The hydrometallurgical extraction of metals from spent lithium-ion batteries (LIBs) was investigated. LIBs were first dismantled and a fraction rich in the active material was obtained by physical separation, containing 95% of the initial electrode, 2% of the initial steel and 22% of plastic materials. Several reducers were tested to improve metals dissolution in the leaching step using sulphuric acid. Sodium metabisulphite led to the best results and was studied in more detail. The best concentration of Na2S2O5 was 0.1 M. The metals dissolution increased with acid concentration, however, concentrations higher than 1.25 M are unnecessary. Best results were reached using a stirring speed of 400 min-1. The metals leaching efficiency from the active material (Li, Mn, Ni, Co) increased with the temperature and was above 80% for temperatures higher than 60 °C. The dissolution of metals also rose with the increase in the liquid/solid ratio (L/S), however, extractions above 85% can be reached at L/S as lower as 4.5 L/kg, which is favourable for further purification and recovery operations. About 90% of metals extraction can be achieved after only 0.5 h of leaching. Sodium metabisulphite can be an alternative reducer to increase the leaching of Li, Mn, Co, and Ni from spent LIBs.

The lithium extraction from a lepidolite concentrate using roasting, followed by water leaching, was studied. Several alternative additives were initially tested. The use of sodium and calcium sulfates as additives was evaluated in more detail. The influence of some process variables, namely the roasting time, roasting temperature and the additive/concentrate mass ratio, was studied applying a design of experiments. The lithium extraction was modelled and the fitted and validated model was used to optimize the process response. The increase in the additive/concentrate mass ratio, roasting time and temperature seems to result in solid state reactions and transformations that lead to phase, morphological and particle size distribution modifications, which were assessed by XRPD, SEM, and particle size analyses. In this process, lithium sodium sulfate formation constitutes a crucial step enabling the Li water leaching. High lithium extractions were estimated for several combinations of factors. At 850°C, lithium extractions over 90% are obtained when the roasting time is above 1.90 hour and the additive/concentrate mass ratios are over 0.77. An increase in the temperature to 875°C also leads to lithium extractions over 90% for a roasting time of 1 hour and an additive/concentrate mass ratio of 0.60.