The electro-oxidation is an environment-friendly hydrometallurgy technique of extraction from molybde-nite concentrate,with moderate reacting conditions and high metal recovery.In this paper,aiming at the key step of the technique,namely the separation of Mo（Ⅵ） and Re（Ⅶ）,some experiments were performed.The results show that,when the mixture of 30% N235＋20% sec-caprylic alcohol＋50% kerosene oil is used as the extractant for the extraction with a W/O ratio of 1∶2 and an acidity of 59g/L HCl at room temperature,the single-stage extraction rates of Mo（Ⅵ） and Re（Ⅶ） respectively reach 99.95% and 95.76%;and that,when 17% ammonia is used as the stripping agent for the stripping with a W/O ratio of 2∶1 at room temperature,the stripping rates respectively reach 99.49% and 98.35%.