采用HBL101萃取石煤高酸浸出液中的钒
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摘要
针对现行石煤提钒萃取工艺及研究现状,提出采用新型萃取剂HBL101从石煤高酸浸出料液中直接萃取钒的方案,考察料液的酸度、料液电位、萃取时间、相比以及温度对萃取率的影响,绘制HBL1010萃取等温曲线。结果表明:在料液酸度为1.458 mol/L,萃取温度为35~45℃,萃取时间为10min,相比O/A=1/1(油相与水相体积比)的条件下,钒的单级萃取率达到95%以上。三级逆流萃取实验结果显示,钒的萃取率达到99.7%以上。采用NaOH对负载有机相进行反萃,反萃液经调节pH后直接加入NH4Cl沉钒,得到的五氧化二钒纯度达到98.68%以上。
A new extractant HBL101 was used to directly extract vanadium from high acid leach solution of stone coal.The effects of acidity and potential of feed,time,phase ratio and temperature on the extraction of vanadium were investigated.The extraction distribution isotherms of vanadium were plotted.The extraction distribution isotherm was also obtained.The results show that the extraction of vanadium from the solution with 1.458 mol/L [H+] reaches 95% in single stage with A/O ratio of 1:1(volume ratio of oil phase to aqueous phase) at 35 45 ℃ for 10 min.In three-stage counter current test,the extraction rate of vanadium is 99.7%.The loaded organic can be easily stripped using NaOH solution.After pH adjustment,the strip liquor is used to precipitate vanadium by adding NH4Cl.The final product of V2O5with purity of 98.68% can be obtained.
A new extractant HBL101 was used to directly extract vanadium from high acid leach solution of stone coal.The effects of acidity and potential of feed,time,phase ratio and temperature on the extraction of vanadium were investigated.The extraction distribution isotherms of vanadium were plotted.The extraction distribution isotherm was also obtained.The results show that the extraction of vanadium from the solution with 1.458 mol/L [H+] reaches 95% in single stage with A/O ratio of 1:1(volume ratio of oil phase to aqueous phase) at 35 45 ℃ for 10 min.In three-stage counter current test,the extraction rate of vanadium is 99.7%.The loaded organic can be easily stripped using NaOH solution.After pH adjustment,the strip liquor is used to precipitate vanadium by adding NH4Cl.The final product of V2O5with purity of 98.68% can be obtained.
引文
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[14]沈明伟,朱昌洛,李华伦.P507-煤油体系在钒钼萃取分离中的试验研究[J].矿产综合利用,2007(4):1418.SHENG Ming-wei,ZHU Chang-luo,LI Hua-lun.P507-Kerosene system in extraction separation of vanadium andmolybdenum[J].Multipurpose Utilization of Mineral Resources,2007(4):14 18.
[15]刘玉国,安悦,付晓东,杨东.P538萃取钒(Ⅳ)的研究[J].光谱实验室,1998,15(5):3234.LIU Yu-guo,AN Yue,FU Xiao-dong,YANG Dong.Study onvanadium(Ⅳ)extracted by P538[J].Chinese Journal ofSpectroscopy Laboratory,1998,15(5):32 34.
[16]KIM K,CHO J W.Selective recovery of metals from spentdesulphurization catalyst[J].Korean Journal of ChemicalEngineering,1997,14(3):162 167.
[17]ZENG L,CHENG C Y.Recovery of molybdenum andvanadium from synthetic sulphuric acid leach solutions of spenthydrodesulphurisation catalysts using solvent extraction[J].Hydrometallurgy,2010,101:141 147.
[18]POST K,RIBINS R G.Thermodynamic diagram for thevanadium–water system at 298.15 K[J].Electrochimica Acta,1976,21:401 405.
[19]BARNARD K R,TURNER N L.The effect of temperature onhydroxyoxime stability in the LIX 63–versatic 10–tributylphosphate synergistic solvent extraction system under syntheticnickel laterite conditions[J].Hydrometallurgy,2011,109:245 251.
[2]鲁兆伶.用酸法从石煤中提取五氧化二钒的试验研究与工业实践[J].湿法冶金,2002,21(4):175183.LU Zhao-ling.Investigation and industrial practice on extractionof V2O5from stone coal containing vanadium by acid process[J].Hydrometallurgy of China,2002,21(4):175 183.
[3]王晓丹,朱云.制酸废催化剂回收钒[J].有色金属,2010,62(4):62 64.WANG Xiao-dan,ZHU Yun.Vanadium recovery from spentacid-making catalyst[J].Nonferrous Metals,2010,62(4):62 64.
[4]胡建锋,朱云.P204萃取硫酸体系中钒的性能研究[J].稀有金属,2007,31(7):367370.HU Jian-feng,ZHU Yun.Extraction of vanadium by P204 fromsulfuric acid solution[J].Chinese Journal of Rare Metals,2007,31(7):367 370.
