A novel adsorbent was prepared with maleic anhydride and acrylamide as functional monomer, N,N-methylenebisacrylamide as cross-linking agent, and ammonium persulfate as initiator through aqueous polymerization reaction. The adsorbent was characterized by Fourier transmission infrared spectra (FTIR) and Thermogravimetry (TG). The adsorption properties and selectivity properties were investigated by inductively coupled plasma atomic emission spectrum (ICP-AES). The result indicated that the optimum acidity was pH 3.5 and the reaction attained equilibrium at 1 h under stirring. The polymer adsorbent exhibited high selectivity for Fe3+ and its saturated adsorption capacity was 78.81 mg·g-1. The adsorption kinetics was well described by pseudo-second kinetic equation, and the adsorption of the copolymer for Fe3+ accorded with Freundlich isothermal model. The adsorption process was found to be endothermic.