A simple and efficient approach for the high-purity CaSO₄·2H₂O (DH) whiskers and α-CaSO₄·0.5H₂O (α-HH) whiskers derived from such phosphogypsum (PG) was proposed. The impact of different experimental parameters on supersaturated dissolution–recrystallization and preparation processes of α-CaSO₄·0.5H₂O was elaborated. At 3.5 mol/L HCl concentration, the dissolution temperature and time were 90 °C and 20 min, respectively. After eight cycles and 5–8 times cycles, total crystallization amount of CaSO₄·2H₂O was 21.75 and 9.97 g/100 mL, respectively, from supersaturated HCl solution. The number of cycles affected the shape and amount of the crystal. Higher HCl concentration facilitated CaSO₄·2H₂O dissolution and created a much higher supersaturation, which acted as a larger driving force for phase transformation of CaSO₄·2H₂O to α-CaSO₄·0.5H₂O. The HCl solution system’s optimum experimental conditions for HH whiskers preparation involved acid leaching of CaSO₄·2H₂O sample, with HCl concentration 6.0 mol/L, reaction temperature 80 °C, and reaction time 30 min–60 min. Under the third cycle conditions, α-CaSO₄·0.5H₂O whiskers were uniform in size, clear, and distinct in edges and angles. The length range of α-CaSO₄·0.5H₂O whiskers was from 106 μm to 231 μm and diameter range from 0.43 μm to 1.35 μm, while the longest diameter ratio was 231. Purity of α-CaSO₄·0.5H₂O whiskers was approximately 100%, where whiteness reached 98.6%. The reuse of the solution enables the process to discharge no waste liquid. It provides a new reference direction for green production technology of phosphogypsum.

In this study, the effect of citric acid on iron leaching from titanium gypsum (TiG) was systematically investigated. The conditions for the leaching of valuable metals were optimized while varying such parameters as the leaching time, citric acid mass fraction, leaching temperature, and the liquid–solid ratio. It was found that under the conditions of a citric acid mass fraction of 10%, at a 80 °C leaching temperature, a leaching duration of 80–90 min and a liquid–solid ratio of 8, the whiteness of titanium gypsum (TiG) increased from 8.1 to 36.5, and the leaching efficiencies of iron reached 84.37%. The kinetic analysis indicated that the leaching process of iron from TiG was controlled by the reaction product layer from 0–20 min, while the leaching process of iron from TiG was controlled by internal diffusion from 20–90 min. The apparent activation energy of the leaching reactions was 33.91 kJ/mol and 16.59 kJ/mol, respectively. High-value-added calcium oxalate and ferrous oxalate were prepared from the calcium and iron in the filtrate of the oxalic acid extraction. The leaching liquid could be recycled, which will provide a new way to utilize titanium gypsum.