Semi-solid Fenton process (SSFP) was firstly conducted on hazardous solid waste detoxication. Batch tests, Box-Behnken designs, and response surface methodology were applied to optimize the key factors including the pH, the initial Fe(II) content, and the liquid-to-solid ratio (L/S). It shows that the optimal pH, the initial Fe(II) content, and the L/S in SSFP are 3.5, 0.062 mol kg −1 dry weight and 1.77, respectively. Correspondingly, the removal efficiencies of ONA and ArNH 2 are 98.5±0.5% and 100% which agree well with the results of an established polynomial model. It suggests that SSFP is an efficient and environmentfriendly method for hazardous solid waste detoxication without wastewater generation.