CN105861827B - A kind of soda acid coupling extraction system separated for many metal solution extractions and its application - Google Patents

A kind of soda acid coupling extraction system separated for many metal solution extractions and its application Download PDF

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CN105861827B
CN105861827B CN201610219087.0A CN201610219087A CN105861827B CN 105861827 B CN105861827 B CN 105861827B CN 201610219087 A CN201610219087 A CN 201610219087A CN 105861827 B CN105861827 B CN 105861827B
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extractant
extraction system
soda acid
acid
solutions
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CN105861827A (en
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胡久刚
付明波
李娅
汤佳
刘士军
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Central South University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/26Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
    • C22B3/40Mixtures
    • C22B3/402Mixtures of acyclic or carbocyclic compounds of different types
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B19/00Obtaining zinc or zinc oxide
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00Obtaining nickel or cobalt
    • C22B23/04Obtaining nickel or cobalt by wet processes
    • C22B23/0453Treatment or purification of solutions, e.g. obtained by leaching
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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Abstract

Extraction system and its application are coupled the invention discloses a kind of soda acid for multi-metal complex solution extract and separate;Soda acid coupling extraction system includes the extractant and diluent being made up of basic extractant and acidic extractant;Synergy in soda acid coupling extraction system between each extractant component is obvious, basic extractant can substantially suppress extraction of the acidic extractant to part metals ion, so as to promote efficiently separating between various metals in many metallic solutions, the separative efficiency to similar metals elements such as Zn/Cu, Ni/Co or Cu/Ni in various complicated solutions is remarkably improved tens to hundred times;And extractant cost used is low, extraction process is ripe, it is easy to popularization and application.

Description

A kind of soda acid coupling extraction system separated for many metal solution extractions and its application
Technical field
It is used to promote the soda acid of many metal solution extraction separation to couple extraction system, Yi Jisuo present invention relates particularly to a kind of State soda acid and couple application of the extraction system in many metallic solutions in metal extraction separation;Belong to the solvent extraction point of non-ferrous metal From technical field.
Background technology
Significant portion is non-traditional unmanageable resource, bag in the strategic nonferrous metal resource in short supply such as China's nickel, cobalt, copper, zinc Include the mine tailing, waste residue and the barren rock that are produced during various low-grade complex ore deposits, oxide ore, selecting and purchasing smelting, pelagite resource etc.. The common association of many metals is the main feature of the strategic nonferrous metal resource in short supply such as China's nickel, cobalt, copper, zinc, explored mineral products money Difficult choosing, the low grade oxidation ore of difficult smelting and multi-metal complex ore deposit account for more than 60% in source, many metal symbiosis vulcanization cupro-nickels in such as Jinchuan Ore deposit, copper zinc oxidation of sulfureted composite ore of Lanping, yunnan Province etc., have the same phase of class matter, the features such as basic gangue content is high, metal is comprehensive more Close utilization rate low.Hydrometallurgical technology is widely used in the comprehensive utilization ratio for improving associated resources altogether;Wherein, multi-metal complex solution Efficiently separating for middle valuable metal is the key for realizing associated resources comprehensive utilization altogether.
Solvent extraction is a kind of efficient metal isolation technics, and body extraction, the rare earth member of nuclear fuel are widely used at present The separation of element and the extraction of non-ferrous metal.In recent years, the exploitation for the efficient extractant of each metal ion species is abstraction technique Solid foundation has been established in extensive use in non-ferrous metal hydrometallurgy, and nickel, the success of copper hydrometallurgy are greatly promoted Development of the abstraction technique in non-ferrous metal hydrometallurgy.However, because the exploitation of Novel Extractant is very expensive, time-consuming, The market unsettled of product, causes the enthusiasm of extractant manufacturer research and development new extractant both domestic and external not high, in face of increasingly Complicated many metallic solution systems, it is difficult to find the special efficacy extraction system of suitable various solution.
