Based on the difference in tendency to polymerize between tungsten and molybdenum, a new method using D309 resin was propounded. The batch tests indicate that the optimum pH value and contact time for the separation are 7.0 and 4 h respectively, the maxium separation factor of W and Mo is 9.29. And the experimental resules show that isothermal absorbing tungsten and molybdenum belongs to Langmuir model and Freundlich model respectively, and the absorbing kinetics for tungsten is controlled by intra-particle diffusion. With a solution containing 70 g/L WO3 and 28.97 g/L Mo, the effluent with a mass ratio of Mo to WO3 of 76 and the eluate with a mass ratio of WO3 to Mo of 53.33 are obtained after column test.