Preparation of 4N5 High Purity Manganese by One-step Vacuum Distillation
SUN Yuanjun1, ZHAO Yongzhe2, YANG Shuangping2,*, DING Xiangdong1, SUN Jun1
1 College of Materials Science and Engineering, Xi’an Jiaotong University, Xi’an 710049, China 2 College of Metallurgical Engineering, Xi’an University of Architecture and Technology, Xi’an 710055, China
Abstract: With the development of high-tech fields, high purification of metal manganese has become an inevitable trend in the development of the industry. In this study, using electrolytic manganese as raw material, through self-developed high-efficiency distillation furnace, the high-purity manganese with a purity of more than 4N5 was prepared in one step combined with partition condensation, the length of the main metal condensation zone was extended by setting a constant temperature condensation section in the condensation zone to achieve the purpose of improving the metal yield. The theory of vacuum distillation of electrolytic manganese was analyzed, and the effects of different distillation temperatures and times on the volatilization rate and the temperature of the constant temperature condensation section (condensation temperature) on the metal yield were studied. At the same time, the impurity content in the condensed manganese at different distillation temperatures was detected by inductively coupled plasma mass spectrometry (ICP-MS). The results show that the main metal Mn is easy to separate from the impurity metal at the selected distillation temperature, but the higher the temperature, the weaker the separation ability. With the increase of distillation temperature and holding time, the volatilization rate increases. Setting the main metal constant temperature condensation section can greatly improve the me-tal yield, with the increase of condensation temperature, the metal yield increases first and then decreases. With the increase of distillation temperature, the contents of Cd, K, Na, and Zn in condensed manganese are almost unchanged, while the contents of Mg, Ca, Pb, Cu, Cr, Ni, Fe, and Co increased with the increase of distillation temperature. Considering comprehensively, high-purity manganese with the purity of 4N5 can be obtained under a system pressure of 10-3—10-2 Pa, a condensation temperature of 1 100 ℃, a holding time of 90 min, and a distillation temperature of 1 400 ℃. In this instance, the volatilization rate is 86.94%, and the yield can reach 94.32%.
1 Guan C, He J J, Zeng H, et al. Chinese Journal of Rare Metals, 2017, 41(2), 120 (in Chinese). 关冲, 何金江, 曾浩, 等. 稀有金属, 2017, 41(2), 120. 2 Lee J H, Black R, Popov G, et al. Energy & Environmental Science:EES, 2012, 5(11), 9558. 3 Du J, Liu X B, Liu Z H, et al. China’s Manganese Industry, 2008(2), 15 (in Chinese). 杜军, 刘晓波, 刘作华, 等. 中国锰业, 2008(2), 15. 4 Jin X Z, Yang Z P, Cheng Z B, et al. China’s Manganese Industry, 2006(1), 28 (in Chinese). 靳晓珠, 杨仲平, 陈祝炳, 等. 中国锰业, 2006(1), 28. 5 Liu B, Zhang Y, Lu M, et al. Minerals Engineering, 2019, 131, 286. 6 Dai E B. China’s Manganese Industry, 2001(2), 9 (in Chinese). 戴恩斌. 中国锰业, 2001(2), 9. 7 Chen Q, Yao Y, Li X, et al. Journal of Water Process Engineering, 2018, 26, 289. 8 Zhang W, Cheng C. Hydrometallurgy, 2007, 89, 160. 9 Goher M E, Hassan A M, Moniem I A A, et al. Egyptian Journal of Aquatic Research, 2015, 41(2), 155. 10 Khobragade M U, Pal A. Journal of Environmental Chemical Engineering, 2014, 2(4), 2295. 11 Budinova T, Savova D, B. Tsyntsarski, et al. Applied Surface Science, 2008, 255(8), 4650. 12 Albuquerque C F, Luna-Finkler C L, Rufino R D, et al. International Review of Chemical Engineering Rapid Communicati, 2012, 4(2), 156. 13 Masindi V, Osman M S, Shingwenyana R. Journal of Environmental Chemical Engineering, 2019, 7(3), 103082. 14 Kononova O N, Bryuzgina G L, Apchitaeva O V, et al. Arabian Journal of Chemistry, 2019, 12(8), 2713. 15 Zhao J, Cao J R, Wang W H, et al. Technology of Water Treatment, 2020, 46(5), 55 (in Chinese). 赵瑾, 曹军瑞, 王文华, 等. 水处理技术, 2020, 46(5), 55. 16 Yuan T, Xiaopan Z, Tao Q, et al. Materials Research Express, 2021, 8(5), 056506. 17 Li Q, Hu Z F, Li Z Q, et al. Nonferrous Metals, 2014, 4(6), 21 (in Chinese). 李卿, 胡志方, 李忠岐, 等. 有色金属工程, 2014, 4(6), 21. 18 Dong L, Yang T, Bin Y, et al. Vacuum, 2021, 192, 110464. 19 Wang L, Liu D C, Yang B, et al. Chinese Journal of Vacuum Science and Technology, 2010, 30(3), 283 (in Chinese). 王林, 刘大春, 杨斌, 等. 真空科学与技术学报, 2010, 30(3), 283. 20 Liu D C, Yang B, Wang F, et al. Physics Procedia, 2012, 32, 363. 21 Prasad D S, Munirathnam N R, Rao J V, et al. Materials Letters, 2005, 59(16), 2035. 22 Ali S T, Prasad D S, Munirathnam N R, et al. Separation and Purification Technology, 2004, 43(3), 263. 23 Cheng Z Y, Long J P, Yang W Y, et al. Guangzhou Chemical Industry, 2021, 49(5), 54 (in Chinese). 程籽毅, 龙剑平, 杨武勇, 等. 广州化工, 2021, 49(5), 54. 24 Ali S T, Rao J V, Varma K S, et al. Bulletin of Materials Science, 2002, 25(6), 479. 25 Ali S T, Munirathnam N R, Sudheer C, et al. Materials Letters, 2003, 58(10), 1638. 26 TanH L, Xiong H, Yang B, et al. Chinese Journal of Rare Metals, 2016, 40(5), 515 (in Chinese). 闫华龙, 熊恒, 杨斌, 等. 稀有金属, 2016, 40(5), 515. 27 Xu Z P, Jia L L, He Z Q, et al. Transactions of Nonferrous Metals Society of China, 2024, 34(5), 1634. 28 姚力军, 郭廷宏, 潘杰, 等. 中国专利, CN202111161334. 3, 2022.
渝公网安备50019002502923号 版权所有：《材料导报》编辑部
2025, Vol. 39 