[5]LI Xing-bin,WEI Chang,DENG Zhi-gan,LI Min-ting,LICun-xiong,FAN Gang.Selective solvent extraction of vanadiumover iron from a stone coal/black shale acid leach solution byD2EHPA/TBP[J].Hydrometallurgy,2010,105:359 363.
[6]李兴彬,魏昶,樊刚,邓志敢,李旻廷,李存兄.溶剂萃取铵盐沉钒法从石煤酸浸液中提取五氧化二钒的研究[J].矿冶,2010,19(3):4953.LI Xing-bin,WEI Chang,FAN Gang,DENG Zhi-gan,LIMin-ting,LI Cun-xiong.Research of vanadium pentoxide froman acid leaching solution of stone coal using solvent extractionand ammonium precipitation[J].Mining&Metallurgy,2010,19(3):49 53.
[7]李晓健.酸浸萃取工艺在石煤提钒工业中的设计与运用[J].湖南有色金属,2000,16(3):2123.LI Xiao-jin.Design and application of acid leaching—Extractionprocessing in bone coal extracting vanadium industry[J].HunanNonferrous Metals,2000,16(3):21 23.
[8]曹耀华,高照国,刘红召,李琦.萃取法从含钒酸浸液中提取钒的研究[J].河南化工,2007,24(6):2023.CAO Yao-hua,GAO Zhao-guo,LIU Hong-zhao,LI Qi.Studyon vanadium extraction from vanadium acid leaching solution[J].Henan Chemical Industry,2007,24(6):20 23.
[9]WANG Yu-xing,LUO Qin-ge,LIU Shu-me.A study onextraction mechanism of vanadium(Ⅴ)by primary amine第23卷第4期李青刚,等:采用HBL101萃取石煤高酸浸出液中的钒1113N1923[J].Natural Science Journal of Xiangtan University,1990,19(3):139 146.
[10]刘彦华,杨超.用溶剂萃取法从含钒浸出液中直接沉淀钒[J].湿法冶金,2010,29(4):263267.LIU Yan-hua,YANG Chao.Research on direct precipitate ofvanadium in vanadiferous leaching solution[J].Hydrometallurgyof China,2010,29(4):263 266.
[11]刘波,冯光熙,黄祥玉,张敏.用N263从钒溶液中回收钒[J].化学研究与应用,2003,15(1):5457.LIU Bo,FENG Guang-xi,HUANG Xiang-yu,ZHANG Min.Recovery of vanadium pentoxide from contained vanadiumsolution with methyltri(C9-11 alkyl)ammonium chloride[J].Chemical Research and Application,2003,15(1):54 57.
[12]张云,范必威,彭达平,陈细发.从石煤酸浸液中萃取钒的工艺研究[J].成都理工学院学报,2001,28(1):107109.ZHANG Yun,FAN Bi-wei,PENG Da-ping,CHEN Xi-fa.Technology of extracting V2O5from the stone coal acid-leachingsolution with TOA[J].Journal of Chengdu University ofTechnology,2001,28(1):107 109.
[13]姚宝书.TBP萃取偏钒酸铵的条件[J].化学世界,1990,31(1):12 14.YAO Bao-shu.The conditions of ammonium metavanadateextraction using TBP[J].Chemical World,1990,31(1):12 14.
[14]沈明伟,朱昌洛,李华伦.P507-煤油体系在钒钼萃取分离中的试验研究[J].矿产综合利用,2007(4):1418.SHENG Ming-wei,ZHU Chang-luo,LI Hua-lun.P507-Kerosene system in extraction separation of vanadium andmolybdenum[J].Multipurpose Utilization of Mineral Resources,2007(4):14 18.
[15]刘玉国,安悦,付晓东,杨东.P538萃取钒(Ⅳ)的研究[J].光谱实验室,1998,15(5):3234.LIU Yu-guo,AN Yue,FU Xiao-dong,YANG Dong.Study onvanadium(Ⅳ)extracted by P538[J].Chinese Journal ofSpectroscopy Laboratory,1998,15(5):32 34.
[16]KIM K,CHO J W.Selective recovery of metals from spentdesulphurization catalyst[J].Korean Journal of ChemicalEngineering,1997,14(3):162 167.
[17]ZENG L,CHENG C Y.Recovery of molybdenum andvanadium from synthetic sulphuric acid leach solutions of spenthydrodesulphurisation catalysts using solvent extraction[J].Hydrometallurgy,2010,101:141 147.
[18]POST K,RIBINS R G.Thermodynamic diagram for thevanadium–water system at 298.15 K[J].Electrochimica Acta,1976,21:401 405.
[19]BARNARD K R,TURNER N L.The effect of temperature onhydroxyoxime stability in the LIX 63–versatic 10–tributylphosphate synergistic solvent extraction system under syntheticnickel laterite conditions[J].Hydrometallurgy,2011,109:245 251.