The preparation of high-performance electrode materials from metallurgical solid waste is an effective strategy to address current energy and environmental challenges. This study utilizes a mixed acid leaching and ultrasound-assisted precipitation process to extract valuable metallic iron from titanium-extraction tailings (TET) to produce high-purity nano-FePO4 electrode material precursors with unique crystal structures. A leaching efficiency of 95.2% for Fe was attained by using the optimized process parameters, which included a mixed acid concentration of 4 mol/L, a liquid-to-solid ratio of 4:1, and a leaching temperature of 70 °C for 1 h. The optimal precipitation conditions were a pH of 2.0, a temperature of 60 °C, an aging time of 30 min, and a stirring speed of 600 rpm, resulting in FePO4 purity up to 99.6% and fine particle size. Thermodynamic calculations, combined with various characterizations, elucidated the leaching and precipitation mechanisms, highlighting the synergistic effect of phosphoric acid and hydrochloric acid in enhancing the leaching reaction. The thermogravimetric analysis indicated that the decomposition of residual ammonium chloride impurities requires calcination above 360 °C. This research not only provides new insights into the high-value, clean utilization of metallurgical solid waste but also supports sustainable resource recovery and environmental protection by transforming waste into valuable products.
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