Coal fly ash, collected from ICI soda ash plant, was modified by two different surfactants namely hexadecyltrimethyl ammonium bromide (HDTMA) and sodium dodecyl sulfate (SDS). Surfactant treated ash was characterized by SEM, TGA, FTIR and BET, to explore the surface morphology, thermal stability, presence of functional groups, and porosity respectively. The two modified forms were also experimented to test their efficiency for the removal of chloro- and nitrobenzenes from aqueous phase. Different parameters like effect of adsorbent dose, solution pH, temperature, contact time and initial solution concentration. The analysis results showed HDTMA modified fly ash is superior than SDS modified fly ash. The uptake capacity of fly ash treated with HDTMA is 224 mg/g for chlorobenzene and 84 mg/g for nitrobenzene. The adsorption of chlorobenzene is exothermic over both adsorbents while nitrobenzene showed the endothermic behavior. The isotherm analysis depicted the multilayer adsorption of both pollutants onto the surface of surfactant modified ash.