A novel dihydroxyl azacrown ether chitosan was synthesized by reacting dihydroxyl azacrown ether with epoxy activated chitosan. The adsorption property of the azacrown ether chitosan for Pb2+, Cr3+, and Ag+, were determined. The experimental results showed that the dihydroxyl azacrown ether grafted chitosan has high adsorption capacity and high selectivity for some metal ions.