Acetic acid (HAc), a hydroxyl radical probe in ozonation, was chosen as a target contaminant to be degraded in strong acidic solution by different ozone-based processes. The highest removal rate of HAc was obtained by S-ZF/H2O2/O-3. The indirect method of dimethyl sulfoxide (DMSO) capture showed that hydroxyl radical was effectively produced in this process. A mechanism study indicated that the S-Fe(III) peroxo complex intermediate played an important role in the process. The effects of different parameters such as pH value, amount of catalyst, concentration of H2O2, and rate of ozone input were investigated. The experimental results showed that the presence of SO2-4/ZrO2-Fe2O3, abbreviated as SZF, could greatly improve the oxidative efficiency of H2O2/O-3 in the pH range from 0 to 5.0. The result is very significant to the application of H2O2/O-3 in strong acid wastewater pretreatment.