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Recovery of rare earths, lithium and fluorine from rare earth molten salt electrolytic slag via fluoride sulfate conversion and mineral phase reconstruction
Minerals Engineering ( IF 4.8 ) Pub Date : 2021-06-18 , DOI: 10.1016/j.mineng.2021.106965
Lei Tian , Lijie Chen , Ao Gong , Xuangao Wu , Caifang Cao , Zhifeng Xu

To solve the problem of rare earths (RE) lithium (Li) and fluorine (F) recovery in rare earth molten salt electrolysis slag, a recovery method was developed based on magnetic separation, sulfuric acid leaching, HF recycling, water leaching, fluorination precipitation. First, RE, Li and iron-containing phases in a slag sample were separated using a magnetic separation method. Second, sulfuric acid-leaching was used to reconstruct the phases of RE and Li in the non-magnetic fraction, which were transformed into a rare earth sulfate easily dissolved in water. At the same time, the HF generated in the sulfuric acid leaching process is recovered by multistage adsorption. Finally, qualified fluoride rare earth products were obtained by HF cycle precipitation. The results show that the recovery of iron is 85.30% under the condition that the magnetic separation intensity of 0.668 T, particle size of 58–75 μm, and the main phase in the non-magnetic fraction is the rare earth phase, and the iron content is only 2.90%. Under the conditions of a concentrated acid concentration of 98.00%, a temperature of 633 K, a liquid–solid ratio of 2:1, a particle size of 58–75 μm, a constant stirring speed of 300 r·min−1, and reaction time of 3 h, the removal rate of F is 95.30%, and the transformation rates of Nd, Pr, Dy, and Li reached more than 95.00%. Through water immersion and fluorination precipitation, rare earth fluoride products can be obtained. The purity, particle size, and water content of the products met the standards required for industrial rare earth molten salt electrolysis.



中文翻译:

氟化物硫酸盐转化和矿相重构从稀土熔盐电解渣中回收稀土、锂和氟

针对稀土熔盐电解渣中稀土(RE)、锂(Li)、氟(F)的回收问题,开发了基于磁选、硫酸浸出、HF回收、水浸出、氟化沉淀的回收方法. 首先,使用磁分离方法分离渣样中的稀土、锂和含铁相。其次,硫酸浸出用于重建非磁性部分中稀土和锂的相,将其转化为易溶于水的稀土硫酸盐。同时,硫酸浸出过程中产生的HF通过多级吸附回收。最后通过HF循环沉淀得到合格的氟化稀土产品。结果表明,铁的回收率为85。在磁选强度为0.668 T,粒径为58-75 μm,非磁性部分中的主要相为稀土相,铁含量仅为2.90%的条件下,30%。在浓酸浓度98.00%、温度633 K、液固比2:1、粒径58-75 μm、恒速搅拌300 r·min条件下-1,反应时间3 h,F去除率为95.30%,Nd、Pr、Dy和Li的转化率达到95.00%以上。通过水浸和氟化沉淀,可以得到稀土氟化物产品。产品的纯度、粒度、含水量均符合工业稀土熔盐电解要求的标准。

更新日期:2021-06-18
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