Metallic Mg is an important strategic metal and its properties are greatly affected by impurities. Silicothermic reduction and electrolysis are the most used approaches to prepare metallic Mg. The products of these processes need to be further refined to obtain high-purity Mg metal. However, previous research has mainly focused on refining the crude Mg (CM) produced via silicothermic reduction, whereas no in-depth investigations have been conducted on refining the CM produced via electrolysis. Here, vacuum distillation was used to refine electrolytically produced CM. The content and morphological characteristics of the impurity elements in CM were studied via glow discharge mass spectrometry, mineral dissociation analysis, and electron probe microanalysis. The effect of different distillation temperatures and times on the quality of the refined Mg was investigated. The results show that the main impurity elements are Al, Fe, Si, Ti, Cr, S, Cl, and Ni. The content of impurities, such as Si, Al, Fe, Ni, Ti, and Cr, in the refined Mg is significantly reduced at a temperature of 1023 K and a time of 120 min, and the purity of the refined Mg reaches 99.99%, which meets the Mg9999 national standard for primary Mg ingots in China (GB/3499-2011).
After decades of development of the vanadium titanomagnetite (VTM) ore in the Panzhihua district changes have taken place to the ore characteristics. In addition, preliminary research carried out in this area mainly focused on the separation and extraction of iron resources and lacked a systematic research focus on the process mineralogy of ilmenite, resulting in a low grade and yield of the separated ilmenite. Therefore, the present study investigates the compositions, textures, element distributions, and particle size characteristics of VTM ores in Panzhihua were studied via mineral dissociation analysis (MLA), electron microscope–microprobe analysis (EPMA), scanning electron microscopy (SEM), and X-ray diffraction (XRD). The results show that the chemical and mineral compositions of the VTM ore samples were basically stable. However, the size of the embedded particles of ilmenite and titanomagnetite was smaller than that reported previously. In addition, the olivine content was found to have significantly increased, and a large number of altered minerals (such as chlorite and sphene) were also present, as a result of which the degrees of monomer dissociation of ilmenite and titanomagnetite reached 85% when the fraction of particles with size in the range of 0.04–0.15 mm was 75%.
Titanium tetrachloride (TiCl4) is an important intermediate material for the preparation of titanium products. The organic impurities in TiCl4 are easily accumulated during the production of titanium sponges due to the problems of imperfect detection methods and the lack of effective control methods, resulting in a poor quality of sponge titanium. Among all impurities, chloroacetyl chloride (CAC) is the most important in TiCl4. Herein, the determination of the CAC content in TiCl4 solution, with a low detection limit of 0.633 ppm, was established by the standard addition method using Fourier transform infrared (FTIR) spectrometry. This test method presented good repeatability, excellent accuracy, and moderate precision. Furthermore, the influencing factors of CAC separation in the continuous rectification process, including the heating power (the ratio of total heating power to feed rate), reflux temperature, top tower pressure, and feed temperature were optimized based on an orthogonal experimental design. The experimental data demonstrated that the average CAC removal rate reached 78.94% ± 1.00% under the optimal distillation conditions, with 72.21% of the CAC removed via the off-gas system. Therefore, excellent control of the negative pressure of the tail gas is highly desirable for the removal of CAC impurities.
Vanadium titanomagnetite (VTM) is an important mineral for developing titanium resources, but the comprehensive recovery of ilmenite separation is extremely poor, resulting in the low-efficiency utilization of titanium resources. Here, the separation of ilmenite from VTM ore is studied by combining magnetic separation and flotation technologies. In particular, the floatability of mixed MOH/PG-1 collectors is thoroughly investigated. The results show that a concentrate with a TiO2 grade of 9.90% can be separated via weak magnetic separation and coarse particle tailing dumping. The concentrate grade is then increased to 14.32% via strong magnetic separation and floating separation of sulfur minerals. Finally, a TiO2 grade of 46.34% is obtained through closed-circuit flotation using mixed MOH/PG-1 collectors. The mixed collectors are very efficient and can enhance the chemical adsorption of the Ti4+, Fe3+, and Fe2+ ions in the ilmenite concentrate compared with the MOH collector, thereby increasing the TiO2 grade and recovery by 3.31% and 1.20%, respectively. This is beneficial for improving the comprehensive utilization of titanium resources in VTM ores.
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