Nanocomposite hydrogels based on poly(methacrylamide-co-acrylic acid) and nano-sized montmorillonite were prepared by aqueous dispersion and in situ radical polymerization. Optimum sorption conditions were determined as a function of montmorillonite content, contact time, pH, and temperature. The equilibrium data of Cu2+ and Ni2+ conformed to the Freundlich and Langmuir isotherms in terms of relatively high regression values. The maximum monolayer adsorption capacity of the nanocomposite hydrogel (with 3 wt% montmorillonite content), as obtained from the Langmuir adsorption isotherm, was found to be 49.26 and 46.94 mg g−1 for Cu2+ and Ni2+, respectively, at contact time = 60 min, pH = 6.8, adsorbent dose = 100 mg/ml, and temperature = 318 K. Kinetic studies of single system indicated that the pseudo-second order is the best fit with a high correlation coefficient (R 2 = 0.97–0.99). The result of five times sequential adsorption–desorption cycle shows a good degree of desorption and a high adsorption efficiency.
