Research on vanadium extraction from vanadium-titanium iron concentrate pellets by gradient calcination roasting and sulfuric acid selective leaching
-
摘要: 以钒钛铁精矿为原料,氧化钙为添加剂,采用球团梯度钙化焙烧—硫酸浸出工艺进行选择性提钒,系统研究了梯度钙化焙烧制度和选择性浸出工艺参数对钙化球团钒和铁浸出率及球团强度的影响规律。梯度焙烧制度的研究结果表明,随着一次氧化温度提高和一次氧化时间的延长,钒的浸出率先升高后降低;提高二次氧化温度和延长二次氧化时间,钒的浸出率先升高后趋于平稳。选择性浸出试验结果表明,随着浸出时间的延长和液固质量比的提高,钒的浸出率先升高后趋于平稳;随着硫酸浓度升高,钒的浸出率先升高后降低。固定氧化钙配比为3%,优化的梯度焙烧制度为一次氧化温度和时间分别为850 ℃、90 min,二次氧化温度和时间为
1200 ℃、45 min,优化的浸出工艺参数为:浸出时间120 h、硫酸浓度2 mol/L、液固质量比7,在此条件下钒和铁的浸出率分别为79.86%和0.65%,浸出前后球团的抗压强度分别为1920.8 N/球和143.3 N/球。Abstract: Using vanadium-titanium magnetite concentrate as the raw material and calcium oxide as the additive, the selective extraction of vanadium was carried out by the process of gradient calcination roasting and sulfuric acid leaching. The influence laws of the gradient calcination roasting system and the selective leaching process parameters on the leaching rates of vanadium and iron from the calcined balls and the strength of the balls were systematically studied. The research results of the gradient calcination roasting system indicated that as the primary oxidation temperature increased and the primary oxidation time extended, the leaching rate of vanadium first increased and then decreased. Increasing the secondary oxidation temperature and extending the secondary oxidation time led to an increase in the leaching rate of vanadium first and then tended to be stable. The experimental results of the selective leaching showed that as the leaching time extended and the liquid-solid ratio increased, the leaching rate of vanadium first increased and then tended to be stable. As the sulfuric acid concentration increased, the leaching rate of vanadium first increased and then decreased. With a fixed calcium oxide ratio of 3%, the optimized gradient calcination system was a primary oxidation temperature and time of 850 ℃ and 90 min, a secondary oxidation temperature and time of1200 ℃ and 45 min. The optimized leaching process parameters were an leaching time of 120 h, a sulfuric acid concentration of 2 mol/L, and a liquid-solid ratio of 7. Under these aforementioned conditions, the leaching rates of vanadium and iron were 79.86% and 0.65%, respectively, and the compressive strengths of the balls before and after leaching were 1920.8 N/Pellet and 143.3 N/Pellet.-
Key words:
- vanadium-titanium iron concentrate /
- gradient roasting /
- selective leaching /
- sulfuric acid /
- vanadium
-
表 1 钒钛铁精矿的化学成分
Table 1. Chemical composition of vanadium-titanium magnetite concentrate
% TFe FeO TiO2 V2O5 Cr2O3 SiO2 CaO MgO Al2O3 P2O5 SO3 58.34 9.28 10.32 0.67 0.31 4.65 1.19 3.50 3.17 0.11 0.58 -
