In order to evaluate the sorption of copper(II), cobalt(II) and zinc(II) ions from water systems in the batch systems, a novel elecrtospun zirconia modified with thiol and amine groups/Poly vinyl pyrrolidone (APTES/TMPTMS/Zirconia/PVP/P123) was synthesized. The morphology of nanofibers was characterized by FTIR, SEM, BET and BJH analyses. Based on results, the average fiber diameter of APTES/TMPTMS/Zirconia/PVP/P123 adsorbent was found to be 98.9 nm. The adsorption experiments were carried out to investigate the effect of different adsorption parameters such as solution pH, contact time, initial concentration and temperature. The kinetic data of metal ions were well described by the double-exponential model. The maximum sorption capacities of Cu(II), Co(II) and Zn(II) ions were estimated to be 4.146, 3.050 and 2.352 mmol/g, respectively in the single system. In all binary systems, the sorption capacity decreased with increasing the other metal ion concentrations. The combined effect of metal ions onto the nanofiber was found to be antagonistic. The selectivity order of metal ions sorption onto the adsorbent was Cu(II)>Co(II)>Zn(II).