In a tungsten and molybdenum mine located in Inner Mongolia, the primary metal sulfides include pyrite, pyrrhotite, arsenopyrite, molybdenite, sphalerite, and galena. The main metal oxide minerals found are wolframite and limonite, while the predominant gangue minerals consist of quartz, feldspar, mica, amphibole, topaz, and chlorite. Wolframite and wolframite are the target minerals recovered in the experiment. Molybdenum minerals mainly exist in the form of sulfide minerals such as molybdenite, and the distribution rate is 97.02%. Tungsten mainly exists in the form of wolframite, with a distribution rate of 90.34%. To achieve high efficiency separation of molybdenum and tungsten from tungsten and molybdenum ore, flotation and gravity experiments separation were carried out. The findings indicate that in a closed-circuit test for molybdenum flotation of tungsten and molybdenum ore with a Mo grade of 0.16% and a WO₃ grade of 0.35%, the separation index achieved for molybdenum fine ore is 0.323%, with a Mo grade of 46.070% and a recovery rate of 94.330%. The re-separation of molybdenum tailings through coarse, medium, and selection shaking tables in the tungsten separation process resulted in a final yield of tungsten fine minerals at 0.548%, with a WO₃ grade of 55.360% and a recovery rate of 86.713% based on technical indicators. The results can provide technical basis for the separation of tungsten and molybdenum ore.