A new composite material based on alginate and magadiite/Di-(2-ethylhexyl) phosphoric acid (CAM-D2EHPA) was successfully prepared by previous impregnation of layered magadiite with D2EHPA extractant, and then immobilized into the alginate matrix. Air dried beads of CAM-D2EHPA were characterized by FTIR and SEM–EDX techniques. The sorbent was used for the separation of lead and nickel from nitrate solutions; the main parameters of sorption such as contact time, pH of the solution, and initial metal concentration were studied. The beads recovered 94% of Pb(II) and 65% of Ni(II) at pH 4 from dilute solutions containing 10 mg L⁻¹ of metal (sorbent dosage, S.D. 1 g L⁻¹). The equilibrium data gave a better fit using the Langmuir model, and kinetic profiles were fitted using a pseudo-second order rate equation. The maximum sorption capacities obtained (at pH 4) were 197 mg g⁻¹ and 44 mg g⁻¹ for lead and nickel, respectively. The regeneration of the sorbent was efficiently carried out with a dilute solution of HNO₃ (0.5 M). The composite material was reused in 10 sorption–elution cycles with no significant differences on sorption uptake. A study with synthetic effluents containing an equimolar concentration of both metals indicated a better selectivity towards lead ions.