This Doctoral Thesis focuses on the recovery by electrodeposition of Sb present in an effluent from the copper metallurgy. The effluent on which this study is based is generated during the regeneration with concentrated hydrochloric acid of the ion exchange resins used in one of the sub-stages of copper electro-refining. It is an acid electrolyte containing several impurities, among them, antimony and bismuth, which are considered critical raw materials by the European Union due to their supply risk and economic relevance.