Cyanex272深度净化氯化镍溶液除去杂质钴的研究
|
摘要
采用溶剂萃取法,研究了用氨皂化的Cyanex272(二(2,4,4-三甲基戊基)次膦酸)对镍离子含量为25 g·L~(-1),钴离子含量为0.1 g·L~(-1)的氯化镍水溶液进行二级萃取除去溶液中杂质钴过程。考察了萃取振荡时间、有机相与水相比例(O/A)、初始水相pH值和Cyanex272体积浓度等因素对钴、镍离子萃取的影响。在单因素实验的基础上进行了正交试验,分别确定了各因素对钴、镍离子的影响主次关系。在综合考虑情况下确定了优化的工艺条件为:振荡时间为30 min、相比(O/A)为0.10∶1.00、初始水相pH值为5、 Cyanex272体积浓度为15%。此时,镍离子的损失率为10.84%,钴离子的萃取率为99.11%,水相中钴离子浓度为0.83×10~(-6)。通过红外光谱分析可知,钴、镍离子均会与萃取剂发生阳离子交换反应,且在钴、镍离子同时存在时,萃取剂与钴离子的结合要优于同镍离子的结合。
The secondary extraction of impurity cobalt from nickel chloride aqueous solution containing 25 g·L~(-1) nickel ion and 0.1 g·L~(-1) cobalt ion using Cyanex272(bis(2,4,4-trimethylpentyl) phosphonic acid) saponified with ammonia was studied by solvent extraction.The effects of the factors such as extraction oscillation time, the ratio of organic phase to aqueous phase(O/A), the initial pH value of aqueous phase and the volume concentration of Cyanex272 on the extraction of nickel and cobalt ions were investigated. The orthogonal experiment was carried out to determine the primary and secondary effects of various factors on nickel and cobalt ions on the basis of single factor experiment. The optimized process conditions were determined under condition of comprehensive consideration: the oscillation time was 30 min, the ratio of organic phase to aqueous phase(O/A) was 0.10∶1.00, the initial pH value of aqueous phase was 5, and the Cyanex 272 volume concentration was 15%. The results showed that the loss ratio of nickel ions was 10.84%, the extraction ratio of cobalt ions was 99.11%, and the concentration of cobalt ions in the aqueous phase was 0.83×10~(-6) under these conditions. It was proved that both cobalt and nickel ions could exchange cation with the extractant, moreover, the combination of the extractant with cobalt ion was better than that with nickel ion in the presence of both cobalt and nickel ions by the infrared spectrum analysis.
The secondary extraction of impurity cobalt from nickel chloride aqueous solution containing 25 g·L~(-1) nickel ion and 0.1 g·L~(-1) cobalt ion using Cyanex272(bis(2,4,4-trimethylpentyl) phosphonic acid) saponified with ammonia was studied by solvent extraction.The effects of the factors such as extraction oscillation time, the ratio of organic phase to aqueous phase(O/A), the initial pH value of aqueous phase and the volume concentration of Cyanex272 on the extraction of nickel and cobalt ions were investigated. The orthogonal experiment was carried out to determine the primary and secondary effects of various factors on nickel and cobalt ions on the basis of single factor experiment. The optimized process conditions were determined under condition of comprehensive consideration: the oscillation time was 30 min, the ratio of organic phase to aqueous phase(O/A) was 0.10∶1.00, the initial pH value of aqueous phase was 5, and the Cyanex 272 volume concentration was 15%. The results showed that the loss ratio of nickel ions was 10.84%, the extraction ratio of cobalt ions was 99.11%, and the concentration of cobalt ions in the aqueous phase was 0.83×10~(-6) under these conditions. It was proved that both cobalt and nickel ions could exchange cation with the extractant, moreover, the combination of the extractant with cobalt ion was better than that with nickel ion in the presence of both cobalt and nickel ions by the infrared spectrum analysis.
引文
[1] Chen Q Z,Gao F,Shi L.Experimental study on recovery of cobalt and nickel from manganese-cobalt-nickel slag by full wet method [J].Enterprise Technology Development,2014,(4):20.(陈奇志,高锋,史磊.全湿法从锰钴镍渣中回收钴、 镍的试验研 [J].企业技术开发,2014,(4):20.)
[2] Li Y W,Shang X,Huang X X,Lü P,Yang Z L.Effects of ultrasound on nickel sulfate plating and coating properties [J].Electroplating & Finishing,2012,34(6):10.(李延伟,尚雄,黄晓曦,吕频,杨哲龙.超声波对硫酸盐镀镍及镀层能的影响研究 [J].电镀与精饰,2012,34(6):10.)
[3] Liu H F,Xu G G,Fang S Y.Preparation of electrolytic nickel powder using chloride and sulfate electrolyte [J].Nonferrous Metals (Smelting),1999,(4):36.(刘海飞,许根国,方淑媛.用氯化盐和硫酸盐电解液制备电解镍 [J].有色金属(冶炼部分),1999,(4):36.)
[4] Feng C S.Electrodeposition of nickel from chloride solution [J].China Nonferrous Metallurgy,1995,(5):48.(冯长生.从氯化物溶液中电积镍 [J].中国有色冶金,1995,(5):48.)
