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In this paper, N-methylene phosphonic acid chitosan (NPCS-PEI) was synthesized from chitosan, phosphorous acid, formaldehyde and hyperbranched polyethyleneimine (PEI), and Cu2+ and Pb2+ removal performance was examined in aqueous solution. NPCS-PEI exhibited three-dimensional porous architectures, with a specific surface area of 490.61 m2/g. The effects of pH, initial concentration, adsorption time, temperature and ionic strength on the adsorption capacity were investigated. The adsorption kinetics indicated that Cu2+ and Pb2+ adsorption onto NPCS-