Ural Federal University named after the first President of Russia B. N. Yeltsin, Yekaterinburg, Russia:

S. S. Naboychenko, Professor-Consultant, Department of Metallurgy of Non-Ferrous Metals, Institute of New Materials and Technologies, Doctor of Technical Sciences
A. A. Korolev, Сhief Engineer

JSC “Uralelectromed”, Verkhnyaya Pyshma, Russia:

G. I. Maltsev, Chief Specialist of the Research Centre, Doctor of Technical Sciences, e-mail: mgi@elem.ru
K. L. Timofeev, Head of the Research Centre, Candidate of Technical Sciences, e-mail: K.Timofeev@elem.ru

Analysis of modern technological processes in the production of lead, antimony and tin showed that compared with the common methods of separation and refining of base metals from the impurity elements, vacuum distillation of polymetallic alloys and related industrial products of lead production is technologically acceptable and economically feasible, which allows to obtain saleable, including monoelement products of the required composition. The objects of research were model alloys: model double alloys Pb – Sb, Pb – Sn, Sb – Sn; triple model alloys Sb – Pb – Sn; as well as by-products of the existing production of lead manufature — a real lead-tin alloy; decopperised rough lead. In addition to experimental data on the determination of melting temperature at constant pressure and melting pressure at constant temperature in the system, metal alloys of different nature and composition the calculation method based on the basic equations of the volume model of molecular interaction (MIVM) for the construction of equilibrium phase diagrams (VLE) “liquid – gas” in the coordinates "temperature –alloy composition" and "pressure – alloy composition" to predict the composition of the products of sublimation of double and triple alloys containing lead, antimony, tin were used. Preliminary analysis of the calculated systems of double and triple alloys allows to minimize the number of basic experiments, greatly simplifies the process of finding the optimal parameters of vacuum distillation of polymetallic materials. For processing tin industrial products of oxidative refining of lead with a tin content of 20–30%, a technology based on their step reduction melting on Pb – Sn – Sb alloy (50–60% Sn) and vacuum distillation with the formation of rough tin (94–98% Sn), suitable for further processing by known methods, is proposed. To produce rough tin (≥90% Sn), pilot tests were carried out, as a result of which the principal possibility and reasonability of using vacuum distillation were confirmed. The results of tests on vacuum distillation of 100 kg of Pb – Sn – Sb-alloy composition in the JSC ‘Uralelectromed” showed that the recovery of tin in the distillation residue for the best experiments is more than 99% with tin content up to 97%. In total 50 kg of tin of rough composition were received; As-condensate; Sb – Pb-condensate. Economic efficiency of processing of lead-containing raw materials with the use of vacuum distillation, calculated for Pb – Sn – Sb-alloy due to the production of a purer and therefore expensive product.

