采用HDNNS/4PC协萃体系从硫酸盐中萃取钴过程中的相分离（英文）
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摘要
相分离速率是决定溶剂萃取体系在湿法冶金中得到应用的关键。研究二壬基萘磺酸和4-吡啶甲酸异辛酯协同混合体系从单金属硫酸盐溶液中萃取钴的相分离,探索负载有机相的物理化学性质以及反胶束的形态对相分离的影响。结果表明,负载有机相的黏度及増溶水量是影响相分离的主要因素。随着这两个因素的增加,混合澄清速率明显降低。X射线小角散射(SAXS)测量结果证实负载有机相中反相胶束的形貌会随混合澄清速率的变化而变化。
Phase separation rate is a critical character in determining the usefulness of a solvent extraction system in hydrometallurgy. A survey of the synergistic mixture containing dinonylnaphthalene sulfonic acid(HDNNS) and 2-ethylhexly 4-pyridinecarboxylate ester(4 PC) for the extraction of cobalt from acidic single metal sulfate solution was carried out to suggest how the physicochemical properties and the morphology of the reverse micelles in the loaded organic phase affect the phase separation. The results show that effective parameters affecting the phase separation are the viscosity and the excess water uptake of the loaded organic phase. It is obvious that the specific settling rate(SSR) decreases with the apparent increase of these two parameters. The measurement of small angle X-ray scattering(SAXS) proves that the morphology of the reversed micelles in the loaded organic phase changes evidently with the change of the specific settling rate(SSR).
Phase separation rate is a critical character in determining the usefulness of a solvent extraction system in hydrometallurgy. A survey of the synergistic mixture containing dinonylnaphthalene sulfonic acid(HDNNS) and 2-ethylhexly 4-pyridinecarboxylate ester(4 PC) for the extraction of cobalt from acidic single metal sulfate solution was carried out to suggest how the physicochemical properties and the morphology of the reverse micelles in the loaded organic phase affect the phase separation. The results show that effective parameters affecting the phase separation are the viscosity and the excess water uptake of the loaded organic phase. It is obvious that the specific settling rate(SSR) decreases with the apparent increase of these two parameters. The measurement of small angle X-ray scattering(SAXS) proves that the morphology of the reversed micelles in the loaded organic phase changes evidently with the change of the specific settling rate(SSR).
引文
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[5]HU Fang,HU Hui-ping,HU Jiu-gang,ZHU Shan,YANG Jin-peng,WANG Yon-xi.Improving selective separation of Cu(II)from acidic polymetallic media with 2-ethylhexyl 4-pyridinecarboxylate ester:Extraction behaviors,coordination structure and microscopic mechanism[J].Journal of Molecular Liquids,2017,248:1050-1058.
[6]LI Ji-yuan.Study on the extraction and mechanism of nickel in polymetallic solution by HDNNS/4PC[D].Changsha:Central South University,2017.(in Chinese)
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[9]WANG Shu-chan,ZHANG Ting-an,ZHANG Zi-mu,LV Chao,ZHAO Qiu-yue,LIU Yan.Effect of stirring on oil-water separation in rare earth mixer-settler[J].China Petroleum Processing&Petrochemical Technology,2014,16(3):99-103.
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[13]LIU Xiao-rong,QIU Guan-zhou,HU Yue-hua,YANG Jun-he,JINMin-lin.Effect of Lix984N content on phase disengagement dynamics in copper-SX[J].Transactions of Nonferrous Metals Society of China,2003,13(4):963-967.
[14]LIU Yan-jun,LIU Xiao-rong,LI Hui,LI Qing,LI Yong-sheng,SUChang,TIAN Jun,WANG Yu-cheng.Effects of strong-acid on performances of copper solvent extraction[J].Advanced Materials Research,2014,881-883:48-51.
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[16]XUE Shu-yun,FU Xun,XIONG Ya-hong,ZHANG Shao-na,HUZheng-shui.Study on the thiophosphinic extractants.I.The basic properties of the extractants and the phase behavior in their saponified systems[J].Solvent Extraction and Ion Exchange,2002,20(3):331-344.
[17]MOVER B A,Mc DOWELL W J.Factors influencing phase disengagement rates in solvent extraction systems employing tertiary amine extractants[J].Separation Science,1981,16(9):1261-1289.
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[20]RAATZ S,KLAPPER P,REPKE J U.Micellar extraction of zinc using di(2-ethylhexyl)phosphorsure in presence of surfactant cetyltrimethyl ammonium bromide[J].Chemie Ingenieur Technik,2011,83(4):518-524.(in German)
[21]BARNEA E.Liquid-liquid contacting-art or science?Part I.Characterization of liquid-liquid system[J].Hydrometallurgy,1979,5:15-28.
