D0L:10.13374.issn1001-053x.2013.10.011 第35卷第10期 北京科技大学学报 Vol.35 No.10 2013年10月 Journal of University of Science and Technology Beijing 0ct.2013 机械活化强化铌钽矿碱性水热体系浸出 孙青1,2)，汪加军)，王晓辉2)凶，杨秀丽)，郑诗礼2)，谢华1)，郑水林) 1)中国矿业大学（北京）化学与环境工程学院，北京100083 2)中国科学院过程工程研究所湿法治金清洁生产技术国家工程实验室，绿色过程与工程院重点实验室，北京100190 3)昆明理工大学治金与能源工程学院，昆明650093 ☒通信作者，E-mail:wangxh@home.ipe.ac.cm 摘要针对现行铌钽矿HF酸处理工艺氟污染严重的问题，提出以KOH溶液替代高毒性HF介质的铌钽矿碱性水热 体系浸出新方法，研究了铌钽矿在KOH碱性水热体系浸出规律.结果表明，在KOH质量分数50%范围内，KOH质量 分数和反应温度的提高会促进铌钽矿分解生成可溶性六铌（钽）酸钾，但过高的KOH质量分数和反应温度会使可溶性 六铌（钽）酸钾向不溶性偏铌（钽）酸钾转化，造成铌、钽浸出率的下降.在KOH质量分数35%、反应温度200℃、碱矿 质量比4：1以及反应时间2h的最佳浸出条件下，铌和钽浸出率仅为18.73%和9.4%：通过机械活化对铌钽矿进行预处 理后，铌和钽浸出率可大幅度提高至95%和60%，说明机械活化可显著强化铌钽矿碱性水热浸出过程.铌钽矿经机械活 化后，矿物粒度减小，比表面积增加，晶格畸变增大，无定形化程度增加，内部缺陷程度增加，矿物的反应活性大大增 加，铌钽矿的浸出率显著提高. 关键词铌矿处理：钽矿处理：机械活化：氢氧化钾：浸出 分类号TF111:TF841.6 Leaching of mechanically activated niobium-tantalum ore in an alkaline hydrothermal system SUN Qing2),WANG Jia-jun),WANG Xiao-hu),YANG Xiu-1),ZHENG Shi-Li),XIE Hua), ZHENG Shui-lin) 1)School of Chemical and Environment Engineering,China University of Mining and Technology(Beijing),Beijing 100083,China 2)National Engineering Laboratory for Hydrometallurgical Cleaner Production Technology,Key Laboratory of Green Process and Engineering,Institute of Process Engineering,Chinese Academy of Science,Beijing 100190,China 3)Faculty of Metallurgical and Energy Engineering,Kunming University of Science and Technology,Kunming 650093,China Corresponding author,E-mail:wangxh@home.ipe.ac.cn ABSTRACT Aiming at serious fluorine pollution problems in current hydrofluoric acid treatment processes of niobium-tantalum ore,a new leaching process of niobium-tantalum ore with an alkaline hydrothermal system was pro- posed that KOH solution was used as a reaction medium to substitute highly toxic HF solution.The reaction rules of niobium-tantalum ore in the alkaline hydrothermal system were investigated.It is found that decomposition of niobium- tantalum ore into soluble potassium hexa-niobate (tantalate)is promoted by increasing the KOH mass fraction and reaction temperature when the KOH mass fraction range is less than 50%,but soluble potassium hexa-niobate(tan- talate)will change to insoluble potassium niobate (tantalate)when the KOH mass fraction and reaction temperature are too high,then the leaching rates of niobium and tantalum decrease.The leaching rates of niobium and tantalum are merely 18.73%and 9.4%respectively under optimum leaching conditions that the KOH mass fraction is 35%,the reaction temperature is 200 C,the KOH-to-ore mass ratio is 4:1 and the reaction time is 2 h,but they will increase 收稿日期：2012-08-25 基金项目：因家自然科学基金青年基金资助项目(51004094)：国家高技术研究发展计划资助项目(2009AA06Z103)第 35 卷 第 10 期 北 京 科 技 大 学 学 报 Vol. 35 No. 10 2013 年 10 月 Journal of University of Science and Technology Beijing Oct. 2013 机械活化强化铌钽矿碱性水热体系浸出 孙 青1,2)，汪加军1)，王晓辉2) ，杨秀丽3)，郑诗礼2)，谢 华1)，郑水林1) 1) 中国矿业大学 (北京) 化学与环境工程学院，北京 100083 2) 中国科学院过程工程研究所湿法冶金清洁生产技术国家工程实验室，绿色过程与工程院重点实验室，北京 100190 3) 昆明理工大学冶金与能源工程学院，昆明 650093 通信作者，E-mail: wangxh@home.ipe.ac.cn 摘 要 针对现行铌钽矿 HF 酸处理工艺氟污染严重的问题，提出以 KOH 溶液替代高毒性 HF 介质的铌钽矿碱性水热 体系浸出新方法，研究了铌钽矿在 KOH 碱性水热体系浸出规律. 