This article presents the results of studies on the distribution of rare metals among the products of the alkali sulfate processing of nepheline syenites. In response to the limited reserves of Bayer bauxite in the alumina industrial production region of Kazakhstan, the feasibility of using alternative alumina-containing nonbauxite raw materials was investigated. The most promising nonbauxite raw materials in Kazakhstan are nepheline and kaolinite clays. At present, there is no effective technology for processing nepheline ores. This article describes a proposed complex technology involving nepheline processing with the associated extraction of gallium and vanadium. The technology includes the activation of raw materials, followed by two-stage leaching, where potassium is extracted in the first stage. The sludge and solution obtained from the second stage of the leaching process are utilized for calcium silicate production and two-stage carbonization, respectively. In the first stage, aluminum hydroxide is extracted, and, in the second stage, a concentration of rare metals, such as gallium and vanadium, is obtained. Vanadium is extracted from the solution via crystallization, and gallium is extracted via electrodeposition. Overall, 38.48% of the Ga2O3 and 56.12% of the V2O5 are recovered from raw nepheline syenite. A technological scheme of the developed technology is presented in this article.