In-situ preparation of VS4 from vanadium-containing leaching solution of vanadium chromium slag
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摘要: 目前传统的提钒工艺仍以制备钢铁和化工行业的钒产品为主，为进一步促进钒产品深加工，提出含钒浸出液原位制备高附加值含钒材料VS4的新技术，该产品可用于储能和催化等领域。以钒铬渣为原料，分别以不同焙烧、浸出工艺所得含钒浸出液为钒源，硫代乙酰胺为硫源制备了VS4产品，并对其物相和微观形貌进行表征。结果表明，钒铬渣钠化焙烧水浸工艺和钙化焙烧碳酸钠浸出工艺所得含钒浸出液均可作为含钒母液原位转化VS4，但钠化焙烧水浸工艺由于焙烧过程中生成硅酸钠、铬酸钠等产物导致浸出液中含大量钠、硅、铬等杂质离子，所得VS4产品纯度较低。而钙化焙烧碳酸钠浸出工艺中由于钙盐对钒的选择性钙化效应，浸出过程钒铬分离效率很高，所得VS4产品纯度较高，且与分析纯偏钒酸钠为钒源制备的VS4具有相似的形貌。该工艺不仅实现了钒铬渣的增值利用，更显著缩短了含钒材料VS4的制备流程。Abstract: At present, the traditional vanadium extraction process is still based on the preparation of vanadium products for steel and chemical industries. In order to promote the deep processing of vanadium products, a new technology of in-situ preparation of high value-added material VS4 from vanadium leaching solution was proposed in this paper, which can be used in energy storage and catalysis fields. VS4 was prepared from vanadium chromium slag with different roasting and leaching processes as the vanadium source and thioacetamide as sulfur source. The results show that the leaching solution from sodium roasting-water leaching process and calcification roasting-sodium carbonate leaching process can be used as mother liquor for VS4 generation. However, due to the formation of sodium silicate, sodium chromate and other sodium salts in the sodium roasting process, the corresponding leaching solution contains a large amount of sodium, silicon, chromium and other impurities, resulting in low purity of VS4 products. Due to the selective calcification effect of calcium salt on vanadium, the separation efficiency of vanadium and chromium is very high in the process of calcium roasting and sodium carbonate leaching process. The purity of VS4 product is high, and it has similar morphology with VS4 prepared using sodium metavanadate as the vanadium source. The process not only realizes the value-added utilization of vanadium chromium slag, but also significantly shortens the preparation process of vanadium containing materials.
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Key words:
- vanadium chromium slag /
- VS4 /
- in-situ preparation /
- purity
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图 2 不同焙烧方式焙烧熟料的XRD图谱
Figure 2. XRD patterns of roasted samples under different roasting methods
图 3 不同提钒方式钒铬浸出率比较
Figure 3. Comparison of leaching rates of vanadium and chromium by different methods
图 4 偏钒酸钠为钒源所得VS4的XRD图谱（a）和VS4标准卡片（b）
Figure 4. XRD pattern of (a) VS4 with NaVO3 as vanadium source and (b) VS4 standard card
图 6 n(Na2CO3)/n(V2O3)为1条件下所得VS4的XRD图谱
Figure 6. XRD pattern of VS4 with n(Na2CO3)/n(V2O3) of 1
图 7 n(Na2CO3)/n(V2O3)为1条件下所得VS4的SEM形貌
Figure 7. SEM of VS4 with n(Na2CO3)/n(V2O3) of 1
图 8 n(Na2CO3)/n(V2O3)为3条件下所得VS4的XRD图谱
Figure 8. XRD pattern of VS4 with n(Na2CO3)/n(V2O3) of 3
图 9 n(Na2CO3)/n(V2O3)为3条件下所得VS4的SEM形貌
Figure 9. SEM of VS4 with n(Na2CO3)/n(V2O3) of 3
图 10 钙化焙烧碳酸钠浸出液为母液所得VS4的XRD谱
Figure 10. XRD pattern of VS4 obtained from Na2CO3 leaching liquid after CaO roasting
图 11 钙化焙烧碳酸钠浸出液为母液所得VS4的SEM形貌
Figure 11. SEM of VS4 obtained from Na2CO3 leaching liquid after CaO roasting
表 1 钒铬渣主要化学成分
Table 1. Chemical compositions of the vanadium-chromium slag %
FeO V2O3 Cr2O3 SiO2 TiO2 MnO CaO Total 39.21 11.88 9.45 15.73 11.19 7.03 1.67 96.16 
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