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The aim of this study was to evaluate the efficiency of the coagulation/ flocculation and flotation process for aniline removal from aqueous solutions, which the dissolved air flotation (DAF) was applied in laboratory scale. After determination of the optimal condition of pH and the dosage of Polyaluminum chloride by coagulation/ flocculation process, the effect of the effective parameters including the concentration of the coagulant, coagulation time, flotation time and saturation pressure on the removal efficiency of the aniline and COD By dissolved air flotation was studied. The DAF process can reduce COD and aniline up to 89.6% and 95%, respectively. The optimum condition was as follows: pH=6, initial concentration of aniline= 200 mg/L, flocculation time = 10 min, flotation time= 20 sec, the pressure= 4 atm and PAC concentration of 20 mg/L. The coagulation/ flocculation -flotation (DAF) processes can an effective method to remove the aniline from aqueous solution.