A simple process,vacuum distillation,was utilized for purification of methyl orange(MO) as dye effluent.The dye effluent characteristic of high chemical oxygen demand (COD) value and high chromaticity is a headache for the industrial wastewater treatment,so the validity of this new method for advanced purification was studied,especially for high concentration.In our work,the effect of some factors on the distillation efficiency,including pressure,concentration and the surfactant based on the optimal conditions was evaluated.The results showed that the COD removal for 98.56％,recovery efficiency for 67％ and the distillation efficiency for 2.43ml/min were obtained when the concentration of MO is 2000 mg/L under the pressure of 0.085 MPa.Moreover,the polyacrylamide (cationic) used in initial concentration of 500 mg/L show satisfactory removal efficiency in the further test.