In this paper, an efficient procedure to prepare N,O-carboxyethyl-chitosan (N,O-CE-CTS) was established by the reaction of 3-chloropropionic acid and chitosan. The optimum conditions of the preparation of N,O-CE-CTS were found as follows: 90% DD of chitosan, the mass fraction of sodium hydroxide of 15%, the reaction temperature of 60°C-70°C, the reaction time of 3 h, and the ratio of the raw material (CTS/ClCH2CH2COOH) of 1:1.5. Under these conditions, the degree of substitution (DS) of N,O-CE-CTS reached 0.83. The chemical structure of N,O-CE-CTS was characterized by FT-IR and XRD, and the thermal properties were analyzed by DSC and TGA. The adsorption properties of N,O-CE-CTS were also investigated. The results reveal that the modified chitosan has good adsorption capacities for metal ions than the chitosan.