Some research and practice have shown that, using existing business extractant constitute hybrid extraction system, can obviously improve extraction The thermodynamics and kineticses performance of system, increases distribution ratio, improves extraction saturated capacity, realizes the efficient of metal ion in solution Extraction, such as Wei Zhicong is mixed using 2- hydroxyls -5- nonyls benzaldoxime with neutral organic compound containing phosphine can effectively improve ammonia Property solution in extraction (CN103710547A), the Chen Qiyuan etc. of zinc mixed using high steric-hindrance amino beta-diketon with organic hydroxyl oxime compound Promote the extraction (CN101560601A) of zinc in ammonia solution;Part business extractant is also to use two or more extractant groups Into such as LIX64N (LIX65N+LIX63), LIX973 (LIX84+LIX860), LIX984 (LIX860+LIX84).However, existing Mainly it is made up of hybrid extraction system by acidic extractant with acidity or with Neutral-neutral Extractants, although metal ion can be effectively improved Extraction behavior, but each component of extractant is generally respectively provided with extracting power to many kinds of metal ions in complicated solution, it is difficult to Realize efficiently separating for metal ion.Interacted by adding other components with extractant, so as to reduce extractant to part The extracting power of metal ion, is a kind of new approaches of promotion multi-metal complex solution extract and separate.
The content of the invention
For the present situation of complex multi-metal solution extract and separate, first purpose of the invention is to be to provide a kind of extraction The soda acid that agent is made up of basic extractant and acidic extractant couples extraction system, and its extracting power is adjustable, it is adaptable to many metals Various metal efficient selectives separation in solution.
Another object of the present invention is to be to provide the application that the soda acid couples extraction system, is applied to and includes The extract and separate of each metal ion species in many metallic solutions such as copper, cobalt, nickel, zinc, with selective extraction separating effect, is especially fitted Selective Separation for Zn/Cu, Ni/Co or Cu/Ni in many metallic solutions.
In order to realize above-mentioned technical purpose, the invention provides a kind of soda acid coupling separated for many metal solution extractions Extraction system, comprising extractant and diluent, described extractant is made up of basic extractant and acidic extractant.
It is preferred that scheme, extractant neutral and alkali extractant and acidic extractant mol ratio are 1~9:1~5, according to be separated Species of metal ion and selection different extractants combination, can be to basic extractant and the molar ratio of acidic extractant Appropriate regulation is carried out within the range.
More preferably scheme, basic extractant is tri-n-octyl methyl ammonium chloride, three hexyl myristyl phosphonium chlorides, three just pungent Base phosphine oxide, tributyl phosphate, three (2- ethylhexyls) at least one of phosphates and trioctylamine.Tri-n-octyl methyl ammonium chloride (trade name Aliquat336), three hexyl myristyl phosphonium chlorides (trade name Cyphos IL101) etc. are strong basicity extractant; It is trioctylphosphine (trade name Cyanex923), tributyl phosphate (TBP), three (2- ethylhexyls) phosphates (TEHP), three pungent Amine (TOA) etc. is lewis base extractant.
More preferably scheme, acidic extractant is that double (2- ethylhexyls) phosphates, two (2,4,4- tri-methyl-amyls) are secondary In phosphoric acid, two (2,4,4- tri-methyl-amyls) phosphonic acids, 1- phenyl -1,3- last of the ten Heavenly stems diketone and 2- hydroxyl -5- nonylacetophenone oximes extremely Few one kind.Double (2- ethylhexyls) phosphates (trade name D2EHPA), two (2,4,4- tri-methyl-amyls) hypophosphorous acid (trade names Cyanex272), two (2,4,4- tri-methyl-amyls) phosphonic acids (trade name Cyanex302) etc. are highly acid extractant.1- phenyl- 1,3- last of the ten Heavenly stems diketone (trade name LIX54), 2- hydroxyl -5- nonylacetophenone oximes (trade name LIX84) etc. extract for faintly acid (chelating) Take agent.
It is preferred that scheme, diluent is sulfonated kerosene.
, should by described soda acid coupling extraction system present invention also offers the application that described soda acid couples extraction system To contain the selective extraction separation of target metal ions in the two or more many metallic solutions of copper, cobalt, nickel, zinc.
It is preferred that scheme, in the soda acid coupling extraction system concentration of extractant be in many metallic solutions metal target from 10~60 times of sub- concentration.
It is preferred that scheme, target metal ions be copper, cobalt, nickel and zinc in one kind, two or three.
It is preferred that scheme, many metallic solutions be pH<5 Zn/Cu mixing sulfuric acid solutions, or be the Ni/Co that pH is 6~10 Ammonia solution, or be the Cu/Ni ammonia solutions that pH is 7~10.
It is preferred that scheme, various concentration of metal ions are respectively 0.1~3g/L in many metallic solutions.