[22]ZHU Shan,HU Hui-ping,HU Jiu-gang,LI Ji-yuan,HU Fang,WANG Yong-xi.Structural insights into the extraction mechanism of cobalt(II)with dinonylnaphthalene sulfonic acid and 2-ethylhexyl4-pyridinecarboxylate ester[J].Journal of coordination chemistry,2018,71(15):2441-2456.
[23]LI Ji-yuan,HU Hui-ping,ZHU Shan,HU Fang,WANG Yong-xi.The coordination structure of the extracted nickel(II)complex with a synergistic mixture containing dinonylnaphthalene sulfonic acid and2-ethylhexyl 4-pyridinecarboxylate ester[J].Dalton Transactions,2017,46:1075-1082.
[24]PRESTON J,PREEZ A D.The solvent extraction of nickel and cobalt bymixtures of carboxylic acids and pyridinecarboxylate esters[J].Solvent Extraction&Ion Exchange,1995,13(3):465-494.
[25]CHENG C Y,BARNARD K R,DAVIES M G.A study on the chemical stability of the Versatic 10-Acorga CLX50 synergistic system[J].Minerals Engineering,2002,15(12):1151-1161.
[26]ZHOU Li-ping,ZENG Xiao-qin,LI De-jiang,YANG Chun-ming.Ageing precipitation behavior of Mg-12Gd alloy[J].Chinese Journal of Nonferrous Metals,2015,25(6):1409-1416.(in Chinese)
[27]FRITZ G,BERGMANN A,GLATTER O.Evaluation of small-angle scattering data of charged particles using the generalized indirect Fourier transformation technique[J].Journal of Chemical Physics,2000,113(21):9733-9740.
[28]SALGI P,RAJAGOPALAN R.Polydispersity in colloids:Implications to static structure and scattering[J].Advances in Colloid&Interface Science,1993,43(2-3):169-288.
[29]PERCUS J K,YEVICK G J.Analysis of classical statistical mechanics by means of collective coordinates[J].Physical Review,1958,110:1-13.
[30]FRITZ G,GLATTER O.Structure and interaction in dense colloidal systems:evaluation of scattering data by the generalized indirect Fourier transformation method[J].Journal of Physics Condensed Matter,2006,18(36):S2403-S2419.
[31]NING Peng-ge,CAO Hong-bin,ZHANG Yi.Stability of the interfacial crud produced during the extraction of vanadium and chromium[J].Hydrometallurgy,2013,133(2):156-160.
[32]VIDYALAKSHMI V,SUBRAMANIAN M S,RAJESWARI S,SRINIVASAN T G,VASUDEVA RAO P R.Interfacial tension studies of N,N-dialkyl amides[J].Solvent Extraction&Ion Exchange,2003,21(3):399-412.
[33]RYDBERG J,COX M,MUSIKAS C,CHOPPIN G R.Solvent extraction principles and practice[M].2nd ed.Boca Raton:CRCPress,2004.
[34]GONG Xing-chu,LV Yang-cheng,LI Mu,MA Xue-feng,NIQian-yin LUO Guang-sheng.Selection and evaluation of a new extractant for caprolactam extraction[J].Chinese Journal of Chemical Engineering,2008,16(6):876-880.
[35]ALBERTS E,DORFLING C.Stripping conditions to prevent the accumulation of rare earth elements and iron on the organic phase in the solvent extraction circuit at skorpion zinc[J].Minerals Engineering,2013,40(40):48-55.
[36]MUSADAIDZWA J M,TSHININGAYAMWE E I.Skorpion zinc solvent extraction:The upset conditions[J].Journal of the Southern African Institute of Mining&Metallurgy,2009,109:691-695.
[37]TESTARD F,BAUDUIN P,ZEMB T,BERTHON L.Third-phase formation in liquid/liquid extraction:A colloidal approach[M].Boca Raton,FL and London:CRC Press,Taylor&Francis Group,2010.
[38]CHIARIZIA R,DANESI P R,D'ALESSANDRO G,SCUPPAR B.Interfacial behaviour of dinonylnaphthalenesulfonic acid at the toluene-HCl O4 interface[J].Journal of Inorganic&Nuclear Chemistry,1976,38(7):1367-1369.
[39]OSSEO-ASARE K,KEENEY M E.Aspects of the interfacial chemistry of nickel extraction with LIX63-HDNNS mixtures[J].Metallurgical and Materials Transactions B,1980,11:63-67.
