The electrochemical and chemical complex oxidation process is used to handle wastewater from acrylonitrile production and the quality of effluent of each treatment unit is analyzed.It is found that the degradation rates of amide and carboxyl compounds in acrylonitrile wastewater show a good linear relationship with the pollutant indexes such as TOC and COD.By means of UV-Vis spectra and functional groups titration,the migration and conversion of refractory pollutants along the treatment process can be characterized effectively.