The Hall–Héroult aluminum production process generates lithium-rich waste barrier materials, which are challenging to process using conventional acid leaching due to the environmental risks posed by hydrofluoric acid (HF) emissions. This research introduces a two-stage water–HCl sequential leaching (WHSL) approach to recover lithium while reducing these environmental impacts. The method evaluates key factors, such as the liquid–solid ratio, temperature, duration, rotation speed, and HCl concentration, and compares its efficacy with traditional HCl leaching using XRD, FTIR, DBP, and SEM techniques. The findings indicate that initial water leaching dissolves NaF salts, creating surface grooves and cracks. Subsequent HCl leaching selectively extracts lithium from aluminum and silicon, forming silica gel while preserving the nepheline phase due to its structural integrity. The process produces a porous residue with smaller particles, reduced surface potential, and promotes colloidal aggregation. This two-step process achieves efficient lithium recovery while reducing acid consumption and minimizing hydrogen fluoride (HF) emissions. [ABSTRACT FROM AUTHOR]

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