Ocean polymetallic nodules are oxide ores rich in Ni, Co, Cu, and Mn, which are valuable metals found in deep-sea mineral resources. Such non-ferrous metals do not exist in isolation, and producing concentrates using conventional mineral separation techniques is challenging without pre-treatment. We propose an effective, environmentally-friendly recovery technology combined with solid-state metalized reduction treatment and magnetic separation to recycle these metals from ocean polymetallic nodules. We conducted single-factor tests to investigate the effects of additives, anthracite dosage, duration, and reduction temperature on metal recovery and to obtain optimal operating parameters. We found that valuable metals in ocean polymetallic nodules may be selectively reduced to a metallic state. Only a fraction of Mn was reduced to metal. The reduced metals were recovered to concentrates using magnetic separation. More than 80% of these metals were concentrated to magnetic concentrates with mass ratios of 10–15%. The recovery rates of Ni, Co, Cu, Mn, and Fe in concentrates were optimum at 86.48%, 86.74%, 83.91%, 5.63%, and 91.46%, respectively, when using CaF₂ 4%, anthracite 7%, SiO₂ dosage 5%, and FeS 6% at 1100 °C for 2.5 h. This approach to non-ferrous metal extraction using conventional hydrometallurgical processes could be a step toward practical industrial-scale techniques for the recovery of metals from polymetallic nodules.

Sulfuric acid curing and leaching is a promising technology for treating refractory ores. In this work, a refractory concentrate containing 3191 ppm uranium (U), 2135 ppm niobium (Nb), and 0.7% rare earth minerals (REMs) went through two stages: curing by high-concentration H₂SO₄ and leaching by low-concentration H₂SO₄. We investigated the behavior of those valuable metals during the two stages. For both curing and leaching, the operating parameters include the acid-to-solid ratio, time, temperature, and H₂SO₄ concentration. The recovery for U, Nb, and REMs was as high as 95%, 86%, and 73.5% using a curing acid-to-solid ratio of 1:1, curing temperature of 200 °C, curing time of 1 h, H₂SO₄ concentration of 98%, leaching liquid-to-solid ratio of 4:1, leaching time of 2 h, leaching temperature of 60 °C, and leaching H₂SO₄ concentration of 5 g/L. A “sulfuric acid curing–leaching-U extraction by N235–Nb recovery by resin adsorption–REMs’ recovery by resin adsorption” method was implemented, where the overall U, Nb, and REMs’ recovery reached 93.1%, 84.5%, and 69.6%, respectively.

This study presents a combined process of sulfide precipitation followed by hydrogen peroxide leaching for rhenium recovery from copper smelting waste acid under ambient temperature and pressure. The process first removed copper through selective sulfide precipitation, then achieved co-precipitation of rhenium and arsenic to obtain a rhenium-rich precipitate. Subsequently, exploration of rhenium-containing precipitate leaching using H₂O₂ solution was conducted under isothermal conditions at 20 °C. The effects of H₂O₂ concentration, liquid-to-solid ratio, acidity, and leaching time rhenium extraction efficiency were examined systematically. The optimal leaching conditions were determined as: H₂O₂ concentration of 150 g/L, liquid-to-solid ratio of 5:1 mL/g, stirring speed of 350 r/min, and leaching time of 30 min. Under these conditions, the leaching conversions of rhenium and arsenic reached 96.0% and 93.8%, respectively. Through characterization of precipitate and leaching residue using ICP, SEM-EDS, XRD, and XPS analyses, the process and related reactions were elucidated. Results demonstrated that low-valence rhenium oxides and sulfides serve as the main reactive species during H₂O₂ leaching, whereas organic sulfur, high-valence oxides, and copper sulfide remained stable and resistant to leaching. Selective precipitation of copper effectively eliminated insoluble metal sulfides from rhenium-containing precipitates, thereby enabling efficient separation of rhenium under mild conditions.