The present work elucidates an environmental friend by process for heavy metals removal from aqueous solutions using mesoporous silicate, containing zirconium and iron. The process comprises the three following steps: (1) synthesis and characterization of mesoporous silicate bed (the prepared adsorbent materials were characterized by powder X-ray diffraction, nitrogen isotherms, FTIR, TGA, and SEM). (2) Evaluation of the efficiency of this new adsorption bed for Cu and Cd removal from aqueous solutions. (3) Study of metal concentration (50-1000 ppm), stirring time (0.5-5 h) and pH (1.5-12) effects on the adsorption power using batch techniques. Results obtained indicate that under optimum conditions, pH in the vicinity of 5-6, Zr-M has the maximum adsorption capacity for both cations Cu and Cd. On the other hand, ZrFe-M1 containing a higher molar ratio of iron showed lower adsorption capacity for the cations Cu and Cd. (C) 2011 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.