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Metals 2021, 11, 1301 11 of 17 of 75% of V in the form of VCl4 and/or VOCl3 was recovered by Cl2/air gas mixture at less than 600 ◦C. 1/7V2S3 + Cl2 = 2/7VCl4 (l,g) + 3/7SCl2 (50) 1/4V2S3 + 3/4O2 + Cl2 = 1/2VCl4 (l,g) + 3/4SO2 (51) 1/3V2S3 + 3/4O2 + Cl2 = 2/3VOCl3 (l,g) + SO2 (52) Vanadium sulfide in the spent catalyst is first oxidized to oxide at 300–500 ◦C. Vana- dium oxide was chlorinated by Cl2/N2, Cl2/O2, or Cl2/CO in the temperature range 300 ◦C to 600 ◦C. Finally, V was volatilized in the form of VCl4 or VOCl3 to achieve separation from other elements (Co, Ni). A total of 65% of V from oxidized V sulfide can be recovered by Cl2/N2 = 1 at 500 ◦C for 19 h. Meanwhile, V sulfide is directly chlorinated without roasting, and 80% of V can be recovered by Cl2/N2 = 1 at 500 ◦C for 0.5 h [76]. The affinity of metal to oxide is stronger than that of metal to sulfur. Under the same conditions, sulfides are easier to chlorinate than oxides. Thus, direct chlorination of vanadium sulfide is better than chlorination after oxidation of vanadium sulfide [77]. 4.6. Chlorination of V2O5 Mink et al. [78] reported that CCl4 reversibly dissociate and adsorbs on the two ex- posed vanadium atoms of the basic (001) plane of V2O5 before the chlorination reaction. The mechanism of chlorination of V2O5 by CCl4 was analyzed by MS and XPS. Before the formation of the volatile final product VOCl3, the surface vanadium atoms gradually acquire two chlorine atoms [79]. The kinetics of chlorination of V2O5 by CCl4 was inves- tigated by Jean et al. [80]. A total of 87% of V2O5 could be chlorinated by CCl4 at 480 ◦C in 30min. Chlorination reaction conforms to topochemical reaction model. According to analysis of kinetics results, the following mechanisms, Equations (53)–(58), at different temperatures, were proposed. a. 280–370 ◦C b. 410–515 ◦C V2O5 + 3CCl4 = 2VCl4 + 2CO2 + COCl2 + Cl2 (59) slow V2O5 + CCl4 → VOCl3 + VO2Cl + CO2 (53) f ast VO2Cl + CCl4 → VCl5 + CO2 (54) f ast VCl5 → VCl4 + 1/2Cl2 (55) f ast VOCl3 + CCl4 + 1/2Cl2 → VCl4 + COCl2 + Cl2 (56) f ast CCl4 → C+4Cl (57) slow V2O5 +C+4Cl → VOCl3 +VO2Cl+CO2 (58) The whole reaction can be expressed by the following Formula (59) Gaballah et al. [81] studied kinetics of chlorination of V2O5 with Cl2-CO-N2, Cl2-N2, and Cl2-air gas mixtures. Thermodynamic calculation showed that chlorinated product was mainly VOCl3 during the Cl2 chlorination of V2O5. However, VCl4 may be formed during the carbochlorination of vanadium pentoxide. The results of kinetics indicated that the rate-control step of V2O5 chlorination process between 500 ◦C and 570 ◦C with Cl2-N2 was a chemical reaction. Pore diffusion and chemical reaction were the limitingPDF Image | Extraction of the Rare Element Vanadium
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