白云鄂博尾矿中钪的浸出及铌富集物制备工艺研究
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摘要
以白云鄂博尾矿作为研究对象,通过先浓酸浸出,再助剂焙烧,最后酸浸的工艺路线,研究了白云鄂博尾矿浸出钪的工艺条件。考查了盐酸浸出条件和焙烧条件对钪浸出率的影响,实验发现浓酸浸出条件为:盐酸浓度8 mol/L、固液比为1∶5,酸浸二次浸出的盐酸浓度为4.8 mol/L;焙烧条件为:碱矿质量比1∶1、助剂使用硝酸钠,焙烧温度400℃、焙烧时间2 h时,钪的浸出率可达90%,经过处理的酸浸渣中铌的品位可达3%以上,作业回收率大于40%。
The process of recovering scandium from Bayan Obo mine tailings by pre-leaching with hydrochloric acid,calcining with Na OH and Na NO3,and leaching with hydrochloric acid again,was studied in this paper. And also the relationships between the leaching rate of scandium and leaching conditions and roasting conditions were studied. The research showes that when the concentration of hydrochloric acid is 8 mol/L,and solid-liquid ratio is 1∶ 5 during the pre-leaching; and when the calcinating temperature is 400 ℃,the roasting time is 2 h,the mass ratio of tailing-alkali is 1∶ 1,and fused salt is sodium nitrate during the process of calcining fused salt,and when the concentration of hydrochloric acid is 4. 8 mol/L during the process of acid leaching again,the leaching rate of scandium is more than 99%,and also the content of niobium in the acid slag is more than 3% and in the same time niobium operation recoverey is more than 40%.
The process of recovering scandium from Bayan Obo mine tailings by pre-leaching with hydrochloric acid,calcining with Na OH and Na NO3,and leaching with hydrochloric acid again,was studied in this paper. And also the relationships between the leaching rate of scandium and leaching conditions and roasting conditions were studied. The research showes that when the concentration of hydrochloric acid is 8 mol/L,and solid-liquid ratio is 1∶ 5 during the pre-leaching; and when the calcinating temperature is 400 ℃,the roasting time is 2 h,the mass ratio of tailing-alkali is 1∶ 1,and fused salt is sodium nitrate during the process of calcining fused salt,and when the concentration of hydrochloric acid is 4. 8 mol/L during the process of acid leaching again,the leaching rate of scandium is more than 99%,and also the content of niobium in the acid slag is more than 3% and in the same time niobium operation recoverey is more than 40%.
引文
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[15]陈宏.从含铌铁矿中提铌及制铌铁的新方法[J].钢铁,1999,34(3):13-19.Chen H.A new method on the extraction of Nb from Nbbearing iron ore for making Fe-Nb[J].Iron And Steel,1999,34(3):13-19.
[16]蒋曼.含铌铁精矿煤基直接还原过程中铌的行为研究[J].稀有金属,2011,35(5):731-735.Jiang M.Distribution behavior of niobium in process of coal-based direct reduction roasting of Nb-bearing iron concentrates[J].Chinese Journal of Rare Metals,2011,35(5):731-735.
[17]王中磊.氯化法从包头铁矿尾矿中提取铌和稀土的研究[J].中国稀土学报,2008,26(6):501-505.Wang Z L.Study on extraction of niobium and rare earth from Baotou iron ore tailings by chlorination method[J].Journal of the Chinese Society of Rare Earths,2008,26(6):501-505.
[18]李梅,周富强,高凯,等.白云鄂博稀土尾矿酸浸渣制备白炭黑[J].现代矿业,2014,(9):190-192,205.Li M,Zhou F Q,Gao K,et al.Preparation of precipitated silica by Baiyunebo rare earth tailings leaching residue[J].Modern Mining,2014,(9):190-192,205.
[19]于洪浩,薛向欣,贺燕,等.熔盐法从铁尾矿中制取高纯白炭黑[J].化工学报,2009,60(8):2124-2129.Yu H H,Xue X X,He Y,et al.Preparation of high purity precipitated silica from iron ore tailings by molten salt method[J].CIESC Journal,2009,60(8):2124-2129.
[2]程建忠,侯运炳,车丽萍.白云鄂博矿床稀土资源的合理开发及综合利用[J].稀土,2007,28(1):70-74.Cheng J Z,Hou Y B,Che L P.Making rational multipurpose use of resources of RE in Baiyunebo deposit[J].Chinese Rare Earths,2007,28(1):70-74.
[3]李全春.ICP-AES法测定白云鄂博矿中微量Sc203[J].稀土,1996,17(1):46-49.Li Q C.Determination of the trace element scandium in Baiyunobo ore by ICP-AES[J].Chinese Rare Earths,1996,17(1):46-49.
[4]刘世友.钪的资源生产应用与开发[J].稀有金属与硬质合,1995,23(2):57-61.Liu S Y.Resources,production and application of scandium[J].Rare Metals and Cemented Carbides,1995,23(2):57-61.
[5]Zhou M,Zhang J J,Ji L D,et al.Phase transition and piezoelectric,ferromagnetic response of B-site(Co,Nb)modified Ba Ti O3ceramics[J].Ceramics International,2014,40(1):853-857.
