Adsorptive separation of Pb(II) and Cu(II) using modified waste Lyocell fiber adsorbent was investigated in this research. The waste Lyocell fiber was functionalized through carboxymethylation of the hydroxyl moieties using sodium chloroacetate as modifying agent and was crosslinked with epichlorohydrin to provide water stability. The maximum equilibrium batch uptake in single metal system was 353.45 mg/g for Pb(II) and 98.33 mg/g for Cu(II), according to the Langmuir isotherm model. The adsorption rates were very fast and reached equilibrium within 3 and 5-10 min for Cu(II) and Pb(II), respectively. In competitive binary metal system, the uptake of Cu(II) largely decreased to 38.40 mg/g, and Pb(II) selectivity was observed. Elemental and functional characterization suggested that the adsorption proceeded by ion exchange between the adsorbent and metal ions. In a flow-through column system, adsorption followed by desorption aided in effectively eluting *260 mg of Pb(II) (out of *300 mg total adsorbed) from the Pb(II)-Cu(II) binary solution. Finally, the adsorbent was very effective in four successive adsorption-desorption cycles with over 99 % uptake and 94 % desorption efficiencies. The present study may provide an alternative option for waste fiber recycling and could be useful in recovering heavy metal ions from aqueous sources to complement their depleting reserves.