从钨渣硫酸浸出液中萃取钪的研究
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摘要
采用P204-TBP从钨渣硫酸浸出液中萃取Sc,H_2SO_4洗脱负载有机相中的Fe,NaOH反萃洗脱有机相中的Sc。试验结果表明,在5%P204+3%TBP+煤油体系中,温度25℃,O/A=1∶10,时间15min条件下,经五级逆流萃取,Sc萃取率为97.37%。经4mol/L的H_2SO_4五级逆流洗脱,Fe洗脱率为98.63%,而Sc损失率小于1%。洗脱Fe后的有机相用3mol/L的NaOH反萃,Sc单级反萃率为98.31%。经该方法获得的粗Sc纯度达82%以上,Sc总回收率达95%以上。
The extraction of scandium from the leaching solution of tungsten residue was carried out by P204-TBP,sulfuric acid eluted the iron in the loaded organic phase and scandium was stripped in the eluted organic phase by sodium hydroxide.The results show that in the system of 5% P204+3% TBP+ kerosene,the extraction rate of scandium is 97.37%through five-stage counter current extraction with O/A ratio of 1∶10,temperature of 25 ℃,and time of 15 min.Through five-stage counter current elution by 4 mol/L H_2 SO_4,the elution rate of iron is 98.63%,while the scandium loss rate is less than 1%.The eluted organic phase was stripped with 3 mol/L sodium hydroxide.The single-stage stripping rate of scandium reaches 98.31%.By using the method,the purity of crude scandium can reach more than 82%,and the total recovery rate of scandium is more than 95%.
The extraction of scandium from the leaching solution of tungsten residue was carried out by P204-TBP,sulfuric acid eluted the iron in the loaded organic phase and scandium was stripped in the eluted organic phase by sodium hydroxide.The results show that in the system of 5% P204+3% TBP+ kerosene,the extraction rate of scandium is 97.37%through five-stage counter current extraction with O/A ratio of 1∶10,temperature of 25 ℃,and time of 15 min.Through five-stage counter current elution by 4 mol/L H_2 SO_4,the elution rate of iron is 98.63%,while the scandium loss rate is less than 1%.The eluted organic phase was stripped with 3 mol/L sodium hydroxide.The single-stage stripping rate of scandium reaches 98.31%.By using the method,the purity of crude scandium can reach more than 82%,and the total recovery rate of scandium is more than 95%.
引文
[1]HIRANO M,WATANABE S,KATO E,et al.High electrical conductivity and high fracture strength of Sc2O3-doped zirconia ceramics with submicrometer grains[J].Journal of the American Ceramic Society,1999,82(10):2 861-2 864.
[2]李力,姜锋,李汉广.新世纪钪的应用开发和科技发展前景[J].稀有金属与硬质合金,2002,30(3):38-41.
[3]李汉广,尹志民.钪的发展动态和发展战略[J].稀有金属与硬质合金,1996,24(1):47-51.
[4]朱海玲,邓海波,吴承桧,等.钨渣的综合回收利用技术研究进展[J].中国钨业,2010,25(4):15-18.
[5]杨秀丽,王晓辉,向仕彪,等.盐酸法富集钨渣中的钽和铌[J].中国有色金属学报,2013(3):873-881.
[6]梁勇,王瑞祥,刘俊.高纯稀土化合物制备的现状与发展[J].上海有色金属,2004,25(4):188-191.
[7]廖春生,徐刚.新世纪的战略资源——钪的提取与应用[J].中国稀土学报,2001,19(4):289-297.
[8]钱强.溶剂萃取在湿法冶金中的应用[M].北京:冶金工业出版社,1979.
[9]王克勤,于永波,王皓,等.赤泥盐酸浸出提取钪的试验研究[J].稀土.2010,31(1):95-98.
[10]姜平国,廖春发.从赤泥盐酸浸出液中提取钪的工艺研究[J].中国有色冶金.2012,41(1):66-68.
[11]杨革.从钨渣中提取高纯氧化钪[J].湖南有色金属,2001,17(1):18-20.
[12]徐廷华,邓佐国,李伟,等.从钨渣浸出液中提取钪的研究[J].江西有色金属.1997,11(4):32-35.
[13]LI D,WANG C.Solvent extraction of Scandium(Ⅲ)by Cyanex 923and Cyanex 925[J].Hydrometallurgy.1998,48(3):301-312.
[14]PEPPARD D F,PARK O,NACHTMAN E S.Separation of scandium from aqueous solutions:US2824783[P].1958-02-25
[15]KOROVIN V,SHESTAK Y,POGORELOV Y.Scandium extraction by neutral organo-phosphorus compounds supported on a porous carrier[J].Hydrometallurgy.1999,52(1):1-8.
