By using 188Re as a radiotracer, the extraction behavior of Re(VII) by a tertiary amine extractant N-235 from HCl and the back-extraction behavior of Re(VII) by HNO3 and ammonia were studied. A chemical separation procedure, which combined the acid alumina column and solvent extraction was established. The procedure was rapid and efficient for the separation of 186Re from 186W irradiated by 16 MeV deuterons. No-carrier-added 186ReO4– saline solution with high specific volume activity was obtained. The overall recovery yield of 186Re was about 85%.