An efficient biosorbent containing magnetic nanoparticles, walnut shell powder, foam, and alginate (AMWSF) was prepared and used in Pb(II) removal. The adsorption process was performed in an airlift magnetic separation loop system. Optimum adsorption conditions were tested at pH 3–7, biomass dose of 0.03–0.4 g, temperature of 15–35 °C, initial Pb(II) ion concentration of 50–400 mg·L−1, and contact time of 10–480 min. The equilibrium adsorption capacity reached up to 69.45 mg·g−1. The physicochemical properties of AMWSF were analyzed by scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy and Fourier transform infrared spectroscopy. The experimental data were in agreement with the pseudo-second-order kinetic and Langmuir isotherm models. The influences of Cu(II), Cd(II), and Zn(II) on Pb(II) adsorption showed antagonistic effect strength in the order of Cu(II) > Cd(II) > Zn(II). AMWSF was reused seven times and separated rapidly by magnetic field. The results demonstrated the potential of AMWSF in practical applications involving Pb(II).

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