A new process for the development and utilization of titanium-iron sand ore from Yunnan province is proposed. We provide a detailed analysis of the chemical composition and mineral structure of the raw material, and describe a pretreatment involving low-temperature oxidation and reduction, hydrofluoric acidolysis, and hydrochloric acid leaching to remove impurities and generate titanium-rich materials. Hydrofluoric acid was used to break down the complex titanite, silica-titanium, and calcium-titanium mixture in the starting mineral into simple oxides. The results have indicated that the thermal reduction process should not be conducted at elevated temperatures. Optimal process conditions are established for the leaching process: leaching temperature of 80 °C; leaching time of 240 min; hydrofluoric acid concentration of 3%; liquid–solid ratio of 6 m l/g. Under these conditions, the extent of TFe leaching reached 96%, while the leaching of Ca and Mg reached 94%. The TiO2 grade of the final titanium-rich material was 89.95%, with a CaO content of 0.39%, a MgO content of 0.15%, and a TFe content of 7.5%. This material can serve as raw material for subsequent chlorination.
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