Abstract: By using 188 Re as a tracer, the extraction behavior of Re with N 235 in dimethylbenzene is studied. A chemical separation procedure,which consists of the elution from the acid alumina column and the liquid liquid extraction with N 235 in dimethylbenzene is established. The procedure is rapidly and efficiently used for the separation of 186 Re from 186 W irradiated by 16 MeV deuterons.Carrier free 186 ReO 4 - saline solution with high radioactive concentration is obtained, and no radioactive impurities of 187 W and 183 Ta are found. The overall recovery yield of 186 Re is about 85 %.