氨性溶液中铜、镍、锌金属离子的萃取行为及微观机理研究
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摘要
立足于解决国内紧缺战略有色金属矿产资源高效利用的难题,开发适合低品位矿、尾矿等非传统矿物的技术和工艺流程是我国有色冶金工业发展的重要方向。在众多的冶炼技术中,“氨浸—萃取—电积”工艺是处理低品位复杂氧化矿物最具前景的技术之一,萃取工序是该技术中最关键的步骤。因此,清楚掌握萃取过程的机理对改进萃取剂配方、设计萃取工艺流程具有重要意义。
本文以铜、镍、锌金属为研究对象,以实验室合成的1-苯基-4-乙基-1,3-辛二酮(HA)为萃取剂,从萃取平衡和溶液结构两个方面,系统研究了氨-硫酸铵溶液中铜、镍、锌金属离子的萃取行为,分析了水和氨在萃取有机相中的分配规律,结合紫外-可见光谱(UV-Vis)、红外光谱(FT-IR)和X-射线近边吸收光谱(XANES)和扩展X-射线精细结构光谱(EXAFS)等方法研究了水相及有机相中的物种及其微观结构对萃取过程的影响,阐明了氨性溶液中铜、镍、锌金属离子的微观萃取机理,为低品位复杂氧化矿物氨配合冶金体系的建立提供了可靠的理论依据。
具体研究内容及结论如下：
(1)系统研究了氨性溶液中铜离子的萃取行为和微观机理。发现1-苯基-4-乙基-1,3-辛二酮在氨性体系可高效萃取铜离子,水相中铜氨配位离子的生成会抑制铜萃取反应,当pH>8.5时铜萃取率显著下降；萃取有机相中水分子不与铜萃合物配位,而少量氨分子可随铜萃合物萃取进入有机相；p-二酮与铜离子主要形成平面四边形构型的CuA2萃合物,其结构不受水相pH的影响；随着pH升高,氨性溶液中铜离子的结构从变形八面体构型逐渐转变为扭曲的平面四边形构型,从而抑制了铜离子的萃取,导致高pH下铜萃取率急剧下降。
(2)系统研究了氨性溶液中镍离子的萃取行为和微观机理。发现氨性溶液pH对镍离子的萃取具有明显影响,镍萃取率在pH<8.5时随pH升高而增大,但在8.59.5时开始显著升高；水分子和氨分子可与镍萃合物配位进入有机相,生成的水合及氨配位镍萃合物降低了萃合物在非极性溶剂中的溶解度,从而抑制了镍离子的萃取；当水相pH>9.5时有机相析出绿色的萃合物晶体,有效降低了非有机相中镍萃合物的浓度,从而促进了镍离子的萃取反应,但该萃取行为不利于工业实际应用；有机相中镍萃合物组成为NiA2·H2O·NH3,萃合物在有机相中的结构与萃取法制备的镍萃合物结构相同,均为八面体构型。在镍氨溶液中,随着pH的增大,氨分子逐级取代镍离子中的水分子,形成各种稳定的镍氨物种,虽然其配位结构均为八面体构型,但镍氨物种的稳定性逐渐增大,尤其是Ni(NH3)52+和Ni(NH3)62+的生成显著抑制了萃取反应的进行。(3)系统研究了氨性溶液中锌离子的萃取行为和微观萃取机理。结果表明,氨性体系锌离子的萃取平衡对水相pH非常敏感,尤其是在pH>7.35时锌萃取率急剧降低,在pH>9时基本没有萃锌能力；水分子和氨分子可直接与锌萃合物配位,形成水合及氨配位的锌萃合物,增大水相pH可促进氨配位锌萃合物的生成；有机相中锌离子主要为四面体构型的ZnA2萃合物,水分子和氨分子与部分ZnA2生成五配位ZnA2·H2O和ZnA2·NH3;水相中氨分子逐级取代水合锌离子的水分子,形成各种稳定的锌氨配位离子,抑制了锌离子的萃取反应；当第三个氨分子与锌离子配位后,使锌离子从八面体构型转变为更稳定四面体构型,导致高pH下锌萃取率急剧降低。
(4)以正辛醇、甲苯和壬烷为溶剂,研究了氨性体系锌离子萃取过程中的溶剂效应。发现增大溶剂极性可显著提高氨性溶液中锌离子的萃取率,萃锌性能正辛醇>甲苯≈壬烷,疏水性较低的水合和氨配位锌萃合物在极性溶剂中更易溶解,从而促进了锌离子的萃取,但辛醇体系中锌离子的萃取率在pH>7.3时仍急剧下降,表明增大溶剂极性仍难以促进四面体构型锌氨离子的萃取。
(5)以三辛基氧膦(TOPO)、磷酸三丁酯(TBP)和三丁基膦(TBuP)三种含磷中性配体(B)为协萃剂,研究了氨性体系锌离子萃取过程中的协同效应。发现加入协萃剂可显著提高氨性溶液中锌的萃取率,萃锌性能TOPO>TbuP>TBP,且TOPO和TBuP体系在7.26 (6)以1-丁基-3-甲基咪唑六氟磷酸盐([BMIM]PF6)、1-辛基-3-甲基咪唑六氟磷酸盐([OMIM]PF6)、1-丁基-3-甲基咪唑双三氟甲磺酰亚胺盐([BMIM]NTf2)、口1-辛基-3-甲基咪唑双三氟甲磺酰亚胺盐([OMIM]NTf2)等四种离子液体为溶剂,首次研究了离子液体萃取体系从氨性溶液中萃取锌离子的行为。结果表明,p-二酮与疏水性离子液体萃取体系可用于氨性溶液中锌离子的萃取,萃锌性能[BMIM]PF6>[BMIM]NTf2>[OMIM]PF6>[OMIM]NTf2,极性较强的离子液体有利于锌离子的萃取。在四种离子液体中,锌萃合物主要以五配位结构存在；强极性离子液体的离子组分可能与锌萃合物外配位层相互作用,从而增强了萃合物的稳定性,促进了锌离子的萃取。