[40]WONG M,THOMAS J K,GRAETZEL M.Fluorescence probing of inverted micelles.The state of solubilized water clusters in alkane diisooctyl sulfosuccinate(aerosol ot)solution[J].Journal of the American Chemical Society,1976,98(9):2391-2397.
[41]LI Quan,WENG Shi-fu,WU Jin-guang,ZHOU Nai-fu.Comparative study on structure of solubilized water in reversed micelles 1.FT-IRspectroscopic evidence of water/AOT/n-heptane and water/NaDEHP/n-heptane systems[J].Journal of Physical Chemistry B,1998,102(17):3168-3174.
[42]ANTONIO M R,CHIARIZIA R,GANNAZ B,BERTHON L,ZORZN,HILL C,COTE G.Aggregation in solvent extraction systems containing a malonamide,a dialkylphosphoric acid and their mixtures[J].Separation Science&Technology,2008,43(9-10):2572-2605.
[43]LAW S J,BRITTON M M.Sizing of reverse micelles in microemulsions using NMR measurements of diffusion[J].Langmuir,2012,28(32):11699-11706.
[44]SHINODA K,FRIBERG S.Microemulsions:colloidal aspects[J].Advances in Colloid&Interface Science,1975,4(4):281-300.
[45]KUNIEDA H,SHIGETA K,NAKAMURA K,IMAE T.Formation and structure of reverse vesicles[J].Progress in Colloid&Polymer Science,1996,100:1-5.
[46]SHARMA S C,SHRESTHA R G,SHRESTHA L K,ARAMAKI K.Viscoelastic wormlike micelles in mixed nonionic fluorocarbon surfactants and structural transition induced by oils[J].Journal of Physical Chemistry B,2009,113(6):1615-1622.
[47]SHRESTHA L K,SHRESTHA R G,ARAMAKI K.Intrinsic parameters for the structure control of nonionic reverse micelles in styrene:SAXS and rheometry studies[J].Langmuir,2011,27(10):5862-5873.
[48]SHRESTHA L K,SATO T,DULLE M,GLATTER O,ARAMAKI K.Effect of lipophilic tail architecture and solvent engineering on the structure of trehalose-based nonionic surfactant reverse micelles[J].Journal of Physical Chemistry B,2010,114(37):12008-12017.
[2]CHENG Chu-yong,BARNARD K R,ZHANG Wen-sheng,ROBINSON D J.Synergistic solvent extraction of nickel and cobalt:A review of recent developments[J].Solvent Extraction and Ion Exchange,2011,29(5-6):719-754.
[3]PRESTON J S,du PREEZ A C.Solvent extraction of nickel from acidic solutions using synergistic mixtures containing pyridinecarboxylate esters.Part 3.Systems based on arylsulphonic acids[J].Journal of Chemical Technology&Biotechnology,1998,71(1):43-50.
[4]PADILLA R,RUIZ M C,TRUJILLO W.Separation of liquid-liquid dispersions in a deep-layer gravity settler:Part I.Experimental study of the separation process[J].Hydrometallurgy,1996,42(2):267-279.
[5]HU Fang,HU Hui-ping,HU Jiu-gang,ZHU Shan,YANG Jin-peng,WANG Yon-xi.Improving selective separation of Cu(II)from acidic polymetallic media with 2-ethylhexyl 4-pyridinecarboxylate ester:Extraction behaviors,coordination structure and microscopic mechanism[J].Journal of Molecular Liquids,2017,248:1050-1058.
[6]LI Ji-yuan.Study on the extraction and mechanism of nickel in polymetallic solution by HDNNS/4PC[D].Changsha:Central South University,2017.(in Chinese)
[7]SUN Zhuo,PAN Yun-cong,JIANG Ji-mu.Design manual for heave non-ferrous metal smelting(copper-nickel volume)[M].Beijing:Metallurgical Industry Press,1996.(in Chinese)
[8]COUGHLIN R W,BERG R L V.Mass and heat transfer to drops in a mixer-settler[J].Chemical Engineering Science,1966,21(1):3-18.
[9]WANG Shu-chan,ZHANG Ting-an,ZHANG Zi-mu,LV Chao,ZHAO Qiu-yue,LIU Yan.Effect of stirring on oil-water separation in rare earth mixer-settler[J].China Petroleum Processing&Petrochemical Technology,2014,16(3):99-103.
[10]EL-RIFAI M A.Composition dynamics in multi-mixer-settler extractive reaction batteries[J].Chemical Engineering Science,1975,30(1):79-87.
[11]RYON A D,DALEY F L,LOWRIE R S.Design and scale up of mixer-settlers for the DAPEX solvent extraction process[R].Dapex Process,1960.
