of Bi can be effectively inhibited by adding tartaric acid, and then 10% NH₄SCN solution is used to desorb Re to obtain rhenium enrichment solution. The concentration of Cu, As, Sb and Bi in rhenium enrichment solution decrease to less than 1 mg.L^_-1. Re concentration in acid washing solution is enriched four times.