More preferably scheme, using containing double (2- ethylhexyls) phosphates and three hexyl myristyl phosphonium chlorides and/or three The soda acid coupling extraction system of octylmethylammonium chloride, is separated for the Zn in Zn/Cu mixing sulfuric acid solutions and Cu.It is further excellent The scheme of choosing, extraction system is coupled using containing double (2- ethylhexyls) phosphates with the soda acid of three hexyl myristyl phosphonium chlorides, For the separation of Zn and Cu in pH=4 Zn/Cu mixing sulfuric acid solutions, Zn/Cu separations up to 1748.4, wherein, double (2- second Base hexyl) mol ratios of phosphate and three hexyl myristyl phosphonium chlorides is 3/7.Further preferred scheme, using containing double (2- Ethylhexyl) phosphate couples extraction system with the soda acid of tri-n-octyl methyl ammonium chloride, the Zn/Cu mixing sulfuric acid for pH=4 Zn and Cu separation in solution, Zn/Cu separations up to 1211.3, wherein, double (2- ethylhexyls) phosphates and trioctylphosphine first The mol ratio of ammonium chloride is 1/9.
More preferably scheme, using containing two (2,4,4- tri-methyl-amyl) hypophosphorous acid and three hexyl myristyl phosphonium chlorides And/or the soda acid coupling extraction system of trioctylamine, the separation for Ni and Co in Ni/Co mixing ammonia solutions.Further preferably Scheme, couple extractor body with the soda acid of three hexyl myristyl phosphonium chlorides using containing two (2,4,4- tri-methyl-amyl) hypophosphorous acid System, for the separation of Ni and Co in pH=8.2 Ni/Co mixing ammonia solutions, Ni/Co separations up to 150.28, wherein, two The mol ratio of (2,4,4- tri-methyl-amyls) hypophosphorous acid and three hexyl myristyl phosphonium chlorides is 3/7.Further preferred scheme, Extraction system is coupled with the soda acid of trioctylamine using containing two (2,4,4- tri-methyl-amyl) hypophosphorous acid, the Ni/Co for pH=8.2 Mix ammonia solution in Ni and Co separation, Ni/Co separations up to 70.08, wherein, two (2,4,4- tri-methyl-amyl) secondary phosphorus The mol ratio of acid and trioctylamine is 1/9.
More preferably scheme, using phenyl containing 1- -1,3- last of the ten Heavenly stems diketone and trioctylphosphine and/or three (2- ethylhexyls) The soda acid coupling extraction system of phosphate, the separation for Cu and Ni in Cu/Ni mixing ammonia solutions.Further preferred side Case, couples extraction system, for pH=9.5's using-the 5- of hydroxyl containing 2- nonylacetophenone oximes with the soda acid of trioctylphosphine Cu and Ni separation in Cu/Ni mixing ammonia solutions, Cu/Ni separations up to 384.59, wherein, 2- hydroxyl -5- nonyl benzene second The mol ratio of ketoxime and trioctylphosphine is 4/1.Further preferred scheme the, using -5- nonylacetophenone oximes of hydroxyl containing 2- Couple extraction system with the soda acid of three (2- ethylhexyls) phosphates, for Cu in pH=9.5 Cu/Ni mixing ammonia solutions and Ni separation, Cu/Ni separations up to 401.89, wherein, 2- hydroxyl -5- nonylacetophenone oximes and three (2- ethylhexyls) phosphoric acid The mol ratio of ester is 4/1.
The extraction separating method of the present invention, extraction separating method routinely is implemented:By basic extractant and acid extract After agent mixing, dilution dilution agent is added, soda acid is coupled extraction system by composition soda acid coupling extraction system (extracting organic phase) Mixed with many metallic solutions, carry out liquid-liquid extraction, object element, which is optionally extracted, enters organic phase, so as to realize valuable metal Separation.
Technical scheme based on principle be:For specific multi-metal complex solution, existing conventional acidity (or chelating) extractant is generally respectively provided with Coordination Adsorption ability to various metals, so being difficult to obtain effective using single extractant Metal separating capacity.And technical solution of the present invention, the introducing portion basic extractant in acidic extractant system, alkaline extraction Electrostatic attraction, hydrogen bond and Van der Waals force between agent and acidic extractant etc. interact, and can suppress acidic extractant to portion Divide the coordination ability of metal ion, so as to be effectively facilitated the separation of multi-metal complex solution;Also, by adjusting hybrid extraction Agent constitutes controllable extract and separate ability.
Compared with the prior art, the technical advantage that technical scheme is brought:
(1) synergy between soda acid of the invention coupling each extractant component of extraction system is obvious, basic extractant Extraction of the acidic extractant to part metals ion can substantially be suppressed, so as to promote the height in many metallic solutions between various metals Effect separation, the separative efficiency to the similar metals element such as Zn/Cu, Ni/Co or Cu/Ni is remarkably improved tens to hundred times, is To the useful supplement of conventional hybrid extraction system.
