A novel poly(methacrylic acid) material (IIP/CTAB) was prepared by a hierarchical double-imprinting process with Ni2+ ion and cationic surfactant-cetyltrimethylammonium bromide (CTAB) as templates, and it was employed to adsorb Ni2+ ions from aqueous medium. Other poly(methacrylic acid) materials- single imprinted (IIP/no CTAB) and nonimprinted (NIP/no CTAB) were investigated in adsorption studies. All the synthesized polymers were characterized by FTIR, SEM, and nitrogen adsorption-desorption isotherm The maximum Ni2+ adsorption capacities of IIP/CTAB and NIP/no CTAB were found to be 33.31 and 18.64 mg respectively, at pH 7.25. The relative selectivity coefficient (k') values for Ni2+/Cu2+, Ni2+/Mn+, Ni2+/Co2+ and Ni2+/Pb2+ systems were higher than 1, thus confirming the significant improvement in the selectivity of the polymer. The kinetic data were described very well by the pseudo-secona-order model, thereby confirming the chemical nature of the Ni2+ adsorption (chemisorption), whereas the dual-site Langmuir-Freundlich equation provided the best fit to the isotherm data, suggesting the existence of two kinds of adsorption sites (with low and high binding energies) on the polymer surface. The high chemical stability of IIP/CTAB was verified with 300 Ni2+ adsorption-desorption cycles using 1.0 mol L-1 HNO3 as stripping agent