(99m)Tc-99m(T1/2:6.02hr) is the most widely used radioisotope in nuclear medicine, accounting for more than 80% of all diagnostic nuclear medicine procedures. (99m)Tc is almost exclusively produced from the decay of parent (99)Mo(T1/2:66hr). The (99)Mo separation and purification process, consisted of four unit processes such as target dissolution in acid, α-benzoinoxime precipitation, adsorption on activated carbon impregnated with silver, adsorption on alumina, is proposed for domestic production in this study. And then, the the optimum process conditions are suggested, and the results of performance test of process can be reach to Mo recovery yield of 85% and Mo purification yield of 97%(requirement ≥ 95%).