The development of new technologies used for high efficient extraction of non-traditional ores, which include low grade ore, tailings, and drosses etc., is an urgent target in order to solve the shortage problem of strategic non-ferrous metal resources in china. Among many metallurgical methods, the "ammoniacal leaching—solvent extraction—acidic electrowinning"(AL-SX-AE) is one of the most promising technologies used to treat the low-grade complex oxide minerals. And solvent extraction is the most key process in this technology. Therefore, the detailed insights into the extraction mechanism are essential to optimize extractant formula and design the extraction process.
In this paper, the home-made β-diketone extractant,1-phenyl-4-ethyl-1,3-octanedione (denote as HA), was used to extract copper(II), nickel(II) and zinc(II) from ammonia-ammoniacal sulfate solution. The distribution behavior of water and ammonia in the organic phase has been studied in the absence and presence of metal ions. The coordination structure of the species in both aqueous and organic phases was characterized by using of UV-Vis spectroscopy, FT-IR spectroscopy, X-ray absorption near edge structure spectroscopy (XANES) and extended X-ray absorption fine structure (EXAFS) spectroscopy. The extraction mechanism has been elucidated in view of the extraction equilibrium and structural characteristics of species in both phases. The obtained data are helpful for the development and application of "AL-SX-AE" technology.
1. The extraction behavior and microscopic mechanism of Cu(II) in ammonia-ammoniacal sulfate solution have been investigated.
It was found that the1-phenyl-4-ethyl-1,3-octanedione is a superior extractant for Cu(II) in ammoniacal solution. The formation of copper ammonia complexes inhibits the extraction reaction of Cu(II), resulting in that the extraction efficiency decreases sharply at pH>8.5. Water molecules can not be coordinated with copper extracts in the organic phase, but a small amount of ammonia molecules can be co-extracted into organic phase with copper extracts. The extracted copper complexes (CuA2) are four coordinate structure with a square planar configuration, which is independent of the aqueous pH. However, as the pH increases, the coordination structure of copper ions in ammoniacal solution can be gradually transformed from a six-coordinated octahedral geometry into a distorted square planar configuration, which is the essential reason why the extraction efficiency of copper(Ⅱ) decreases.
2. The extraction behavior and microscopic mechanism of nickel(Ⅱ) in ammonia-ammoniacal sulfate solution have been investigated.