[1] LIU X. Study on calcification roasting of vanadium slag, vanadium speciation and element migration and transformation behavior[D]. Chongqing: Chongqing University, 2023. (刘羲. 钒渣钙化焙烧、钒形态及元素迁移转化行为的研究[D]. 重庆: 重庆大学, 2023.LIU X. Study on calcification roasting of vanadium slag, vanadium speciation and element migration and transformation behavior[D]. Chongqing: Chongqing University, 2023. [2] GAO Y Z. Vanadium resources and it’s supply and demand situation in China[J]. China Mining Magazine, 2019, 28(S2): 5-10. (高永璋. 中国钒矿资源及供需形势分析[J]. 中国矿业, 2019, 28(S2): 5-10.GAO Y Z. Vanadium resources and it’s supply and demand situation in China[J]. China Mining Magazine, 2019, 28(S2): 5-10. [3] XIE Y L. Effect of vanadium on alloying and its applications[J]. Special Steel Technology, 2015, 21(1): 1-5. (谢元林. 钒在钢中的合金化作用及应用[J]. 特钢技术, 2015, 21(1): 1-5.XIE Y L. Effect of vanadium on alloying and its applications[J]. Special Steel Technology, 2015, 21(1): 1-5. [4] XIN J J, WANG N, CHEN M, et al. Direct vanadium alloying of liquid steel with self‐reduction vanadium slag briquette[J]. Steel Research International, 2021, 93(6): 1-11. [5] ZHOU B J, LI L J, QI J, et al. Study on the application of vanadium[J]. Shanxi Metallurgy, 2022, 45(9): 58-59. (周冰晶, 李兰杰, 祁健, 等. 钒的应用研究[J]. 山西冶金, 2022, 45(9): 58-59.ZHOU B J, LI L J, QI J, et al. Study on the application of vanadium[J]. Shanxi Metallurgy, 2022, 45(9): 58-59. [6] YANG L L, TENG H B, ZHOU B J. Application of vanadium titanium new materials[J]. Shanxi Metallurgy, 2023, 46(1): 56-57. (杨丽丽, 滕海波, 周冰晶. 钒钛新材料的应用[J]. 山西冶金, 2023, 46(1): 56-57.YANG L L, TENG H B, ZHOU B J. Application of vanadium titanium new materials[J]. Shanxi Metallurgy, 2023, 46(1): 56-57. [7] MARIA S K, LIU Y C, MICHAEL K, et al. Vanadium electrolyte studies for the vanadium redox battery-a review[J]. Chem Sus Chem, 2016, 9(13): 1-24. [8] SHENG F J. Technologies and application of vanadium redox flow battery[J]. Guangdong Chemical Industry, 2018, 45(20): 107-108. (盛凤军. 全钒液流电池技术及其应用[J]. 广东化工, 2018, 45(20): 107-108.SHENG F J. Technologies and application of vanadium redox flow battery[J]. Guangdong Chemical Industry, 2018, 45(20): 107-108. [9] PENG H, ZHOU Q, LIU H P, et al. Research progress on vanadium extraction technologies from vanadium slag[J]. Acta Petrologica et Mineralogica, 2025, 44(1): 216-226. (彭浩, 周巧, 刘华平, 等. 钒渣提钒技术研究进展[J]. 岩石矿物学杂志, 2025, 44(1): 216-226. doi: 10.20086/j.cnki.yskw.2025.3161PENG H, ZHOU Q, LIU H P, et al. Research progress on vanadium extraction technologies from vanadium slag[J]. Acta Petrologica et Mineralogica, 2025, 44(1): 216-226. doi: 10.20086/j.cnki.yskw.2025.3161 [10] DU G C. Application and research progress of vanadium used in non-steel fields[J]. Iron Steel Vanadium Titanium, 2015, 36(2): 49-56. (杜光超. 钒在非钢铁领域应用的研究进展[J]. 钢铁钒钛, 2015, 36(2): 49-56.DU G C. Application and research progress of vanadium used in non-steel fields[J]. Iron Steel Vanadium Titanium, 2015, 36(2): 49-56. [11] FAN L, ZHANG W. Vanadium resources and its preparation technology[J]. Advanced Materials Industry, 2016(1): 41-46. (范亮, 张炜. 钒资源及其制备技术[J]. 新材料产业, 2016(1): 41-46. doi: 10.3969/j.issn.1008-892X.2016.01.010FAN L, ZHANG W. Vanadium resources and its preparation technology[J]. Advanced Materials Industry, 2016(1): 41-46. doi: 10.3969/j.issn.1008-892X.2016.01.010 [12] CHANG F Z, ZHAO B B, LI L J, et al. Research status and prospect of vanadium extraction from vanadium titano-magnetite[J]. Iron Steel Vanadium Titanium, 2018, 39(5): 71-78. (常福增, 赵备备, 李兰杰, 等. 