结果表明，在 KOH 质量分数 50%范围内，KOH 质量 分数和反应温度的提高会促进铌钽矿分解生成可溶性六铌 (钽) 酸钾，但过高的 KOH 质量分数和反应温度会使可溶性 六铌 (钽) 酸钾向不溶性偏铌 (钽) 酸钾转化，造成铌、钽浸出率的下降. 在 KOH 质量分数 35%、反应温度 200 ℃、碱矿 质量比 4:1 以及反应时间 2 h 的最佳浸出条件下，铌和钽浸出率仅为 18.73%和 9.4%；通过机械活化对铌钽矿进行预处 理后，铌和钽浸出率可大幅度提高至 95%和 60%，说明机械活化可显著强化铌钽矿碱性水热浸出过程. 铌钽矿经机械活 化后，矿物粒度减小，比表面积增加，晶格畸变增大，无定形化程度增加，内部缺陷程度增加，矿物的反应活性大大增 加，铌钽矿的浸出率显著提高. 关键词 铌矿处理；钽矿处理；机械活化；氢氧化钾；浸出 分类号 TF111；TF841.6 Leaching of mechanically activated niobium-tantalum ore in an alkaline hydrothermal system SUN Qing1,2), WANG Jia-jun1), WANG Xiao-hui2) , YANG Xiu-li3), ZHENG Shi-li2), XIE Hua1) , ZHENG Shui-lin1) 1) School of Chemical and Environment Engineering, China University of Mining and Technology (Beijing), Beijing 100083, China 2) National Engineering Laboratory for Hydrometallurgical Cleaner Production Technology, Key Laboratory of Green Process and Engineering, Institute of Process Engineering, Chinese Academy of Science, Beijing 100190, China 3) Faculty of Metallurgical and Energy Engineering, Kunming University of Science and Technology, Kunming 650093, China Corresponding author, E-mail: wangxh@home.ipe.ac.cn ABSTRACT Aiming at serious fluorine pollution problems in current hydrofluoric acid treatment processes of niobium-tantalum ore, a new leaching process of niobium-tantalum ore with an alkaline hydrothermal system was pro￾posed that KOH solution was used as a reaction medium to substitute highly toxic HF solution. The reaction rules of niobium-tantalum ore in the alkaline hydrothermal system were investigated. It is found that decomposition of niobium￾tantalum ore into soluble potassium hexa-niobate (tantalate) is promoted by increasing the KOH mass fraction and reaction temperature when the KOH mass fraction range is less than 50%, but soluble potassium hexa-niobate (tan￾talate) will change to insoluble potassium niobate (tantalate) when the KOH mass fraction and reaction temperature are too high, then the leaching rates of niobium and tantalum decrease. The leaching rates of niobium and tantalum are merely 18.73% and 9.4% respectively under optimum leaching conditions that the KOH mass fraction is 35%, the reaction temperature is 200 ℃, the KOH-to-ore mass ratio is 4:1 and the reaction time is 2 h, but they will increase 收稿日期：2012-08-25 基金项目：国家自然科学基金青年基金资助项目 (51004094)；国家高技术研究发展计划资助项目 (2009AA06Z103) DOI:10.13374/j.issn1001-053x.2013.10.011