The acid activation of bentonite from Middle Anatolia, consisting of mostly montmorillonite, with a hot solution of H2SO4 with different concentrations was carried out. SEM images, nitrogen sorption isotherms and FTIR spectra were used to examine structural changes of the bentonite with acid activation. Acid-base titration method was applied to determine surface acidities. SEM images, nitrogen sorption isotherms indicated that the acid activation caused considerable increases both in the surface area and pore volumes by changing the morphology and aluminum content. FTIR spectra showed the enhancement both in Lewis and Bronsted acidities, significant increases in H-bonding to the structure with acid concentration. Acid treatment gave good structural properties with high surface acidity. Stable structured acid activated bentonite with 2 M was tested in catalytic wet peroxide oxidation (CWPO) of phenol together with raw bentonite. Around 96 % phenol removal was achieved in 135 minutes at reaction temperature of 50 degrees C while the raw bentonite did not show good results. The data were in agreement with the first order dependency with respect to phenol.