1. Smirnov M. P. Refining of lead and processing intermediates. Moscow : Metallurgiya, 1977. 280 р.
2. Smirnov M. P., Vinogradov S. V. Achievements and prospects in the field of lead refining. Tsvetnye Metally. 1986. No. 9. pp. 38–43.
3. Utkin N. I. Production of non-ferrous metals. Moscow : Intermet Inzhiniring, 2000. 442 p.
4. Marchenko N. I. Metallurgy of heavy non-ferrous metals. Krasnoyarsk : Sibirskiy Federalniy Universitet, 2009. 394 p.
5. Orlov A. K. Мetallurgy of lead and zinc. Saint Petersburg : Sankt-Petersburgskiy Gosudarstvennyy Gornyy Institut (Technicheskiy Universitet), 2004. 71 p.
6. Erez B.-Y., Yitzhak V., Brink E. C. M., Ron B. A new Ghassulian metallurgical assemblage from Bet Shemesh (Israel) and the earliest leaded copper in the Levant. Journal of Archaeological Science: Reports. 2016. Vol. 9. pp. 493–504.
7. Yin N.-H., Sivry Y., Avril C. Bioweathering of lead blast furnace metallurgical slags by Pseudomonas aeruginosa. International Biodeterioration & Biodegradation. 2014. Vol. 86. Part C. pp. 372–381.
8. Capannesi G., Rosada A., Avino P. Elemental characterization of impurities at trace and ultra-trace levels in metallurgical lead samples by INAA. Microchemical Journal. 2009. Vol. 93, No. 2. pp. 188–194.
9. Sun B., Yang C., Gui W. A discussion of the control of nonferrous metallurgical processes. IFAC-Papers On Line. 2015. Vol. 48, No. 17. pp. 80–85.
10. Yin N.-H., Sivry Y., Benedetti M. F. Application of Zn isotopes in environmental impact assessment of Zn – Pb metallurgical industries: A mini review. Applied Geochemistry. 2016. Vol. 64. pp. 128–135.
11. Lovchikov V. S. Alkaline refining of lead. Moscow : Metallurgiya, 1961. 150 p.
12. Jamali-Zghal N., Lacarrière B., Le Corre O. Metallurgical recycling processes: Sustainability ratios and environmental performance assessment. Resources, Conservation and Recycling. 2015. Vol. 97. pp. 66–75.
13. Liu C., Qiu K. Separating lead–antimony alloy by fractional crystallization using directional lifting process. Journal of Alloys and Compounds. 2015. Vol. 636. pp. 282–287.

14. Ellis T.W., Mirza A.H. The refining of secondary lead for use in advanced lead-acid batteries. Journal of Power Sources. 2010. Vol. 195, No. 14. pp. 4525–4529.
15. Liu T., Qiu K. Removing antimony from waste lead storage batteries alloy by vacuum displacement reaction technology. Journal of Hazardous Materials. 2018. Vol. 347. pp. 334–340.
16. Dyakov V. E. Development and testing of vacuum apparatus for separation of lead-tin alloy waste. International research journal. 2016. No. 3, Part 2. pp. 11–14.
17. Nan C., Yang H. W., Yang B. Experimental and modeling vapor-liquid equilibria: Separation of Bi from Sn by vacuum distillation. Vacuum. 2017. Vol. 135. pp. 109–114.
18. Kemenov, V. N., Nesterov S. B. Vacuum technique and technology: proc. the manual for high schools. Moscow : Publishing house of MEI, 2002. 84 p.
19. Ivanov V. E., Papirov I. I., Tikhinsky G. F. Pure and ultrapure metals (Obtained by distillation in vacuum). Moscow : Metallurgiya, 1965. 263 p.
20. Vacuum metallurgy. Edited by A. M. Samarin. Moscow : State scientific and technical publishing house of literature on ferrous and nonferrous metallurgy, 1962. 517 p.
21. Korolev A. A., Krayukhin S. A., Maltsev G. I. Gas–liquid Equilibrium systems for Sn – Sb alloy at vacuum distillation. Zhurnal Sibirskogo federalnogo universiteta. Seriya “Tekhnika I Tekhnologii”. 2019. No. 4. pp. 488–503.
22. Korolev A. A., Krayukhin S. A., Maltsev G. I. Phase equilibria in the Pb – Sn system at pyrometallurgical sublimation. Vestnik MGTU im. N. Eh. Bauman. Seriya Mashinostroenie. 2019. No. 1. pp. 51–70.
23. Korolev A. A. Krayukhin S. A., Maltsev G. I. Equilibrium systems “gas–liquid” for the alloy Pb – Sb vacuum distillation. Vestnik PNIPU. Mashinostroenie, materialovedenie. 2017. Vol. 19, No. 3. pp. 75–99.
24. Korolev A. A. Krayukhin S. A., Maltsev G. I. Phase equilibrium for Pb – Sb – Sn alloy with vacuum distillation. Vestnik SamGTU. Seriya “Tekhnicheskie nauki”. 2018. No. 1. pp. 128–141.