This paper presents comparative experimental results for the single-stage and two-stage counter-current acid leaching of battery masses, with the addition of a booster, from different types of LIB waste. Three different types of battery masses were used in this research: Material I, module car; Material II, tablets and laptops; and Material III, mobile phones. These materials were obtained during the mechanical processing of Li-ion battery waste, which were dried at a temperature in the range of 80–180 °C. Leaching studies of these materials were carried out using the single-stage acid leaching method with the addition of hydrogen peroxide, and the innovative two-stage counter-current acid leaching method, also with the addition of hydrogen peroxide. The single-stage leaching of the battery mass (regardless of the composition of the material) in a 15% or 20% sulfuric acid solution with the addition of 30% H₂O₂ aqueous solution, for 2 h, with a solid-to-liquid-phase ratio of 1:5 or 1:4 at a temperature of 60 °C ensures the leaching of cobalt, nickel, copper and lithium with efficiencies above 95%. On the other hand, the use of an innovative method of two-stage counter-current leaching of the battery mass ensures the leaching of cobalt, nickel, copper and lithium at a level significantly greater than 95%, while obtaining a concentration of cobalt in the leaching solution at a level of nearly 50 g/dm³. It also reduces the leaching time of a single stage to 1 h and, importantly, reduces the amount of waste solutions and the consumption of H₂O₂ and sulfuric acid. The developed method of the two-stage counter-current leaching of battery masses is therefore characterized by high efficiency and low environmental impact, thanks to which it can be used in commercial processes for the recycling of lithium-ion batteries.

Antimony (Sb), bismuth (Bi), and arsenic (As) are common contaminants of copper (Cu) electrolyte and anodes, necessitating strict control of their concentrations. The purification of Cu electrolytes is required and demands the application of appropriate techniques. This paper presents the methodology of selective precipitation, applied for Sb, Bi, and As recovery from the acidic eluate of a Cu electrolyte purification plant. An important aspect was the change in solution type from chloride to sulfate, prior to arsenic sequestration. A facile precipitation method, preceded by a reduction in As(V) and Sb(V), was applied. The primary objectives are focused on the preparation of three distinct concentrates: antimony oxychloride, bismuth oxychloride, and iron(III) arsenate(V), emphasizing optimal recovery and purity. The processes were performed in a specially designed, cascade-lined pilot scale installation, with a daily capacity of approximately 2.5 m³. In total, 22 m³ of eluate was processed, yielding 191 kg of Sb concentrate, 97 kg of Bi concentrate, and 163 kg of scorodite. The recovery of Sb was as high as 98%, with antimony content up to 50% in the concentrate. The recovery of bismuth varied from 60 to 99%, depending on the process parameters. The elimination of arsenic from the eluate was close to 100%.