It was found that the extraction behavior of nickel(Ⅱ) is strongly dependent on the aqueous pH. When the pH is lower than8.5, the extraction efficiency of nickel(Ⅱ) increases with the increase of pH, but decreases at8.59.5, which should be the essential reason why the extraction efficiency of nickel dramatically increases when pH is larger than9.5. This extraction behavior of Ni(Ⅱ) is unfavorable for the industrial practical application. The composition of soild nickel extracts is NiA2·H2O·NH3and the coordination structure is identified with an octahedral configuration. The structure of nickel extracts in organic phase is identical to that of the solid extracts. In aqueous phase, ammonia molecule will substitute successive-ly water molecule of Ni(Ⅱ) to form more stable nickel ammonia species with an octahedral configuration, thus inhabiting the extraction reaction of Ni(Ⅱ). Especially, the formation of Ni(NH3)52+and Ni(NH3)62+decreases the extraction efficiency of nickel significantly.
3. The extraction behavior and microscopic mechanism of zinc(Ⅱ) in ammonia-ammoniacal sulfate solution have been investigated.
It was found that the extraction equilibrium of zinc is very sensitive to the aqueous pH. Especially, the extraction efficiency of zinc decreases sharply when pH is larger than7.35. Water and ammonia molecules can be co-extracted into organic phase by coordinated with zinc extracts. Thus, several equilibrium species could co-exist in the organic phase, i.e, ZnA2, hydrated ZnA2and ammonia-solvated ZnA2. The resulting hydrated and ammonia-coordinated zinc extracts have higher hydrophilicity, thereby depressing the distribution of the extracted zinc complexes in a non-polar hydrocarbon solvent. The coordination structure of ZnA2is identified with a tetrahedral geometry. The hydrated ZnA2and ammonia-coordinated ZnA2are penta-coordinate structure. In the ammoniacal solution, as the pH increases, ammonia molecule will substitute successively water molecule of zinc ion to form more stable zinc ammonia species. The coordination structure of zinc ions can be gradually transformed from a six-coordinated octahedral geometry into a four-coordinated tetrahedral configuration, thus the extraction efficiency of zinc will be sharply decreased at pH>7.35.
4. The solvent effect on the extraction of zinc(Ⅱ) in ammoniacal solution has been investigated with n-octanol, toluene, and nonane as solvents.
It was found that the increase of polarity of the solvent can promote the extraction reaction of zinc(Ⅱ) in ammoniacal solution. However, the extraction efficiency of zinc in octanol system still decreases sharply at pH>7.3. And the concentration of water and ammonia in octanol system dramatically increases with the increase of zinc concentration. The strong solvent effect in octanol system could be attributed to the role of hydrogen bonding between zinc extracts and octanol molecules, and the distribution of hydrated ZnA2and ammonia-solvated ZnA2into polar solvent can be improved. The zinc extract is a penta-coordinate structure.
5. The synergistic effect on the extraction of zinc(Ⅱ) in ammoniacal solution has been investigated with tributyl phosphate (TBP), trioctyl-phosphine oxide (TOPO) and tributylphosphane (TBuP) as synergists.
It was found that the addition of neutral phosphorus-containing ligands (denote as B) can significantly promote the extraction reaction of zinc(Ⅱ) in ammoniacal solution. And the extraction performance is stable at7.26 6. The extraction behavior of zinc(Ⅱ) from ammoniacal solution into four hydrophobic ionic liquids ([OMIM]PF6,[BMIM]PF6,[BMIM]NTf2and [OMIM]NTf2) was investigated with HA as the extractant.
It was found that hydrophobic ILs combined with HA can be used to extract zinc(Ⅱ) from ammoniacal solutions. The extraction behavior of zinc(Ⅱ) is dependent on the zinc species in ammoniacal solutions and the hydrophobicity of ILs. The extraction efficiency of zinc decreases in the order of [BMIM]PF6>[BMIM]NTf2>[OMIM]PF6>[OMIM]NTf2. The zinc extract in four ionic liquids is mainly the penta-coordinated structure, and the average coordination number of the zinc extracts decreases with the increase of the hydrophobicity of the ILs. The good extraction performance of [BMIM]PF6system can be attributed to the interaction between zinc extracts with ionic components of the ionic liquid.