(2) soda acid of the invention coupling extraction system is easy to by adjusting the ratio between acidic extractant and basic extractant Example relation adjusts the extract and separate ability belonged to complex multi-metal GOLD FROM PLATING SOLUTION, and relatively single extraction system more relies on pair The control of aqueous phase solution condition, with obvious advantage.
(3) soda acid of the invention coupling extraction system is applied in combination using existing business extractant, and raw material is easy to get, into This is low, and the separation of complex multi-metal solution can be realized using existing ripe extraction process, is conducive to popularization and application.
Embodiment
With reference to embodiment, the invention will be further described, and following examples are intended to illustrate invention rather than right The further restriction of the present invention.
Embodiment 1
Zinc-copper solution separation system:Copper, zinc concentration are respectively 1.3g/L, sodium sulfate concentration 85g/L wherein in aqueous phase solution, PH is 4;Acidic extractant is D2EHPA in organic phase, and basic extractant is Cyphos IL101 or Aliquat336, diluent For kerosene, basic extractant is added into the acidic extractant, the total concentration of extractant is 0.5mol/L, changes soda acid extractant Relative molar concentration constitute following soda acid coupling extraction system (being shown in Table 1).At normal temperatures, according to compared to A/O=1:1 with containing zinc The aqueous phase of copper is extracted respectively, and extraction time is 30min;After stratification, raffinate is taken to obtain metal by icp analysis Ion concentration, calculates the extraction yield and separation factor of the zinc-copper with the conditions of, as a result as shown in table 1.
The extraction yield and separation of the zinc-copper with the conditions of of table 1
As a result show, under the conditions of without basic extractant, the extraction efficiency of zinc-copper is not high, and separation factor exists Less than 10;When adding Cyphos IL101, in the case where ensureing that soda acid coupling extractant total concentration is constant, the extraction yield of copper Reduction, and the extraction yield of zinc is raised, and greatly improves the separative efficiency of zinc-copper, separation is up to more than 1000;Addition Aliquat336 has same impact effect to zinc-copper separative efficiency.
Embodiment 2
Nickel and cobalt solution separation system:Cobalt, nickel concentration are respectively 1.2g/L, ammonium chloride concentration 107g/ wherein in aqueous phase solution L, pH are 8.2.Acidic extractant is Cyanex272 in organic phase, and basic extractant is Cyphos IL101, TOA, and diluent is Kerosene, adds the acidic extractant, the total concentration of extractant is 0.5mol/L, changes soda acid extractant by basic extractant Relative molar concentration constitutes following soda acid coupling extraction system (being shown in Table 2).At normal temperatures, according to compared to A/O=1:1 and nickel and cobalt containing Aqueous phase extracted respectively, extraction time is 30min;After stratification, take raffinate by icp analysis obtain metal from Sub- concentration, calculates the extraction yield and separation factor of the nickel cobalt with the conditions of, as a result as shown in table 2.
The extraction yield and separation of the cobalt nickel with the conditions of of table 2
As a result show, under the conditions of without basic extractant, the extraction efficiency of nickel cobalt is all high, and separation factor is less than 20;In the case where ensureing that acidic extractant Cyanex272 and basic extractant total concentration are constant, as addition Cyphos IL101 When can significantly inhibit the extraction of nickel, so as to promote the separation of cobalt nickel, under the conditions of suitable concentration proportioning, the separation factor of cobalt nickel More than 80 are increased to, addition TOA has same impact effect to cobalt nickel separative efficiency.
Embodiment 3
Cupro-nickel solution separation system:Wherein copper, nickel concentration are respectively 1.3g/L, 1.2g/L in aqueous phase solution, and ammonium sulfate is dense Spend for 132g/L, pH is 9.5.Faintly acid extractant is LIX84I in organic phase, and basic extractant is Cyanex923, TEHP, dilute Agent is released for kerosene, basic extractant the faintly acid extractant is added into, the total concentration of extractant is 0.1mol/L, changes soda acid The relative molar concentration of extractant constitutes following soda acid coupling extraction system (being shown in Table 3).At normal temperatures, according to compared to A/O=1:1 Extracted respectively with the aqueous phase of nickel and cobalt containing, extraction time is 30min;After stratification, raffinate is taken to be obtained by icp analysis To concentration of metal ions, the extraction yield and separation factor of the cupro-nickel with the conditions of are calculated, as a result as shown in table 3.
