<p>Antimony, with its unique chemical properties, plays a critical role in enhancing the hardness of metals and finds extensive application across various industries. This study explores an innovative hydro-pyrometallurgical process for antimony recovery from stibnite concentrate, combining the advantages of hydrometallurgical precision and pyrometallurgical robustness to achieve high recovery rates and product purity. A key feature of the proposed approach is the integration of sulfur fixation in the solid phase and operation at significantly lower temperatures compared to standard oxidative roasting. In this work, mechanically activated antimony concentrate was chlorinated and roasted with NaCl to minimize sulfur dioxide emissions, eliminating the need for costly gas treatment systems. Thermodynamic simulations identified that suitable SbCl₃ recovery occurs in the gas phase at relatively low temperatures (160–400&#xa0;°C), offering a notable advantage over conventional pyrometallurgical methods. The residual solid, containing approximately 50% of the initial antimony, was processed further using hydrometallurgical techniques. Experimental results demonstrated that about 80% of antimony was successfully extracted under the investigated conditions. Additionally, electrowinning experiments achieved an 83% extraction efficiency, producing antimony with a purity of at least 98%. This study highlights the potential of the proposed method to improve antimony recovery efficiency while reducing environmental impact, offering a promising pathway for sustainable and economically viable processing.</p>