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硫酸锰溶液溶剂萃取分离氟及其循环利用研究

Study on Separation and Recycling of Fluorine by Solvent Extraction from Manganese Sulfate Solution

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【作者】 谢渝张贵清李青刚曹佐英关文娟巫圣喜王明玉

【Author】 XIE Yu;ZHANG Gui-qing;LI Qing-gang;CAO Zuo-ying;GUAN Wen-juan;WU Sheng-xi;WANG Ming-yu;School of Metallurgy and Environment, Central South University;

【通讯作者】 巫圣喜;

【机构】 中南大学冶金与环境学院

【摘要】 氟盐沉淀法除钙、镁是制备高纯硫酸锰溶液最普遍的方法,但引入的氟需进一步去除。针对含氟硫酸锰溶液,本文提出溶剂萃取法分离回收氟的新技术,主要包含溶剂萃取分离氟、氧化锰循环反萃氟两个过程。在硫酸锰溶液初始pH为1.9,有机相组成为60%TBP+40%磺化煤油,相比为2∶1,萃取时间3 min的条件下,经过室温五级逆流萃取,硫酸锰溶液中的氟可以降至35 mg/L以下;在氧化锰添加量为理论量的1.0倍,相比5∶1,反萃时间1 h,反应温度298 K的最佳反萃条件下,氧化锰循环反萃率可达98.08%以上,反萃过程析出的氟化锰可以返回用于硫酸锰溶液除钙、镁。相较于现有氟反萃工艺,新技术可在深度除氟的同时实现氟的循环利用。

【Abstract】 Removing calcium and magnesium by fluorine precipitation is the most common method to prepare high-purity manganese sulfate solution.However, the introduced fluorine needs a further removal.In this paper, a new technology is proposed to separate and recover fluorine from fluorine-containing manganese sulfate solution, mainly including the two processes of solvent extraction for fluorine and cyclic stripping of fluorine with manganese oxide.Under such conditions, including initial pH of 1.9 for manganese sulfate solution, organic phase composition of 60% TBP + 40% sulfonated kerosene, O/A ratio of 2∶1,and extraction time of 3 min, the concentration of fluorine in manganese sulfate solution can be reduced to below 35 mg/L after a five-stage countercurrent extraction at room temperature.And under the optimal stripping conditions of manganese oxide addition of 1.0 times the theoretical amount, O/A ratio of 5∶1,stripping time of 1 h, and temperature of 298 K,the cyclic stripping efficiency of manganese oxide reaches above 98.08%,and the manganese fluoride precipitated in the stripping process can be used for the removal of calcium and magnesium in manganese sulfate solution in return.Compared with the existing fluorine stripping process, this new technology can realize the recycling of fluorine while removing fluorine in depth.

【基金】 湖南省自然科学基金项目(2020JJ4728)
  • 【文献出处】 稀有金属与硬质合金 ,Rare Metals and Cemented Carbides , 编辑部邮箱 ,2023年06期
  • 【分类号】O658.2
  • 【下载频次】48
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