In order to solve the treatment problem of DMF distillation residue in synthetie leather enterprises, high temperature and high pressure reaction kettle was used to treat DMF distillation residue with the supercritical water oxidation technology and subcritical water oxidation technology, and the oxidized effluent was treated by MBBR process. The results show that optimizing temperature, reaction time and peroxide coefficient can significantly improve the degradation rate of residual, and the trend is fast firstly and then slow. The effect of solid-liquid ratio on the degradation rate is relatively small, and they are negatively correlated. The optimal conditions are at 400 ℃ for 10 min with a solid-liquid ratio of 1 ∶ 14 and peroxide coefficient of 175%. The degradation rates of TOC and COD in liquid products are 98.7% and 99.5%. Moving bed biofilm reactor (MBBR) process has obvious removal effects on COD, TN, NH+4-N and TP, with highest removal rates of 71.3%, 92.9%, 99.5% and 55.6%, respectively.