The walnut shell grafted polyacrylamide or poly(methyl methacrylate) were prepared using AGET ATRP by walnut shell macroinitiator and monomer (acrylamide or methyl methacrylate) in the catalytic system of FeCl3•6H2O/PPh3 and Vc. The structure and appearance of composite material was characterized by FTIR, TG and SEM. The adsorptive properties of walnut shell-g-polyacrylamide or poly(methyl methacrylate)for metal ions were evaluated. The adsorptive capacity of composite materials was higher than walnut shell for Pb(II) and Cu(II). The results indicated that the maximum adsorption capacity was 40.5, 48.5 mg/g at 293 K and pH 5. 0 when an initial concentration of Pb(II) was 50 mg/L. Kinetic and isotherm studies of Pb(II) revealed that adsorption data followed the pseudo-second-order kinetic model and the Langmuir isotherm. The minimum desorption rate of Pb (II) was 93.4% and 93.1% for 4 times of regeneration. It showed that the materials had better regeneration capacity.