Red mud is a by-product of alumina production, which is largely stored in landfills that can endanger the environment. Red mud, or bauxite residue, is a mixture of inorganic compounds of iron, aluminum, sodium, titanium, calcium and silicon mostly, as well as a large number of rare earth elements in small quantities. Although certain methods of using red mud already exist, none of them have been widely implemented on a large scale. This paper proposes a combination of two methods for the utilization of red mud, first by carbothermic reduction and then, by leaching under high pressure in an autoclave in order to extract useful components from it with a focus on titanium. In the first part of the work, the red mud was reduced with carbon at 1600 °C in an electric arc furnace, with the aim of removing as much iron as possible using magnetic separation. After separation, the slag is leached in an autoclave at different parameters in order to obtain the highest possible yield of titanium, aiming for the formation of titanium oxysulfate and avoiding silica gel formation. A maximal leaching efficiency of titanium of 95% was reached at 150 °C using 5 mol/L sulfuric acid with 9 bar oxygen in 2 h. We found that high-pressure conditions enabled avoiding the formation of silica gel during leaching of the slag using 5 mol/L sulfuric acid, which is a big problem at atmospheric pressure. Previously silica gel formation was prevented using the dry digestion process with 12 mol/L sulfuric acid under atmospheric pressure.

Comparative analysis of red mud reduction techniques was performed using both carbothermal and hydrogen-based reduction methods, combining thermochemical modeling and experimental validation. The reduction process is mostly important because of the high contamination risk assessment of soil with disposed red mud. Therefore, the minimization of red mud during the reduction process can be a novel strategy for the production of metallic iron and solid residue for hydrometallurgical treatment. Different strategies of hydrogen and carbon reduction in static and dynamic conditions were studied between 700 °C and 1700 °C. The separation of solid residue and formed iron was analyzed using magnetic separation. The main aim was to study the advantages and disadvantages of using decarbonizing technologies for the treatment of red mud, aiming to develop an environmentally friendly process. Thermochemical analysis of the reduction offered new data about mass losses during our process through the evaporation, thermal decomposition, and formation of metallic carbide.

The influence of process parameters in the three-stage purification of aluminate solution from the Bayer process and aluminum hydroxide was considered in this paper. One of the ways of purification is treating the aluminate solution in order to reduce the concentrations in the starting raw material (solution) and then treating the aluminum hydroxide at a certain temperature and time in order to obtain an alumina precursor of adequate quality. The purification process itself is divided into three phases. The first phase involves the treatment of sodium aluminate with lime in order to primarily remove Ca²⁺ and (SiO₃)²⁻ impurities. Phase II aims to remove impurities of Zn²⁺, Fe²⁺, and Cu²⁺ by treatment with controlled precipitation using specially prepared crystallization centers. In Phase III, Na⁺ is removed by the process of hydrothermal washing of Al₂O₃ ∙ 3H₂O. In this work, parameters such as temperature (T), reaction time (t), and concentration of lime (c) were studied in order to remove the mentioned impurities and obtain the purest possible product that would be an adequate precursor for special types of alumina.

Submicron and nanosized powders have gained significant attention in recent decades due to their broad applicability in various fields. This work focuses on ultrasonic spray pyrolysis, an efficient and flexible method that employs an aerosol process to synthesize titanium-based nanoparticles by transforming titanium oxy-sulfate. Various parameters are monitored to better optimize the process and obtain better results. Taking that into account, the influence of temperature on the transformation of titanium oxy-sulfate was monitored between 700 and 1000 °C. In addition to the temperature, the concentration of the starting solution was also changed, and the flow of hydrogen and argon was studied. The obtained titanium-based powders had spherical morphology with different particle sizes, from nanometer to submicron, depending on the influence of reaction parameters. The control of the oxygen content during synthesis is significant in determining the structure of the final powder.

The synthesis of oxide nanopowders through ultrasonic spray pyrolysis (USP) represents a sustainable method for producing high-purity, spherical particles tailored for advanced material applications. Recent developments in USP synthesis leverage the continuous transport of aerosols from an ultrasonic generator to a high-temperature furnace, with nanopowders collected efficiently using an electrostatic precipitator. This study explored the use of USP for titanium oxysulfate and aluminum nitrate solutions derived from the aluminum industry, focusing on resource recovery and waste reduction. Titanium oxysulfate was synthesized by leaching slag, generated during the reduction of red mud, with sulfuric acid under oxidizing, high-pressure conditions. After purification, the titanium oxysulfate solution was processed using USP in a hydrogen reduction atmosphere to yield spherical titanium dioxide (TiO₂) nanopowders. The hydrogen atmosphere enabled precise control over the nanoparticles’ morphology and crystallinity, enhancing their suitability for use in applications such as photocatalysis, pigments, and advanced coatings. In parallel, both synthetic and laboratory solutions of aluminum nitrate [Al(NO₃)₃] were prepared. The laboratory solution was prepared by leaching aluminum hydroxide oxide (AlOOH) with hydrochloric acid to form aluminum chloride (AlCl₃), followed by a conversion to aluminum nitrate through the addition of nitric acid. The resulting aluminum nitrate solution was subjected to USP, producing highly uniform, spherical alumina (Al₂O₃) nanopowders with a narrow size distribution. The resulting nanopowders, characterized by their controlled properties and potential applicability, represent an advancement in oxide powder synthesis and resource-efficient manufacturing techniques.

This study explores both pyrometallurgical and hydrometallurgical methods for decarbonizing and recovering valuable metals from bauxite residue, with hydrogen plasma reduction and direct acid leaching as the primary approaches. The goal is to offer innovative techniques for extracting metals from bauxite residue, a by-product of the Bayer process, which cannot be disposed of in an environmentally sustainable manner. Additionally, reducing the volume of bauxite residue through combined treatments is a key objective. In contrast to traditional carbon-based reductive melting, which generated significant CO₂ emissions, hydrogen is now being investigated as a cleaner alternative. Through hydrogen plasma reduction, approximately 99.9% of iron is recovered as crude metallic iron, which can be easily separated from the slag containing other valuable metals. Thermochemical analysis was used to predict slag formation and chemical analysis of slag during hydrogen reduction. To further recover metals like aluminum and titanium, the slag is subjected to sulfuric acid leaching under high-pressure of oxygen in an autoclave avoiding silica gel formation. The results demonstrated a leaching efficiency of 93.21% for aluminum and 84.56% for titanium, using 5 mol/L sulfuric acid at 150 °C, with almost complete iron recovery. Assisted ultrasound leaching of slag with sulphuric acid under atmospheric pressure leads to 54% leaching efficiency of titanium.