[12]PATHAK P N,KANEKAR A S,PRABHU D R,MANCHANDA VK.Comparison of hydrometallurgical parameters of N,N-dialkylamides and of tri-n-butylphosphate[J].Solvent Extraction&Ion Exchange,2009,27(5-6):683-694.
[13]LIU Xiao-rong,QIU Guan-zhou,HU Yue-hua,YANG Jun-he,JINMin-lin.Effect of Lix984N content on phase disengagement dynamics in copper-SX[J].Transactions of Nonferrous Metals Society of China,2003,13(4):963-967.
[14]LIU Yan-jun,LIU Xiao-rong,LI Hui,LI Qing,LI Yong-sheng,SUChang,TIAN Jun,WANG Yu-cheng.Effects of strong-acid on performances of copper solvent extraction[J].Advanced Materials Research,2014,881-883:48-51.
[15]ASENJO J A,MISTRY S L,ANDREWS B A,MERCHUK J C.Phase separation rates of aqueous two-phase systems:Correlation with system properties[J].Biotechnology&Bioengineering,2010,79(2):217-223.
[16]XUE Shu-yun,FU Xun,XIONG Ya-hong,ZHANG Shao-na,HUZheng-shui.Study on the thiophosphinic extractants.I.The basic properties of the extractants and the phase behavior in their saponified systems[J].Solvent Extraction and Ion Exchange,2002,20(3):331-344.
[17]MOVER B A,Mc DOWELL W J.Factors influencing phase disengagement rates in solvent extraction systems employing tertiary amine extractants[J].Separation Science,1981,16(9):1261-1289.
[18]NAKAMURA T,TERASHIMA H,MUKAI K.Emulsion formation and phase separation in some organic solvent-water systems[J].Shigen-to-Sozai,1992,108(11):812-816.
[19]BAILEY N T,MAHI P.The effect of diluents on the metal extracted and phase separation in the extraction of aluminium with monononyl phosphoric acid[J].Hydrometallurgy,1987,18:351-365.
[20]RAATZ S,KLAPPER P,REPKE J U.Micellar extraction of zinc using di(2-ethylhexyl)phosphorsure in presence of surfactant cetyltrimethyl ammonium bromide[J].Chemie Ingenieur Technik,2011,83(4):518-524.(in German)
[21]BARNEA E.Liquid-liquid contacting-art or science?Part I.Characterization of liquid-liquid system[J].Hydrometallurgy,1979,5:15-28.
[22]ZHU Shan,HU Hui-ping,HU Jiu-gang,LI Ji-yuan,HU Fang,WANG Yong-xi.Structural insights into the extraction mechanism of cobalt(II)with dinonylnaphthalene sulfonic acid and 2-ethylhexyl4-pyridinecarboxylate ester[J].Journal of coordination chemistry,2018,71(15):2441-2456.
[23]LI Ji-yuan,HU Hui-ping,ZHU Shan,HU Fang,WANG Yong-xi.The coordination structure of the extracted nickel(II)complex with a synergistic mixture containing dinonylnaphthalene sulfonic acid and2-ethylhexyl 4-pyridinecarboxylate ester[J].Dalton Transactions,2017,46:1075-1082.
[24]PRESTON J,PREEZ A D.The solvent extraction of nickel and cobalt bymixtures of carboxylic acids and pyridinecarboxylate esters[J].Solvent Extraction&Ion Exchange,1995,13(3):465-494.
[25]CHENG C Y,BARNARD K R,DAVIES M G.A study on the chemical stability of the Versatic 10-Acorga CLX50 synergistic system[J].Minerals Engineering,2002,15(12):1151-1161.
[26]ZHOU Li-ping,ZENG Xiao-qin,LI De-jiang,YANG Chun-ming.Ageing precipitation behavior of Mg-12Gd alloy[J].Chinese Journal of Nonferrous Metals,2015,25(6):1409-1416.(in Chinese)
[27]FRITZ G,BERGMANN A,GLATTER O.Evaluation of small-angle scattering data of charged particles using the generalized indirect Fourier transformation technique[J].Journal of Chemical Physics,2000,113(21):9733-9740.
[28]SALGI P,RAJAGOPALAN R.Polydispersity in colloids:Implications to static structure and scattering[J].Advances in Colloid&Interface Science,1993,43(2-3):169-288.
[29]PERCUS J K,YEVICK G J.Analysis of classical statistical mechanics by means of collective coordinates[J].Physical Review,1958,110:1-13.
