4.7 Article

Purification of crude selenium by vacuum distillation and analysis

Journal

JOURNAL OF MATERIALS RESEARCH AND TECHNOLOGY-JMR&T
Volume 9, Issue 3, Pages 2926-2933

Publisher

ELSEVIER
DOI: 10.1016/j.jmrt.2020.01.043

Keywords

Selenium; Purification; Vacuum distillation; Impurity occurrence; Evaporation rate

Funding

  1. Basic Research Key Project of Yunnan Province [2019FA020]
  2. Fund of the National Natural Science Foundation of China [U1902221]
  3. Scientist Studio of Yunnan Province
  4. Science and Technology Planning Project of Yunnan Province [2017FB082]
  5. State Key Laboratory of Complex Non ferrous Metal Resources Clean Utilization, Kunming University of Science and Technology [CNMRCUTS1605]
  6. construction of high-level talents of Kunming University of Science and Technology [20180050]

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In this study, metallurgical grade crude selenium (99.4%), comprehensively recovered from copper electrolysis anode slime, was purified to 99.992% through triple consecutive vacuum distillation (TCVD) on a laboratory scale. The actual evaporation rate and accommodation coefficient alpha of crude selenium were found to be 0.0231 g cm(-2) min and 0.3236, respectively, at 523 K and approximately 4 Pa by a vacuum thermogravimetric furnace. Internal heat vac- uum distillation equipment was employed in the purification experiments with a dynamic vacuum level of approximately 4 Pa. Detailed analysis of the initial and purified selenium was performed using inductively coupled plasma mass spectrometry (ICP-MS) to identify the 15 most common impurity elements. The analysis confirmed the reduction in the total impurity content from 2997.38 ppmw to <79.08 ppmw. The microscopic impurity elemental distribution was analyzed using an electron probe microanalyzer (EPMA), and it shows that the impurities were relatively concentrated and gathered in crude selenium. The results enrich the database of selenium evaporation kinetics and lay a foundation for the industrial purification of selenium. (C) 2020 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

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