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).
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.
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