本文以铜、镍、锌金属为研究对象,以实验室合成的1-苯基-4-乙基-1,3-辛二酮(HA)为萃取剂,从萃取平衡和溶液结构两个方面,系统研究了氨-硫酸铵溶液中铜、镍、锌金属离子的萃取行为,分析了水和氨在萃取有机相中的分配规律,结合紫外-可见光谱(UV-Vis)、红外光谱(FT-IR)和X-射线近边吸收光谱(XANES)和扩展X-射线精细结构光谱(EXAFS)等方法研究了水相及有机相中的物种及其微观结构对萃取过程的影响,阐明了氨性溶液中铜、镍、锌金属离子的微观萃取机理,为低品位复杂氧化矿物氨配合冶金体系的建立提供了可靠的理论依据。
具体研究内容及结论如下：
(1)系统研究了氨性溶液中铜离子的萃取行为和微观机理。发现1-苯基-4-乙基-1,3-辛二酮在氨性体系可高效萃取铜离子,水相中铜氨配位离子的生成会抑制铜萃取反应,当pH>8.5时铜萃取率显著下降；萃取有机相中水分子不与铜萃合物配位,而少量氨分子可随铜萃合物萃取进入有机相；p-二酮与铜离子主要形成平面四边形构型的CuA2萃合物,其结构不受水相pH的影响；随着pH升高,氨性溶液中铜离子的结构从变形八面体构型逐渐转变为扭曲的平面四边形构型,从而抑制了铜离子的萃取,导致高pH下铜萃取率急剧下降。
(2)系统研究了氨性溶液中镍离子的萃取行为和微观机理。发现氨性溶液pH对镍离子的萃取具有明显影响,镍萃取率在pH<8.5时随pH升高而增大,但在8.5
(4)以正辛醇、甲苯和壬烷为溶剂,研究了氨性体系锌离子萃取过程中的溶剂效应。发现增大溶剂极性可显著提高氨性溶液中锌离子的萃取率,萃锌性能正辛醇>甲苯≈壬烷,疏水性较低的水合和氨配位锌萃合物在极性溶剂中更易溶解,从而促进了锌离子的萃取,但辛醇体系中锌离子的萃取率在pH>7.3时仍急剧下降,表明增大溶剂极性仍难以促进四面体构型锌氨离子的萃取。
(5)以三辛基氧膦(TOPO)、磷酸三丁酯(TBP)和三丁基膦(TBuP)三种含磷中性配体(B)为协萃剂,研究了氨性体系锌离子萃取过程中的协同效应。发现加入协萃剂可显著提高氨性溶液中锌的萃取率,萃锌性能TOPO>TbuP>TBP,且TOPO和TBuP体系在7.26
The development of new technologies used for high efficient extraction of non-traditional ores, which include low grade ore, tailings, and drosses etc., is an urgent target in order to solve the shortage problem of strategic non-ferrous metal resources in china. Among many metallurgical methods, the "ammoniacal leaching—solvent extraction—acidic electrowinning"(AL-SX-AE) is one of the most promising technologies used to treat the low-grade complex oxide minerals. And solvent extraction is the most key process in this technology. Therefore, the detailed insights into the extraction mechanism are essential to optimize extractant formula and design the extraction process.
In this paper, the home-made β-diketone extractant,1-phenyl-4-ethyl-1,3-octanedione (denote as HA), was used to extract copper(II), nickel(II) and zinc(II) from ammonia-ammoniacal sulfate solution. The distribution behavior of water and ammonia in the organic phase has been studied in the absence and presence of metal ions. The coordination structure of the species in both aqueous and organic phases was characterized by using of UV-Vis spectroscopy, FT-IR spectroscopy, X-ray absorption near edge structure spectroscopy (XANES) and extended X-ray absorption fine structure (EXAFS) spectroscopy. The extraction mechanism has been elucidated in view of the extraction equilibrium and structural characteristics of species in both phases. The obtained data are helpful for the development and application of "AL-SX-AE" technology.
1. The extraction behavior and microscopic mechanism of Cu(II) in ammonia-ammoniacal sulfate solution have been investigated.
