The present invention relates to sulfur slag vacuum volatilizing process for enriching noble metal, and belongs to the field of vacuum fire metallurgy process. Sulfur slag material is distilled in a vacuum smelting furnace at pressure of 10-30 Pa and temperature of 250-400 deg.c for 50-120 min to volatilize sulfur and the sulfur vapor is cooled to form liquid and exhausted from the vacuum smelting furnace, so as to obtain metal sulfide powder with enriched Cu, Ni, Os, Ag, Au, etc. The process is simple, and has high noble metal enriching ratio, no environmental pollution, low power consumption and low production cost.