In the present research article we explore the synthesis method and adsorption capability of ZnFe oxides nanocomposites by using Pb as dopant. A conventional and simple batch adsorption method is selected and optimized. Pb@ZnFe2O4 NCs were fabricated by facile method i.e. co-precipitation method and characterized by FESEM, XRD, IR, EDX. The removal of dye has monitored by UV method.An outstanding result is obtained as adsorption efficiency of 1042 mg g−1 shows more significant performance than currently available bench-mark adsorbents. The optimized parameters pH 7.1, Adsorbent Mass: 50 mg, Initial Dye Concentration: 150 mg/l and Agitation Time: 90 min results in 96.49 % removal of CR (Congo red) dye. A CCD (central composite design) is applied to evaluate the role of adsorption variables. Based on its excellent performance, cost effectiveness, facile fabrication and large surface area, the Pb@ZnFe2O4 has considerable potential for the manufacture of cost effective and efficient adsorbents for environmental applications.