It had been done a research about adsorption of Cu2+ using polysulfone-FeOOH nanofiber prepared by elektrospinning method. Polysulfone-FeOOH nanofiber was synthesized by dissolving polysulfone pellets in 30 mL dimethylacetamide (DMAc). The effects of process conditions such as concentration, distance between the nozzle and collector, voltage and flow rate on the morphology and diameter of nanofibers were investigated. The optimum conditions of polysulfone nanofiber synthesizing was obtained with concentration 25%, distance 12 cm, voltage 25 kV, and flow rate 0.05 mL/min with average diameters of fibers was 762.927 nm. Polysulfone nanofiber was coated with FeOOH to increase the adsorbtion capacity of Cu2+. The results showed that optimum condition for removal of Cu2+ used polysulfone-FeOOH nanofiber was obtained in 2 hours contact time, pH 6, adsorbent dosage 25 mg, and concentration of Cu2+ 10 mg/L with adsorbstion capacity was 9.79 mg/g, while for polysulfone nanofiber the adsorption capacity was 8.34 mg/g. The adsorbtion pattern of Cu2+ by the both of adsorbent followed the Freundlich isotherm pattern.