In this work, the feasibility of foam fractionation for the enrichment and isolation of phenol from its aqueous solution was studied by using cetyltrimethyl ammonium bromide (CTAB) as the collector. A two-stage foam fractionation technology was developed for simultaneously obtaining a high enrichment ratio and a high recovery percentage. Under the suitable operating conditions, the enrichment ratio and recovery percentage of phenol reached as high as 84.46 and 93.43%, respectively. Subsequently, foam fractionation was also used to isolate phenol from CTAB in the first stage foamate, in which the interaction between phenol and CTAB could be weakened by adjusting pH. The concentration of CTAB significantly decreased from 11.230 g/L in the feeding solution to 0.620 g/L in the residual solution by using the foam fractionation, while the concentration of phenol slightly decreased from 2.533 g/L to 2.450 g/L. The results indicated that it was practicable to successively enrich and isolate phenol from its aqueous solution by using foam fractionation.