[6]李红,戎利军,陈翠英,等.SC法Nd Fe B合金生产中龟裂的产生及预防[J].稀土,2011,32(6):45-50.Li H,Rong L J,Chen C Y,et al.Production and prevention of cracks in Nd Fe B alloy manufacturing with SC process[J].Chinese Rare Earths,2011,32(6):45-50.
[7]郭财胜,李梅,柳召刚,等.白云鄂博稀土、铌资源综合利用现状及新思路[J].稀土,2014,32(6):96-100.Guo C S,Li M,Liu Z G,et al.Present status and new ideas on utilization of Bayan Obo rare earth and niobium resource[J].Chinese Rare Earths,2014,32(6):96-100.
[8]李梅,胡德志,柳召刚,等.白云鄂博稀土尾矿中钪的浸出方法研究[J].中国稀土学报,2013,31(6):703-709.Li M,Hu D Z,Liu Z G,et al.Leaching technology of scandium from Bayan Obo tailings[J].Journal of the Chinese Society of Rare Earths,2013,31(6):703-709.
[9]许延辉,马升峰,赵文怡,等.氯化钙焙烧盐酸分解提取白云鄂博选铌尾矿中的钪[J].稀土,2014,35(6):106-109.Xu Y H,Ma S F,Zhao W Y,et al.Extraction of scandium from Bayan Obo tailings by method of calcium chloride calcining-hydrochloric acid decomposition[J].Chinese Rare Earths,2014,35(6):106-109.
[10]王克勤,李爱秀,邓海霞,等.山西拜耳法赤泥脱铝提取氧化钪的研究[J].稀土,2012,33(3):78-81.Wang K Q,Li A X,Deng H X,et al.Study on removal of aluminum and extraction of scandia from Shanxi Bayer process red mud[J].Chinese Rare Earths,2012,33(3):78-81.
[11]张德文,赵文怡,许延辉,等.活化焙烧硫酸分解提取富铌渣中铌、钛、钪和稀土[J].稀土,2013,34(6):57-60.Zhang D W,Zhao W Y,Xu Y H,et al.Extracting Ni,Ti,Sc and RE from niobium-enriched slag by Ca Cl2roasing and H2SO4decomposition method[J].Chinese Rare Earths,2013,34(6):57-60.
[12]张德文,许延辉,马升峰,等.烧碱分解法提取白云鄂博选铌尾矿中的钪[J].安徽科技,2013,(9):43-44.Zhang D W,Xu Y H,Ma S F,et al.Extraction of scandium from Baiyunebo selected niobium tailings by caustic soda decomposition[J].Anhui Science&Technology,2013,(9):43-44.
[13]《白云鄂博矿矿冶工艺学》编辑委员会.白云鄂博矿矿冶工艺学矿山卷[M].包头:包头钢铁公司,1994.95-99,577-585.“The Technology of Mining and Metallurgy in Baiyunebo Mine”Editorial Board.Baiyun Obo Mining and Metallurgy Technology-Mining volume[M].Baotou:Baotou Iron and Steel Company,1994.95-99,577-585.
[14]徐广尧.包头铌资源综合利用关键技术研究[A].2007年中国稀土资源综合利用与环境保护研讨会编委会主编.2007年中国稀土资源综合利用与环境保护研讨会论文集[C].海南:2007.16-21.Xu G Y.Study on key technologies of comprehensive utilization of Baotou niobium resources[A].Editorial Board of Comprehensive Utilization and Environmental Protection of Rare Earth Resources in China.Proceedings of 2007 China Seminar on Comprehensive Utilization of Rare Earth Resources and Environmental Protection[C].Hainan:2007.16-21.
[15]陈宏.从含铌铁矿中提铌及制铌铁的新方法[J].钢铁,1999,34(3):13-19.Chen H.A new method on the extraction of Nb from Nbbearing iron ore for making Fe-Nb[J].Iron And Steel,1999,34(3):13-19.
[16]蒋曼.含铌铁精矿煤基直接还原过程中铌的行为研究[J].稀有金属,2011,35(5):731-735.Jiang M.Distribution behavior of niobium in process of coal-based direct reduction roasting of Nb-bearing iron concentrates[J].Chinese Journal of Rare Metals,2011,35(5):731-735.
[17]王中磊.氯化法从包头铁矿尾矿中提取铌和稀土的研究[J].中国稀土学报,2008,26(6):501-505.Wang Z L.Study on extraction of niobium and rare earth from Baotou iron ore tailings by chlorination method[J].Journal of the Chinese Society of Rare Earths,2008,26(6):501-505.
[18]李梅,周富强,高凯,等.白云鄂博稀土尾矿酸浸渣制备白炭黑[J].现代矿业,2014,(9):190-192,205.Li M,Zhou F Q,Gao K,et al.Preparation of precipitated silica by Baiyunebo rare earth tailings leaching residue[J].Modern Mining,2014,(9):190-192,205.
[19]于洪浩,薛向欣,贺燕,等.熔盐法从铁尾矿中制取高纯白炭黑[J].化工学报,2009,60(8):2124-2129.Yu H H,Xue X X,He Y,et al.Preparation of high purity precipitated silica from iron ore tailings by molten salt method[J].CIESC Journal,2009,60(8):2124-2129.