无机盐工业
主管:中海油天津化工研究设计院有限公司
主办:中海油天津化工研究设计院有限公司
   中海油炼油化工科学研究院(北京)有限公司
   中国化工学会无机酸碱盐专业委员会
ISSN 1006-4990 CN 12-1069/TQ

无机盐工业 ›› 2024, Vol. 56 ›› Issue (6): 40-45.doi: 10.19964/j.issn.1006-4990.2023-0454

• 研究与开发 • 上一篇    下一篇

氟盐法净化锰电解液中镁离子的研究

鲁菊1,2(), 王家伟1,2,3, 王海峰1,2,3(), 裴正清1,2, 周兴杰1,2, 郑可欣1,2, 马德华1,2   

  1. 1.贵州大学材料与冶金学院,贵州 贵阳 550025
    2.贵州省冶金工程与过程节能重点实验室,贵州 贵阳 550025
    3.贵州省电池用锰材料工程技术研究中心,贵州 铜仁 554300
  • 收稿日期:2023-09-11 出版日期:2024-06-10 发布日期:2024-06-20
  • 通讯作者: 王海峰(1973— ),男,教授,主要从事锰系材料及资源综合利用方面的研究;E-mail:380889450@qq.com
  • 作者简介:鲁菊(1998— ),女,硕士,主要从事锰系材料方面的研究;E-mail:2642656692@qq.com
  • 基金资助:
    铜市科研(2021)13号项目(550025);黔科合重大专项[2022]003(550025);黔科合支撑[2022]重点020项目(554300)

Study on purification of magnesium from manganese electrolyte by fluorine salt method

LU Ju1,2(), WANG Jiawei1,2,3, WANG Haifeng1,2,3(), PEI Zhengqing1,2, ZHOU Xingjie1,2, ZHENG Kexin1,2, MA Dehua1,2   

  1. 1.College of materials and metallurgy,Guizhou University,Guiyang 550025
    2.Guizhou Key Laboratory of metallurgical engineering and process energy conservation,Guiyang 550025
    3.Engineering Technology and Research Center of Manganese Material for Battery,Tongren 554300
  • Received:2023-09-11 Published:2024-06-10 Online:2024-06-20

摘要:

采用电解法制备金属锰,因该工艺制备的金属锰纯度高、污染小而受到广泛应用,而生产过程中镁离子的循环富集会对系统造成很大危害。为降低镁离子的浓度保证电解生产正常进行,以镁离子的质量浓度降至15~20 g/L为研究目的,开展了氟盐法对锰电解液中镁离子的去除研究,考察了沉淀剂种类、用量系数、搅拌时间、温度和pH等因素对镁脱除效果的影响。研究结果表明,使用氟化铵为沉淀剂时,随着沉淀剂用量、搅拌时间、反应温度和体系pH的增加,镁离子浓度均呈现逐渐降低并达到一定水平后趋于稳定,得出较佳除杂条件:温度为50 ℃、搅拌时间为50 min、pH为5~6、沉淀剂用量为理论量(物质的量)的80%,可将溶液中镁离子质量浓度降至15.6 g/L,残余氟质量浓度为1.7 g/L。对除镁后的溶液采用低成本纳米除氟剂进行处理,通过利用EDS和ICP等分析手段可得到以下结果:氟离子质量浓度小于100 mg/L,除氟剂中的铝在硫酸锰溶液中的质量浓度仅为2.51×10-4 g/L,能满足电解锰工业的生产需求。

关键词: 硫酸锰, 氟盐法, 镁脱除率, 除氟剂

Abstract:

Metal manganese prepared by electrolysis is widely used because of its high purity and small pollution.The cyclic rich accumulation of magnesium ions in the production process will cause great harm to the system.In order to reduce the concentration of magnesium ions and ensure the normal production of electrolysis,the research objective was to reduce the mass concentration of magnesium ions to 15~20 g/L and the removal of magnesium from manganese electrolyte by fluorine salt method was carried out.The effects of precipitant type,dosage coefficient,stirring time,temperature and pH on the removal effect of magnesium were investigated.The results showed that when the ammonium fluoride was used as the precipitant,with the increase of precipitation agent,stirring time,the reaction temperature,and system pH,the concentration of magnesium ions was gradually decreased and reached a certain level,and the optimal conditions for impurity removal using ammonium fluoride as a precipitant were as follows:the temperature was 50 ℃,the stirring time was 50 min,the pH was 5~6,and the amount of precipitant was 80% of the theoretical amount,the concentration of magnesium ions in the solution could be reduced to 15.6 g/L,and the residual fluoride content was 1.7 g/L.The solution after magnesium removal was treated with low-cost nano-fluoride removal agent,and the following results could be obtained by using EDS and ICP analysis:the concentration of fluoride ion was reduced to less than 100 mg/L,and the content of aluminum in the fluoride removal agent in the manganese sulfate solution was only 2.51×10-4 g/L,which could meet the production demand of electrolytic manganese industry.

Key words: manganese sulfate, fluoride salt method, magnesium removal rate, fluoride remover

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