The preparation of highly pure vanadyl sulfate from sulfate solutions containing impurities of iron and aluminumwas investigated by solvent extraction with 2-ethylhexyl phosphoric acid mono-2-ethylhexyl ester (EHEHPA) and tri-n-butyl phosphate (TBP) as the phase modifier. The extraction and stripping conditions of vanadium (IV) and its separation from iron and aluminum were optimized. Under the optimal extraction conditions, the extraction of vanadium (IV) and iron were 68% and 53%, respectively, while only 2% aluminum was extracted in a single contact, suggesting good separation of vanadium (IV) from aluminum. Sulfuric acid solution was used for the stripping. Nearly 100% vanadium (IV) and 95% aluminum were stripped, while only 10% iron was stripped under the optimal stripping conditions in a single contact, suggesting good separation of vanadium (IV) from iron. After five stages of extraction and stripping, highly pure vanadyl sulfate containing 76.5 g/L V (IV) with the impurities of 12 mg/L Fe and 10 mg/L Al was obtained, which is suitable for the electrolyte of a vanadium redox flow battery. Organic solution was well regenerated after stripping by oxalic acid solution to remove the remaining iron. The mechanism of vanadium (IV) extraction using EHEHPA was also discussed based on the Fourier transform infrared spectroscopy (FT-IR) analysis.
24 March 2023 in Metallurgical and Materials Transactions B
Natisite (Na2TiSiO5) is a layered sodium titanosilicate containing TiO5 square pyramids. The structure evolution of natisite in water and acid solutions is the basis for its potential applications. With Na2SiO3 as the silicon source, natisite with the shape of the square sheet was selectively prepared from the hydrothermal method with 14.3 mol/L NaOH solution at 240 °C. Natisite has 20 Raman active modes and 22 infrared active modes from the first-principles calculations within density functional theory, and the calculated Raman and infrared spectra agree well with the experimental ones. The characteristic Raman peak at 844 cm−1 is caused by the symmetric stretching of the apical Ti–O bond in the TiO5 unit, assigning to A1g and B2g modes. Natisite remains relatively stable in water with a sodium leaching percentage of lower than 6%. When washing with sulfuric acid solutions, the interlayer spacing of natisite is reduced due to the extensive removal of sodium ions, and an intermediate composed of SiO4 and newly formed TiO6 units may be formed. Moreover, after washing with water and acid solutions, 95.5%, 63.4%, and 35.2% of Na, Si, and Ti in natisite can be leached in total, respectively, resulting in the structural disintegration of natisite.