Abstract: The grade of copper, sulfur, gold and silver in a gold-silver-copper-sulfur ore is 0.70%, 4.76%, 0.10g/t and 3.78g/t, respectively. The ore was taken as the research object in this paper where flotation experiments were systematically carried out with the process of "copper rapid flotation-copper tail activation sulfur separation" under the condition of low slurry alkalinity to reduce the high loss rate of associated gold and silver which was a problem encountered in actual production with high pulp alkalinity process. The closed-circuit test results showed that the copper concentrate and sulfur concentrate could be obtained. The former has copper grade of 24.28% with recovery of 91.93% and the latter has sulfur grade of 45.54% with recovery of 44.76%. Copper concentrate was enriched in 61.51% of gold and 63.86% of silver with good flotation index, and comprehensive recovery of valuable metals was realized in raw ore under low alkali condition.