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Experimental work has been performed to investigate the precipitation mechanism of aluminum hydroxide phases from sodium aluminate/sodium carbonate pregnant solutions by carbon dioxide gas purging. Such solutions result from leaching calcium aluminate slags with sodium carbonate solutions, in accordance with the Pedersen process, which is an alternative process for alumina production. The concentration of carbonate ions in the pregnant solution is revealed as a key factor in controlling the nature of the precipitating phase. Synthetic aluminate solutions of varying sodium carbonate concentrations, ranging from 20 to 160 g/L, were carbonated, and the resulting precipitating phases were characterized by X-ray diffraction analysis. Based on the results of the previous carbonation tests, a series of experiments were performed in which the duration of carbonation and the aging period of the precipitates varied. For this work, a synthetic aluminate solution containing 20 g/L free Na2CO3 was used. The precipitates were characterized with X-ray diffraction analysis and Fourier-transform infrared spectroscopy.

A low-temperature, low-energy method for recovering all the valuable, economically viable, components from the spent lithium-ion batteries has been developed which has allowed the determination of pathways for complete recycling of the battery. Lithium present in the electrolyte has been selectively leached from lithium-ion batteries. Leaching conditions were optimized including time, temperature, solid/liquid ratio, and stirring velocity. All the samples were analyzed using ICP-MS for chemical composition. Leaching is conducted in a flotation machine that was able to separate plastics by flotation, creating bubbles without the use of any external chemical excess reagents. The pregnant solution was concentrated with lithium to a higher amount in order for it to be precipitated, and it was shown that the solution could be concentrated by recirculation of the leach solution. The next set of experiments were composed of battery shredding, steel separation by magnets, leaching with distilled water, and sizing using wet sieving to account for all the components of the battery. Every fraction is sent to rare-earth rolls separation and eddy current separation for full recovery.

Leaching experiments were performed in calcium aluminate slag with a high-sodium carbonate adaptation of the Pedersen process. A theoretical thermodynamic study of the pregnant leaching solution was conducted to specify the thermodynamically favored species that exist within. Using the HSC 9.0 software, a carbonation process simulation (neutralization of the aluminate solution with CO2 gas) was simulated. Laboratory carbonation experiments were conducted to verify the theoretical predictions. According to the thermodynamic study, at temperatures below 50 °C gibbsite precipitates in the first stages of carbonation and then is transformed to dawsonite. Temperatures over 65 °C favor the direct precipitation of dawsonite. The same route (thermodynamic analysis, carbonation simulation, and experimental verification) was followed by a synthetic solution containing lower amount of sodium carbonate to prove that dawsonite precipitation occurred as a result of the high free carbonate content, to investigate the effect of temperature and to precipitate alumina hydrate phases. Graphical Abstract

This study investigates applying the principles of the long-discontinued Pedersen process as a possible route for producing metallurgical grade alumina from low-grade and secondary feed materials. The investigation focused on the hydrometallurgical steps in the process, namely leaching, desilication, and precipitation, and adapting it to valorize bauxite residue. The test material used was a calcium–aluminate slag made by the smelting-reduction of a mixture of bauxite residue (dewatered red mud) and a calcium-rich bauxite beneficiation by-product. Samples of the slag were leached in a 1 L jacketed glass reactor with Na2CO3 solution, varying Na2CO3 concentration and leaching time. Additionally, different approaches to leaching involving mechanical treatment of the leached slag and re-leaching using either fresh or recycled solution were also explored. The desilication step was carried out by treating the leachate solution with powdered CaO, varying the amounts of CaO used. Finally, the desilicated leach solution was sparged with a CO2 gas mixture, after which the precipitate was allowed to age in the solution. The carbonation and aging temperatures and times were varied. As much as 67% of the Al was leached from the slag. The desilication process successfully removed 88% of the Si. The precipitation process produced a product composed mostly of bayerite [Al(OH)3], but some tests had considerable amounts of the unwanted phase dawsonite [NaAlCO3(OH)2]. The results indicated that the highest Al recovery was obtained using low concentrations of Na2CO3 solutions, and aluminum tri hydroxide is formed from these solutions at low temperatures at a fast rate compared to higher solution concentrations and temperatures.