[16]钟学明.伯胺萃取法提取氧化钪的工艺研究[J].稀有金属,2002,26(6):527-529.
[17]钟学明.从钨渣中提取氧化钪的工艺研究[J].江西冶金,2002,22(3):19-22.
[18]KARVE M A,KHOPKAR S M.Separation of scandium(III)as ascorbato complex by extraction with Aliquat 336S[J].Bulletin of the Chemical Society of Japan,1991,64:655.
[19]VIBHUTE C P,KHOPKAR S M.Separation of scandium(III)as citrate complex by extraction with Aliquat336S[J].Indian Journal of Chemistry—Section A,1985,24A(5):444.
[20]SOKOLOVA Y V.Sorption purification of scandium to remove zirconium impurity in hydrochloric acid solutions[J].Russian Journal of Applied Chemistry,2001,74(3):414.
[21]MEHTA V P,KHOPKAR S M.Cation exchange chromatographic separation of scandium from other elements on Dowex 50W-X8[J].Separation Science and Technology.1978,13(10):933-939.
[22]尹志民.钪和含钪合金[M].长沙:中南大学出版社,2007:12.
[23]胡莉蓉,乐晓兵,李宁,等.电感耦合等离子体原子发射光谱法测定钛白废酸萃取相中6种微量元素[J].冶金分析,2015,35(2):52-56.
[2]李力,姜锋,李汉广.新世纪钪的应用开发和科技发展前景[J].稀有金属与硬质合金,2002,30(3):38-41.
[3]李汉广,尹志民.钪的发展动态和发展战略[J].稀有金属与硬质合金,1996,24(1):47-51.
[4]朱海玲,邓海波,吴承桧,等.钨渣的综合回收利用技术研究进展[J].中国钨业,2010,25(4):15-18.
[5]杨秀丽,王晓辉,向仕彪,等.盐酸法富集钨渣中的钽和铌[J].中国有色金属学报,2013(3):873-881.
[6]梁勇,王瑞祥,刘俊.高纯稀土化合物制备的现状与发展[J].上海有色金属,2004,25(4):188-191.
[7]廖春生,徐刚.新世纪的战略资源——钪的提取与应用[J].中国稀土学报,2001,19(4):289-297.
[8]钱强.溶剂萃取在湿法冶金中的应用[M].北京:冶金工业出版社,1979.
[9]王克勤,于永波,王皓,等.赤泥盐酸浸出提取钪的试验研究[J].稀土.2010,31(1):95-98.
[10]姜平国,廖春发.从赤泥盐酸浸出液中提取钪的工艺研究[J].中国有色冶金.2012,41(1):66-68.
[11]杨革.从钨渣中提取高纯氧化钪[J].湖南有色金属,2001,17(1):18-20.
[12]徐廷华,邓佐国,李伟,等.从钨渣浸出液中提取钪的研究[J].江西有色金属.1997,11(4):32-35.
[13]LI D,WANG C.Solvent extraction of Scandium(Ⅲ)by Cyanex 923and Cyanex 925[J].Hydrometallurgy.1998,48(3):301-312.
[14]PEPPARD D F,PARK O,NACHTMAN E S.Separation of scandium from aqueous solutions:US2824783[P].1958-02-25
[15]KOROVIN V,SHESTAK Y,POGORELOV Y.Scandium extraction by neutral organo-phosphorus compounds supported on a porous carrier[J].Hydrometallurgy.1999,52(1):1-8.
[16]钟学明.伯胺萃取法提取氧化钪的工艺研究[J].稀有金属,2002,26(6):527-529.
[17]钟学明.从钨渣中提取氧化钪的工艺研究[J].江西冶金,2002,22(3):19-22.
[18]KARVE M A,KHOPKAR S M.Separation of scandium(III)as ascorbato complex by extraction with Aliquat 336S[J].Bulletin of the Chemical Society of Japan,1991,64:655.
[19]VIBHUTE C P,KHOPKAR S M.Separation of scandium(III)as citrate complex by extraction with Aliquat336S[J].Indian Journal of Chemistry—Section A,1985,24A(5):444.
[20]SOKOLOVA Y V.Sorption purification of scandium to remove zirconium impurity in hydrochloric acid solutions[J].Russian Journal of Applied Chemistry,2001,74(3):414.
[21]MEHTA V P,KHOPKAR S M.Cation exchange chromatographic separation of scandium from other elements on Dowex 50W-X8[J].Separation Science and Technology.1978,13(10):933-939.
[22]尹志民.钪和含钪合金[M].长沙:中南大学出版社,2007:12.
[23]胡莉蓉,乐晓兵,李宁,等.电感耦合等离子体原子发射光谱法测定钛白废酸萃取相中6种微量元素[J].冶金分析,2015,35(2):52-56.