钒钛磁铁矿提钒技术研究现状与展望[J]. 钢铁钒钛, 2018, 39(5): 71-78.CHANG F Z, ZHAO B B, LI L J, et al. Research status and prospect of vanadium extraction from vanadium titano-magnetite[J]. Iron Steel Vanadium Titanium, 2018, 39(5): 71-78. [13] WANG L. The study on direct extracting vanadium from vanadium-titanium magnetite concentrate[D]. Shenyang: Northeastern University, 2011. (王莉. 钒钛磁铁精矿直接提钒研究[D]. 沈阳: 东北大学, 2011.WANG L. The study on direct extracting vanadium from vanadium-titanium magnetite concentrate[D]. Shenyang: Northeastern University, 2011. [14] FU Z B. Research on extraction vanadium from stone coal by no salt roasting and acid leaching process[J]. China Nonferrous Metallurgy, 2011, 40(6): 29-33. (付自碧. 钒钛磁铁矿提钒工艺发展历程及趋势[J]. 中国有色冶金, 2011, 40(6): 29-33.FU Z B. Research on extraction vanadium from stone coal by no salt roasting and acid leaching process[J]. China Nonferrous Metallurgy, 2011, 40(6): 29-33. [15] GUO X, WANG L, ZHENG K H, et al. Research progress of extraction technology for vanadium from vanadium slags[J]. China Mining Magazine, 2016, 25(S1): 435-437. (郭昕, 王玲, 郑康豪, 等. 钒渣提钒工艺及研究进展[J]. 中国矿业, 2016, 25(S1): 435-437.GUO X, WANG L, ZHENG K H, et al. Research progress of extraction technology for vanadium from vanadium slags[J]. China Mining Magazine, 2016, 25(S1): 435-437. [16] ZHENG H Y, ZHANG W L, GOU Y C, et al. Transformation of vanadium-bearing titanomagnetite concentrate in additive-free roasting and alkaline-pressure leaching for extracting vanadium (V)[J]. Minerals, 2019, 9(3): 197. doi: 10.3390/min9030197 [17] ZHENG H Y, SUN Y, DONG Y, et al. Loss of vanadium and iron in calcified roasting and acid leaching of vanadium-bearing titanomagnetite[J]. CIESC Journal, 2015, 66(3): 1019-1025. (郑海燕, 孙瑜, 董越, 等. 钒钛磁铁矿钙化焙烧-酸浸提钒过程中钒铁元素的损失[J]. 化工报, 2015, 66(3): 1019-1025.ZHENG H Y, SUN Y, DONG Y, et al. Loss of vanadium and iron in calcified roasting and acid leaching of vanadium-bearing titanomagnetite[J]. CIESC Journal, 2015, 66(3): 1019-1025. [18] LUO Y, CHE X, CUI X, et al. Selective leaching of vanadium from V-Ti magnetite concentrates by pellet calcification roasting-H2SO4 leaching process[J]. International Journal of Mining Science and Technology, 2021, 31(3): 507-513. doi: 10.1016/j.ijmst.2021.02.002 [19] ZHENG Y, CHEN J L, CHEN S Z, et al. Effect of calcification roasting process on vanadium oxidation and extraction from vanadium titanomagnetite pellets via sulfuric acid Leaching: Mechanism and enhancement[J]. Separation and Purification Technology, 2025, 354: 128859. doi: 10.1016/j.seppur.2024.128859 [20] CAO Y F, ZHU X R, SUN Y S, et al. Non-isothermal oxidation kinetics of synthetic magnetite in air atmosphere[J]. Journal of Central South University (Science and Technology), 2024, 55(11): 4308-4317. (曹一斐, 祝昕冉, 孙永升, 等. 新生磁铁矿空气氧化非等温动力学研究[J]. 