Fenton oxidation technology was applied to treat hexogeon industrial wastewater and response surface methodology was used to optimize the effects of the FeSO4 concentration, H2O2 concentration, pH value, and temperature. A quadratic model was obtained as the result of this design. In the optimization, the coefficient of variation is only 3.17%, indicating a good precision and reliability of the experimental. The coefficient of association (R2) and adj-R2 for quadratic model were evaluated quite satisfactorily as 0.98 and 0.96, respectively. The predicted optimum conditions were determined as 763 mg L−1 of FeSO4 concentration, 107 mg L−1 of H2O2 concentration, 2.64 of pH, and 19°C with 83.5% of chemical oxygen demand removal. The experimental result was 82.92% under optimizing reaction factors.