It was found that the1-phenyl-4-ethyl-1,3-octanedione is a superior extractant for Cu(II) in ammoniacal solution. The formation of copper ammonia complexes inhibits the extraction reaction of Cu(II), resulting in that the extraction efficiency decreases sharply at pH>8.5. Water molecules can not be coordinated with copper extracts in the organic phase, but a small amount of ammonia molecules can be co-extracted into organic phase with copper extracts. The extracted copper complexes (CuA2) are four coordinate structure with a square planar configuration, which is independent of the aqueous pH. However, as the pH increases, the coordination structure of copper ions in ammoniacal solution can be gradually transformed from a six-coordinated octahedral geometry into a distorted square planar configuration, which is the essential reason why the extraction efficiency of copper(Ⅱ) decreases.
2. The extraction behavior and microscopic mechanism of nickel(Ⅱ) in ammonia-ammoniacal sulfate solution have been investigated.
It was found that the extraction behavior of nickel(Ⅱ) is strongly dependent on the aqueous pH. When the pH is lower than8.5, the extraction efficiency of nickel(Ⅱ) increases with the increase of pH, but decreases at8.5
3. The extraction behavior and microscopic mechanism of zinc(Ⅱ) in ammonia-ammoniacal sulfate solution have been investigated.
It was found that the extraction equilibrium of zinc is very sensitive to the aqueous pH. Especially, the extraction efficiency of zinc decreases sharply when pH is larger than7.35. Water and ammonia molecules can be co-extracted into organic phase by coordinated with zinc extracts. Thus, several equilibrium species could co-exist in the organic phase, i.e, ZnA2, hydrated ZnA2and ammonia-solvated ZnA2. The resulting hydrated and ammonia-coordinated zinc extracts have higher hydrophilicity, thereby depressing the distribution of the extracted zinc complexes in a non-polar hydrocarbon solvent. The coordination structure of ZnA2is identified with a tetrahedral geometry. The hydrated ZnA2and ammonia-coordinated ZnA2are penta-coordinate structure. In the ammoniacal solution, as the pH increases, ammonia molecule will substitute successively water molecule of zinc ion to form more stable zinc ammonia species. The coordination structure of zinc ions can be gradually transformed from a six-coordinated octahedral geometry into a four-coordinated tetrahedral configuration, thus the extraction efficiency of zinc will be sharply decreased at pH>7.35.
4. The solvent effect on the extraction of zinc(Ⅱ) in ammoniacal solution has been investigated with n-octanol, toluene, and nonane as solvents.
It was found that the increase of polarity of the solvent can promote the extraction reaction of zinc(Ⅱ) in ammoniacal solution. However, the extraction efficiency of zinc in octanol system still decreases sharply at pH>7.3. And the concentration of water and ammonia in octanol system dramatically increases with the increase of zinc concentration. The strong solvent effect in octanol system could be attributed to the role of hydrogen bonding between zinc extracts and octanol molecules, and the distribution of hydrated ZnA2and ammonia-solvated ZnA2into polar solvent can be improved. The zinc extract is a penta-coordinate structure.
5. The synergistic effect on the extraction of zinc(Ⅱ) in ammoniacal solution has been investigated with tributyl phosphate (TBP), trioctyl-phosphine oxide (TOPO) and tributylphosphane (TBuP) as synergists.
It was found that the addition of neutral phosphorus-containing ligands (denote as B) can significantly promote the extraction reaction of zinc(Ⅱ) in ammoniacal solution. And the extraction performance is stable at7.26
It was found that hydrophobic ILs combined with HA can be used to extract zinc(Ⅱ) from ammoniacal solutions. The extraction behavior of zinc(Ⅱ) is dependent on the zinc species in ammoniacal solutions and the hydrophobicity of ILs. The extraction efficiency of zinc decreases in the order of [BMIM]PF6>[BMIM]NTf2>[OMIM]PF6>[OMIM]NTf2. The zinc extract in four ionic liquids is mainly the penta-coordinated structure, and the average coordination number of the zinc extracts decreases with the increase of the hydrophobicity of the ILs. The good extraction performance of [BMIM]PF6system can be attributed to the interaction between zinc extracts with ionic components of the ionic liquid.
引文
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