Fly ash resulted from coal burning is a waste that can be used in wastewater treatment for removal of dyes and heavy metals by adsorption. Class "F" fly ash (FA), collected from the Central Heat and Power (CHP) Plant Brasov (Romania), with oxides composition SiO2/Al2O3 over 2.4 was used for obtaining a new substrate with good adsorption capacity for dyes and heavy metals from wastewater. A new material was obtained from modified fly ash with NaOH and hexadecyltrimethylammonium bromide (HTAB) a cationic surfactant. Contact time, optimum amount of substrate and the pH corresponding to 50 mL solution of pollutants were the parameters optimized for obtaining the maximum efficiency in the adsorption process. The optimized adsorption parameters were further used in thermodynamic and kinetic studies of the adsorption processes. The adsorption kinetic mechanisms, and the substrate capacities are further discussed correlated with the surface structure (XRD), composition (EDS, FTIR), and morphology (SEM, AFM). The results indicate that the novel nano-substrate composite with fly ash modified can be used as an efficient and low cost adsorbent for simultaneous removal of dyes and heavy metals, the resulted water respects the discharge regulations. (C) 2014 Elsevier B.V. All rights reserved.