In this paper, the parameters affecting the adsorption of CuII and NiII by PAN‐NHx fiber and PAN‐COONa fiber were discussed firstly, such as initial ion concentration, pH, and temperature. Secondly, influence factors toward the separation of CuII and NiII by PAN‐NHx fiber were systematically evaluated by single‐column experiments. The results showed that the PAN‐NHx fiber had good separation of CuII and NiII; NiII accounts for more than 99.00 % of total metal ion content in the initial 1000 mL effluent, while CuII is less than 1 %. With the changed from CCuII: CNiII=90 %:10 % to 95 %:5 %, the ratio of CCuII: CNiII in the treated effluent changed from 6 %: 94 % to 2 %: 98 % (fed flow rate: 0.42 BV min−1). The adsorption capacity of PAN‐NHx adsorption column was well maintained after six cycles. Finally, based on the above laboratory results, a multi‐column process was designed to separate and recover CuII and NiII from wastewater.
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