[5] Guan Q J,Zhou G Y,Wen J K.Effect of impurity ions on separation of nickel and cobalt under different extraction systems [J].Chinese Journal of Rare Metals,2015,39(3):235.(管青军,周桂英,温建康.杂质离子对不同萃取体系下镍钴分离的影响研究 [J].稀有金属,2015,39(3):235.)
[6] Sato Y,Oue S,Heguri S,Shinichi H,Hiroaki N.Effect of dissolved impurities on the lightness and surface morphology of nickel deposits from chloride electrowinning solutions [J].Materials Transactions,2017,58(4):606.
[7] Reddy B R,Priya D N,Park K H.Separation and recovery of cadmium(II),cobalt(II) and nickel(II) from sulphate leach liquors of spent Ni-Cd batteries using phosphorus based extractants [J].Separation & Purification Technology,2006,50(2):161.
[8] Wen J J,Zhang Q X,Zhang G Q,Zhang L P.Deeply removing copper from nickel chloride electrolyte with novel silica-polyamine resin [J].Ion Exchange & Adsorption,2007,24(3):254.
[9] Qiu X,Hu H,Yang J,Yang J P,Wang C X,Cheng Z Y,Ji G F.Selective removal of copper from simulated nickel electrolyte by polystyrene-supported 2-aminomethylpyridine chelating resin [J].Chemical Papers,2018,72(8):2071.
[10] Li J T,Chen A L.Deep removal of copper from nickel electrolyte using manganese sulfide [J].Transactions of Nonferrous Metals Society of China,2015,25(11):3802.
[11] Zhang W,Cheng C Y,Pranolo Y.Investigation of methods for removal and recovery of manganese in hydrometallurgical processes [J].Hydrometallurgy,2010,101(1):58.
[12] Xiao C,Xiao L S.Principles and methods for extraction and separationof cobalt and nickel [J].Journal of Hydrometallurgy,2010,29(4):225.(肖超,肖连生.钴、 镍萃取分离原理与方法 [J].湿法冶金,2010,29(4):225.)
[13] Huang D S,Yu J G,Yi Z Z,Jiang Y,Chen Y S.Separation of cobalt and nickel from wastewater by P204 microemulsion saponified [J].Advanced Materials Research,2012,496:4.
[14] Zhang W J,Ma B Z,Wang C Y.Thermodynamic study on separation of ferrochrome from electroplating sludge based on phosphate precipitation [J].Chinese Journal of Rare Metals,2018,42(10):1084.(张文娟,马保中,王成彦.基于磷酸盐沉淀分离电镀污泥中铬铁的热力学研究 [J].稀有金属,2018,42(10):1084.)
[15] Kang J G,Senanayake G,Sohn J,Shun M Y.Recovery of cobalt sulfate from spent lithium ion batteries by reductive leaching and solvent extraction with Cyanex272 [J].Hydrometallurgy,2010,100(3):168.
[16] Liu J H,Zhou G Y,Wen J K.Kinetics of cobalt and nickel extraction by P507-Cyanex272 sodium soap [J].Chinese Journal of Rare Metals,2013,37(6):939.(刘纪红,周桂英,温建康.P507-Cyanex272钠皂萃取钴、 镍动力学研究 [J].稀有金属,2013,37(6):939.)
[17] Liu D X.Study on the separation of cobalt and nickel by using new generation extractant Cyanex272 [J].Mining & Metallurgy,1996,(3):51.(刘大星.应用新一代萃取剂Cyanex272进行钴镍分离的研究 [J].矿冶,1996,(3):51.)
[18] Wang F C,He F H,Zhao J M,Sui N,Lin X,Liu H Z.Extraction and separation of cobalt(II),copper(II) and manganese(II)by Cyanex272,PC-88A and their mixtures [J].Separation and Purification Technology,2012,93(6):8.
[19] Coll M T,Fortuny A,Kedari C S,Sastr A M.Studies on the extraction of Co(II) and Ni(II) from aqueous chloride solutions using Primene JMT-Cyanex272 ionic liquid extractant [J].Hydrometallurgy,2012,125-126(8):24.
[20] Qiu S,Qiu X C,Huang S M,Sha Z Y.Determination of nickel in nickel plating solution by EDTA complexometric titration [J].Electroplating & Finishing,2002,21(6):47.(丘山,丘星初,黄曙明,沙志勇.EDTA络合滴定法测定镀镍溶液中的镍含量 [J].电镀与涂饰,2002,21(6):47.)
[2] Li Y W,Shang X,Huang X X,Lü P,Yang Z L.Effects of ultrasound on nickel sulfate plating and coating properties [J].Electroplating & Finishing,2012,34(6):10.(李延伟,尚雄,黄晓曦,吕频,杨哲龙.超声波对硫酸盐镀镍及镀层能的影响研究 [J].电镀与精饰,2012,34(6):10.)
[3] Liu H F,Xu G G,Fang S Y.Preparation of electrolytic nickel powder using chloride and sulfate electrolyte [J].Nonferrous Metals (Smelting),1999,(4):36.(刘海飞,许根国,方淑媛.用氯化盐和硫酸盐电解液制备电解镍 [J].有色金属(冶炼部分),1999,(4):36.)