[30]FRITZ G,GLATTER O.Structure and interaction in dense colloidal systems:evaluation of scattering data by the generalized indirect Fourier transformation method[J].Journal of Physics Condensed Matter,2006,18(36):S2403-S2419.
[31]NING Peng-ge,CAO Hong-bin,ZHANG Yi.Stability of the interfacial crud produced during the extraction of vanadium and chromium[J].Hydrometallurgy,2013,133(2):156-160.
[32]VIDYALAKSHMI V,SUBRAMANIAN M S,RAJESWARI S,SRINIVASAN T G,VASUDEVA RAO P R.Interfacial tension studies of N,N-dialkyl amides[J].Solvent Extraction&Ion Exchange,2003,21(3):399-412.
[33]RYDBERG J,COX M,MUSIKAS C,CHOPPIN G R.Solvent extraction principles and practice[M].2nd ed.Boca Raton:CRCPress,2004.
[34]GONG Xing-chu,LV Yang-cheng,LI Mu,MA Xue-feng,NIQian-yin LUO Guang-sheng.Selection and evaluation of a new extractant for caprolactam extraction[J].Chinese Journal of Chemical Engineering,2008,16(6):876-880.
[35]ALBERTS E,DORFLING C.Stripping conditions to prevent the accumulation of rare earth elements and iron on the organic phase in the solvent extraction circuit at skorpion zinc[J].Minerals Engineering,2013,40(40):48-55.
[36]MUSADAIDZWA J M,TSHININGAYAMWE E I.Skorpion zinc solvent extraction:The upset conditions[J].Journal of the Southern African Institute of Mining&Metallurgy,2009,109:691-695.
[37]TESTARD F,BAUDUIN P,ZEMB T,BERTHON L.Third-phase formation in liquid/liquid extraction:A colloidal approach[M].Boca Raton,FL and London:CRC Press,Taylor&Francis Group,2010.
[38]CHIARIZIA R,DANESI P R,D'ALESSANDRO G,SCUPPAR B.Interfacial behaviour of dinonylnaphthalenesulfonic acid at the toluene-HCl O4 interface[J].Journal of Inorganic&Nuclear Chemistry,1976,38(7):1367-1369.
[39]OSSEO-ASARE K,KEENEY M E.Aspects of the interfacial chemistry of nickel extraction with LIX63-HDNNS mixtures[J].Metallurgical and Materials Transactions B,1980,11:63-67.
[40]WONG M,THOMAS J K,GRAETZEL M.Fluorescence probing of inverted micelles.The state of solubilized water clusters in alkane diisooctyl sulfosuccinate(aerosol ot)solution[J].Journal of the American Chemical Society,1976,98(9):2391-2397.
[41]LI Quan,WENG Shi-fu,WU Jin-guang,ZHOU Nai-fu.Comparative study on structure of solubilized water in reversed micelles 1.FT-IRspectroscopic evidence of water/AOT/n-heptane and water/NaDEHP/n-heptane systems[J].Journal of Physical Chemistry B,1998,102(17):3168-3174.
[42]ANTONIO M R,CHIARIZIA R,GANNAZ B,BERTHON L,ZORZN,HILL C,COTE G.Aggregation in solvent extraction systems containing a malonamide,a dialkylphosphoric acid and their mixtures[J].Separation Science&Technology,2008,43(9-10):2572-2605.
[43]LAW S J,BRITTON M M.Sizing of reverse micelles in microemulsions using NMR measurements of diffusion[J].Langmuir,2012,28(32):11699-11706.
[44]SHINODA K,FRIBERG S.Microemulsions:colloidal aspects[J].Advances in Colloid&Interface Science,1975,4(4):281-300.
[45]KUNIEDA H,SHIGETA K,NAKAMURA K,IMAE T.Formation and structure of reverse vesicles[J].Progress in Colloid&Polymer Science,1996,100:1-5.
[46]SHARMA S C,SHRESTHA R G,SHRESTHA L K,ARAMAKI K.Viscoelastic wormlike micelles in mixed nonionic fluorocarbon surfactants and structural transition induced by oils[J].Journal of Physical Chemistry B,2009,113(6):1615-1622.
[47]SHRESTHA L K,SHRESTHA R G,ARAMAKI K.Intrinsic parameters for the structure control of nonionic reverse micelles in styrene:SAXS and rheometry studies[J].Langmuir,2011,27(10):5862-5873.
[48]SHRESTHA L K,SATO T,DULLE M,GLATTER O,ARAMAKI K.Effect of lipophilic tail architecture and solvent engineering on the structure of trehalose-based nonionic surfactant reverse micelles[J].Journal of Physical Chemistry B,2010,114(37):12008-12017.
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