Observations on the Leaching of Milled Black Mass with Additives

In this work, previously produced black mass was treated in sequence by milling, water leaching, and sulfuric acid leaching. Two goals were set: first, whether milling, with reductive additives, could impart reductive phase changes which would allow Li extraction to water in the water leaching; second, co-leaching of the black mass with the additive, CoS, was explored as to ascertain whether synergistic effects could be detected in a leaching system composed of reductive (CoS) and oxidative (NMC oxides) materials in the presence of redox mediator (Fe²⁺/Fe³⁺ redox pair). It was found out that in all experiments, similar Li concentration was obtained despite milling. Fluoride analysis indicated high F concentrations in the water solution and implicated formation of insoluble products such as LiF(s). Water-soluble fluoride ended up in all fractions: water leaching filtrates (ca. 500 mg/L), acid leaching filtrates (ca. 800–1700 mg/L), and leach residues (ca. 68–382 mg/kg). In acidic leaching, CoS appeared to enhance extraction of elements from cathode-active materials, improving extraction from 78 to 92% for Ni under relatively mild leaching conditions (T = 30 °C, solid conc. = 100 g/L, [H₂SO₄] = 1.4 M).