Currently, in the development of the raw materials base of the gold mining industry, there is a tendency to reduce the quality of the initial mineral raw materials due to the depletion of reserves of rich gold-bearing ores. The article discusses the technology of extraction of refractory gold-bearing concentrates based on low-temperature leaching of pyrite concentrate. A decrease in the parameters of the autoclave oxidation of sulfide minerals, such as pyrite and arsenopyrite, leads to the incomplete extraction of gold into the solution and, consequently, its losses during subsequent cyanidation. As a possible option for a more complete extraction of gold using low-temperature oxidation technology, a method of flotation separation of elemental sulfur from leaching cakes is proposed. According to the basic process flow chart, the flotation process designed for gold extraction is carried out after autoclave oxidation, but before cyanidation. A series of experiments were carried out with varying reagent conditions and the dependence of gold losses on the extraction of elemental sulfur in the flotation tailings was established. As determining factors, pH and solid content in the initial pulp were considered. The paper justifies the separation of elemental sulfur from autoclave cake to enriched sulfur concentrate. The cake flotation modes after autoclave oxidative leaching of pyrite concentrate are investigated. The distribution of elemental sulfur and gold by flotation products makes it possible to conduct the tailings cyanidation process with acceptable indicators.