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Date submitted2024-04-10
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Date accepted2024-06-03
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Date published2025-04-25
Combined method for processing spent acid etching solution obtained during manufacturing of titanium products
Possessing high strength, low density and significant chemical resistance, titanium has found wide application in various fields of the national economy – the chemical industry, aviation and rocket technology, mechanical engineering, medicine, etc. The production of titanium products is hampered by a fairly strong oxide film covering its surface. Removal of the oxide film from the surface of titanium workpieces is carried out by etching in solutions of mineral acids of various compositions. A spent acid etching solution (SAES) is formed, containing titanium salt and the remainder of unreacted acids. Almost all etching solutions contain HF and one of the strong acids. This is H2SO4, HCl or HNO3. Thus, the SAES includes ions of titanium, fluorine or chlorine, orsulfate, or nitrate. SAES is quite toxic and must be diluted or cleaned several times before being discharged into a reservoir. Most of the methods used to extract impurities contained in SAES lead to a decrease in their content. As a result of such purification, there is a loss of substances contained in SAES in significant quantities and of interest for further use. The work presents experimental results obtained from the combined processing of SAES containing titanium fluoride, hydrofluoric and hydrochloric acids. At the first stage, SAES is treated with sodium hydroxide. The resulting titanium hydroxide precipitate is filtered off. At the second stage, the filtrate containing sodium fluoride and chloride is processed in a membrane electrolyzer. In this case, not only the extraction of sodium salts from the filtrate occurs, but also the production of sodium hydroxide and a mixture of hydrofluoric and hydrochloric acids. Sodium hydroxide can be used for processing SAES, and a mixture of acids for etching titanium workpieces.
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Date submitted2022-10-10
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Date accepted2023-01-19
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Date published2023-12-25
Assessment of the possibility of using leucoxene-quartz concentrate as raw material for production of aluminium and magnesium titanates
Leucoxene-quartz concentrate is a large-tonnage by-product of development of the Timan oil-titanium field (oil-saturated sandstones) which is not commercially used at present. High content of titanium compounds (to 50 % by weight) and lack of industrial, cost-effective, and safe technologies for its processing determine a high relevance of the work. Conventional processing technologies allow increasing the concentration of TiO2, but they are only a preparation for complex and hazardous selective chlorination. The process of pyrometallurgical conversion of leucoxene-quartz concentrate into aluminium and magnesium titanates was investigated. It was ascertained that the temperature of solid-phase reaction in Al2O3-TiO2-SiO2 system necessary for the synthesis of aluminium titanate (Al2TiO5) is 1,558 °С, and for MgO-TiO2-SiO2 system – 1,372 °С. Scaling up the process made it possible to synthesize a significant number of samples of titanate-containing products, the phase composition of which was studied by X-ray phase analysis. Two main phases were identified in the products: 30 % aluminium/magnesium titanate and 40 % silicon dioxide. In products of pyrometallurgical processing in the presence of aluminium, phases of pseudobrookite (3.5 %) and titanite (0.5 %) were also found. It was ascertained that in magnesium-containing system the formation of three magnesium titanates is possible: MgTiO3 – 25, Mg2TiO4 – 35, MgTi2O5 – 40 %. Experiments on sulphuric acid leaching of samples demonstrated a higher degree of titanium compounds extraction during sulphuric acid processing. An integrated conceptual scheme for processing leucoxene-quartz concentrate to produce a wide range of potential products (coagulants, catalysts, materials for ceramic industry) was proposed.