Abstract: In this paper, the flotation separation of a gross sand of gravity separation of tungsten richly containing Cu and Mo sulfide minerals obtained by jigging process was studied. According to the above sample’s property, the process of bulk flotation of copper and molybdenum minerals, and then flotation separation of copper and molybdenum minerals was adopted. The effective activator BK546 was used to reduce the content of sulfur in tungsten concentrate and improve the recoveries of copper and molybdenum. The results of the closed circuit obtained a molybdenum concentrate with Mo grade of 57.90%, Cu grade of 0.68% and molybdenum recovery rate of 96.44%; a copper concentrate with Cu grade of 37.32% and copper recovery rate of 99.64%; a tungsten concentrate with WO₃ grade of 68.12%, Cu grade of 0.025%, Mo grade of 0.005% and WO₃ recovery rate of 97.30%. It can be achieved the effective separation recovery of the tungsten, copper and molybdenum minerals from the ore by using the new process studied.