中南大学学报(自然科学版), 2024, 55(11): 4308-4317.CAO Y F, ZHU X R, SUN Y S, et al. Non-isothermal oxidation kinetics of synthetic magnetite in air atmosphere[J]. Journal of Central South University (Science and Technology), 2024, 55(11): 4308-4317. [21] GU Y Y, ZHUANG S X, ZHONG S A, et al. Non-pollution roasting technology to extracting vanadium form siliceous navajoite[J]. Chinese Journal of Rare Metals, 2007(1): 102-106. (古映莹, 庄树新, 钟世安, 等. 硅质岩钒矿中提取钒的无污染焙烧工艺研究[J]. 稀有金属, 2007(1): 102-106. doi: 10.3969/j.issn.0258-7076.2007.01.022GU Y Y, ZHUANG S X, ZHONG S A, et al. Non-pollution roasting technology to extracting vanadium form siliceous navajoite[J]. Chinese Journal of Rare Metals, 2007(1): 102-106. doi: 10.3969/j.issn.0258-7076.2007.01.022 [22] LIU Z Q. Study of reasonable oxidation degree and oxidation-induration kinetics of magnetite pellets[D]. Changsha: Central South University, 2023. (刘卓奇. 磁铁矿球团合理氧化程度及氧化-固结动力学研究[D]. 长沙: 中南大学, 2023.LIU Z Q. Study of reasonable oxidation degree and oxidation-induration kinetics of magnetite pellets[D]. Changsha: Central South University, 2023. [23] WANG B, LIU T, ZHANG Y M, et al. Effect of composite additives on roasting of stone coal for vanadium extraction[J]. Nonferrous Metals (Extractive Metallurgy), 2017(3): 31-35. (汪博, 刘涛, 张一敏, 等. 钙质复合添加剂对石煤提钒焙烧效果的影响[J]. 有色金属(冶炼部分), 2017(3): 31-35.WANG B, LIU T, ZHANG Y M, et al. Effect of composite additives on roasting of stone coal for vanadium extraction[J]. Nonferrous Metals (Extractive Metallurgy), 2017(3): 31-35. [24] YU L T, XIANG X R, JU J T, et al. Study on oxidizing roasting behavior of pellets produced with a certain vanadium-titanium magnetite, Hami, Xinjiang[J]. Sintering and Pelletizing, 2025, 50(6): 47-55. (鱼灵通, 项心如, 巨建涛, 等. 新疆哈密某钒钛磁铁矿球团氧化焙烧行为[J]. 烧结球团, 2025, 50(6): 47-55. doi: 10.13403/j.sjqt.2025.06.095YU L T, XIANG X R, JU J T, et al. Study on oxidizing roasting behavior of pellets produced with a certain vanadium-titanium magnetite, Hami, Xinjiang[J]. Sintering and Pelletizing, 2025, 50(6): 47-55. doi: 10.13403/j.sjqt.2025.06.095 [25] XIONG Y T. Experimental study on direct acid leaching of vanadium slag under atmospheric pressure[D]. Tangshan: North China University of Science and Technology, 2022. (熊雨婷. 钒渣常压直接酸浸试验研究[D]. 唐山: 华北理工大学, 2022.XIONG Y T. Experimental study on direct acid leaching of vanadium slag under atmospheric pressure[D]. Tangshan: North China University of Science and Technology, 2022. [26] WU E H, LI J, XU Z, et al. Extraction of vanadium from high-chromium vanadium-bearing titano magnetite pellets by oxidation roasting-HCl leaching process[J]. Iron Steel Vanadium Titanium, 2022, 43(6): 14-23. (吴恩辉, 李军, 徐众, 等. 高铬型钒钛铁精矿球团氧化焙烧-盐酸浸出提钒[J]. 钢铁钒钛, 2022, 43(6): 14-23. doi: 10.7513/j.issn.1004-7638.2022.06.003WU E H, LI J, XU Z, et al. Extraction of vanadium from high-chromium vanadium-bearing titano magnetite pellets by oxidation roasting-HCl leaching process[J]. Iron Steel Vanadium Titanium, 2022, 43(6): 14-23. doi: 10.7513/j.issn.1004-7638.2022.06.003 -
下载: