Abstract: In order to damage the molecular structure of C≡N and reduce the toxicity of acrylonitrile wastewater, iron-carbon micro-electrolysis was used to treat the simulation wastewater with the concentration of 100 mg/L. Iron-carbon micro-electrolysis system and activated carbon control experiment were established to avoid the effect of activated carbon adsorption. The results showed that iron-carbon micro-electrolysis system could effectively decompose acrylonitrile, damage the molecular structure of C≡N and decrease toxicity. When acrylonitrile wastewater was treated by micro-electrolysis, it mainly depended on chemical oxidation reduction effect of the free base H and Fe²⁺ that formed between iron and carbon, while the activated carbon only had a certain adsorption capacity. The iron-carbon micro-electrolysis system could change nitrogen form in acrylonitrile wastewater, rather than have the denitrification capacity.