[4] Feng C S.Electrodeposition of nickel from chloride solution [J].China Nonferrous Metallurgy,1995,(5):48.(冯长生.从氯化物溶液中电积镍 [J].中国有色冶金,1995,(5):48.)
[5] Guan Q J,Zhou G Y,Wen J K.Effect of impurity ions on separation of nickel and cobalt under different extraction systems [J].Chinese Journal of Rare Metals,2015,39(3):235.(管青军,周桂英,温建康.杂质离子对不同萃取体系下镍钴分离的影响研究 [J].稀有金属,2015,39(3):235.)
[6] Sato Y,Oue S,Heguri S,Shinichi H,Hiroaki N.Effect of dissolved impurities on the lightness and surface morphology of nickel deposits from chloride electrowinning solutions [J].Materials Transactions,2017,58(4):606.
[7] Reddy B R,Priya D N,Park K H.Separation and recovery of cadmium(II),cobalt(II) and nickel(II) from sulphate leach liquors of spent Ni-Cd batteries using phosphorus based extractants [J].Separation & Purification Technology,2006,50(2):161.
[8] Wen J J,Zhang Q X,Zhang G Q,Zhang L P.Deeply removing copper from nickel chloride electrolyte with novel silica-polyamine resin [J].Ion Exchange & Adsorption,2007,24(3):254.
[9] Qiu X,Hu H,Yang J,Yang J P,Wang C X,Cheng Z Y,Ji G F.Selective removal of copper from simulated nickel electrolyte by polystyrene-supported 2-aminomethylpyridine chelating resin [J].Chemical Papers,2018,72(8):2071.
[10] Li J T,Chen A L.Deep removal of copper from nickel electrolyte using manganese sulfide [J].Transactions of Nonferrous Metals Society of China,2015,25(11):3802.
[11] Zhang W,Cheng C Y,Pranolo Y.Investigation of methods for removal and recovery of manganese in hydrometallurgical processes [J].Hydrometallurgy,2010,101(1):58.
[12] Xiao C,Xiao L S.Principles and methods for extraction and separationof cobalt and nickel [J].Journal of Hydrometallurgy,2010,29(4):225.(肖超,肖连生.钴、 镍萃取分离原理与方法 [J].湿法冶金,2010,29(4):225.)
[13] Huang D S,Yu J G,Yi Z Z,Jiang Y,Chen Y S.Separation of cobalt and nickel from wastewater by P204 microemulsion saponified [J].Advanced Materials Research,2012,496:4.
[14] Zhang W J,Ma B Z,Wang C Y.Thermodynamic study on separation of ferrochrome from electroplating sludge based on phosphate precipitation [J].Chinese Journal of Rare Metals,2018,42(10):1084.(张文娟,马保中,王成彦.基于磷酸盐沉淀分离电镀污泥中铬铁的热力学研究 [J].稀有金属,2018,42(10):1084.)
[15] Kang J G,Senanayake G,Sohn J,Shun M Y.Recovery of cobalt sulfate from spent lithium ion batteries by reductive leaching and solvent extraction with Cyanex272 [J].Hydrometallurgy,2010,100(3):168.
[16] Liu J H,Zhou G Y,Wen J K.Kinetics of cobalt and nickel extraction by P507-Cyanex272 sodium soap [J].Chinese Journal of Rare Metals,2013,37(6):939.(刘纪红,周桂英,温建康.P507-Cyanex272钠皂萃取钴、 镍动力学研究 [J].稀有金属,2013,37(6):939.)
[17] Liu D X.Study on the separation of cobalt and nickel by using new generation extractant Cyanex272 [J].Mining & Metallurgy,1996,(3):51.(刘大星.应用新一代萃取剂Cyanex272进行钴镍分离的研究 [J].矿冶,1996,(3):51.)
[18] Wang F C,He F H,Zhao J M,Sui N,Lin X,Liu H Z.Extraction and separation of cobalt(II),copper(II) and manganese(II)by Cyanex272,PC-88A and their mixtures [J].Separation and Purification Technology,2012,93(6):8.
[19] Coll M T,Fortuny A,Kedari C S,Sastr A M.Studies on the extraction of Co(II) and Ni(II) from aqueous chloride solutions using Primene JMT-Cyanex272 ionic liquid extractant [J].Hydrometallurgy,2012,125-126(8):24.
[20] Qiu S,Qiu X C,Huang S M,Sha Z Y.Determination of nickel in nickel plating solution by EDTA complexometric titration [J].Electroplating & Finishing,2002,21(6):47.(丘山,丘星初,黄曙明,沙志勇.EDTA络合滴定法测定镀镍溶液中的镍含量 [J].电镀与涂饰,2002,21(6):47.)
© 2004-2018 中国地质图书馆版权所有 京ICP备05064691号 京公网安备11010802017129号 地址：北京市海淀区学院路29号 邮编：100083 电话：办公室：(+86 10)66554848；文献借阅、咨询服务、科技查新：66554700 |