Study on the selective separation of gallium and iron from vanadium converter sludge
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摘要: 采用酸浸法对冶炼流程中的提钒转炉污泥进行了镓的浸出试验，考察了镓在提钒转炉污泥中的赋存状态及多种因素对镓浸出率的影响，包括酸浓度、液固比、反应温度、反应时间和搅拌速率等。结果表明，镓离子主要赋存在氧化铁的晶格中，盐酸可作为有效浸出试剂破坏氧化铁的晶格，在盐酸浓度为5 mol/L，反应时间1 h，反应温度60 °C，液固比为5：1时镓的浸出率为90%。利用元素沉淀pH值的差异可有效分离镓和铁，进而得到富镓料，与提钒转炉污泥对比，富镓料中的镓富集24倍。该研究成果有望为实现钒钛磁铁矿中高附加值关键金属的提取提供技术支撑。Abstract: In this study, the leaching test of gallium from the vanadium extraction converter sludge in the smelting process was conducted using the acid leaching method. The occurrence state of gallium in the vanadium extraction converter sludge and the influence of various factors on the leaching rate of gallium were investigated, including acid concentration, liquid-solid ratio, reaction temperature, reaction time and stirring rate, etc. The results showed that gallium ions were mainly present in the lattice of iron oxide. Hydrochloric acid could be used as an effective leaching agent to break the lattice of iron oxide. Under a specific condition with the hydrochloric acid concentration of 5 mol/L, the reaction time of 1 h, the reaction temperature of 60 °C, and the liquid-solid ratio of 5:1, the leaching rate of gallium was 90%. The difference in pH values of elements can effectively separate gallium and iron, and thereby obtain a gallium-rich material. The gallium enrichment in the gallium-rich material was 24 times as high as the vanadium extraction converter sludge. This research result is expected to provide technical support for the extraction of high-value-added key metals from vanadium-titanium magnetite.
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Key words:
- vanadium extraction converter sludge /
- gallium /
- acid leaching /
- separation
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图 1 提钒转炉污泥的外观形貌(黑色细粉)
Figure 1. Appearance of vanadium extraction converter sludge (black fine powder)
图 2 提钒转炉污泥Fe、Ga分离工艺设计
Figure 2. Process of Fe and Ga separation from vanadium extraction converter sludge
图 4 提钒转炉污泥SEM 背闪射图像和主要元素能谱分布图
Figure 4. Backscattered SEM image of vanadium extraction converter sludge and EDS mapping of the distribution of the main elements
图 5 盐酸浓度对提钒转炉污泥中镓和铁浸出率的影响
Figure 5. Effect of HCl concentration on the Ga and Fe leaching efficiency from vanadium extraction converter sludge
图 6 液固比对提钒转炉污泥中镓和铁浸出率的影响
Figure 6. Effect of liquid/solid ratio on the Ga and Fe leaching efficiency from vanadium extraction converter sludge
图 7 浸出温度对提钒转炉污泥中镓和铁浸出率的影响
Figure 7. Effect of temperature on the Ga and Fe leaching efficiency from vanadium extraction converter sludge
图 8 搅拌时间对提钒转炉污泥中镓和铁浸出率的影响
Figure 8. Effect of agitating time on the Ga and Fe leaching efficiency from vanadium extraction converter sludge
图 9 搅拌速率对提钒转炉污泥中镓和铁浸出率的影响
Figure 9. Effect of agitating rate on the Ga and Fe leaching efficiency from vanadium extraction converter sludge
图 10 镓和铁元素在 pH值为0～14范围内存在形式
(a)Fe3+水解分布；(b) Ga3+水解分布；(c) Fe2+水解分布
Figure 10. Existing states of gallium and iron in the pH range of 0~14
图 11 不同pH条件下镓和铁的沉淀率
Figure 11. Ga and Fe recoveries at different pH during precipitation
表 1 提钒转炉污泥成分分析结果
Table 1. Result of XRF analysis of vanadium extraction converter sludge
% Al Cr Ca Fe Mg Mn Ni P Pb Si Ti V Zn Ga* O 0.2 0.1 0.2 64.2 0.1 0.3 0.3 0.1 0.5 0.6 0.1 0.1 3.0 0.03 Bal. 注：*该元素含量为ICP检测结果。 
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表 2 提钒转炉污泥电子探针物相定量结果
Table 2. EPMA result of vanadium extraction converter sludge
% 物相 SiO2 Fe3O4 ZnO Ga 含硅物相 98.5 1.3 0.017 4 含铁物相 0.7 96.2 1.3 0.057 8
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表 3 富镓料成分分析结果
Table 3. XRF analysis result of Ga-rich material
% Al Cr Ca Fe Mn Ni P Pb Si Ti V Zn Ga O 0.73 0.82 0.04 51.25 0.06 0.03 1.37 2.26 0.07 0.91 2.22 2.03 0.73 Bal.
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