The extraction yield and separation of the cupro-nickel with the conditions of of table 3
As a result show, under the conditions of without basic extractant, the extraction efficiency of cupro-nickel is all high, and separation factor is 10 Hereinafter, when adding Cyanex923, in the case where ensureing that acidic extractant LIX84I and basic extractant total concentration are constant, The extraction yield of nickel is significantly reduced, so that the separation of cupro-nickel is promoted, when LIX84I/Cyanex923 mol ratios are 4/1, cupro-nickel Separation can bring up to 384.59, addition TEHP has same impact effect to copper moulding efficiency.

Claims (5)

1. a kind of soda acid couples the application of extraction system, it is characterised in that:Applied to including two or more many of copper, cobalt, nickel, zinc The selective extraction separation of target metal ions in metallic solution;
The soda acid couples extraction system, and comprising extractant and diluent, described extractant is by basic extractant and acid extract Agent is taken to constitute;
Described many metallic solutions are pH<5 Zn/Cu mixing sulfuric acid solutions, or be the Ni/Co ammonia solutions that pH is 6~10, Or be the Cu/Ni ammonia solutions that pH is 7~10;Various concentration of metal ions are respectively 0.1 in described many metallic solutions ~3g/L;
Using the acid containing double (2- ethylhexyls) phosphates and three hexyl myristyl phosphonium chlorides and/or tri-n-octyl methyl ammonium chloride Alkali couples extraction system, is separated for the Zn in Zn/Cu mixing sulfuric acid solutions and Cu;
Using the soda acid coupling containing two (2,4,4- tri-methyl-amyls) hypophosphorous acid and three hexyl myristyl phosphonium chlorides and/or trioctylamine Close extraction system, the separation for Ni and Co in Ni/Co mixing ammonia solutions;
Coupled using -1,3- the last of the ten Heavenly stems diketone of phenyl containing 1- with the soda acid of trioctylphosphine and/or three (2- ethylhexyls) phosphates Extraction system, the separation for Cu and Ni in Cu/Ni mixing ammonia solutions.
2. soda acid according to claim 1 couples the application of extraction system, it is characterised in that:Described extractant neutral and alkali Extractant and acidic extractant mol ratio are 1~9:1~5.
3. soda acid according to claim 1 couples the application of extraction system, it is characterised in that:Described diluent is sulfonation Kerosene.
4. soda acid according to claim 1 couples the application of extraction system, it is characterised in that:The soda acid couples extractor body The concentration of extractant is 10~60 times of target metal ions concentration in many metallic solutions in system.
5. soda acid according to claim 1 couples the application of extraction system, it is characterised in that:
Extraction system is coupled with the soda acid of three hexyl myristyl phosphonium chlorides using containing double (2- ethylhexyls) phosphates, for pH Zn and Cu separation in=4 Zn/Cu mixing sulfuric acid solutions, wherein, double (2- ethylhexyls) phosphates and the three hexyl tetradecanes The mol ratio of base phosphonium chloride is 3/7;
Extraction system is coupled with the soda acid of tri-n-octyl methyl ammonium chloride using containing double (2- ethylhexyls) phosphates, for pH=4 Zn/Cu mixing sulfuric acid solutions in Zn and Cu separation, wherein, double (2- ethylhexyls) phosphates and tri-n-octyl methyl ammonium chloride Mol ratio be 1/9;
Using containing two (2,4,4- tri-methyl-amyls) hypophosphorous acid extractor body is coupled with the soda acid of three hexyl myristyl phosphonium chlorides System, for the separation of Ni and Co in pH=8.2 Ni/Co mixing ammonia solutions, wherein, two (2,4,4- tri-methyl-amyl) secondary phosphorus The mol ratio of acid and three hexyl myristyl phosphonium chlorides is 3/7;
Extraction system is coupled with the soda acid of trioctylamine using containing two (2,4,4- tri-methyl-amyl) hypophosphorous acid, for pH=8.2's Ni and Co separation in Ni/Co mixing ammonia solutions, wherein, mole of two (2,4,4- tri-methyl-amyl) hypophosphorous acid and trioctylamine Than for 1/9;
Extraction system is coupled with the soda acid of trioctylphosphine using the -5- of hydroxyl containing 2- nonylacetophenone oximes, for pH=9.5's Cu and Ni separation in Cu/Ni mixing ammonia solutions, wherein, 2- hydroxyl -5- nonylacetophenone oximes and trioctylphosphine rub You are than being 4/1;
Extraction system is coupled with the soda acid of three (2- ethylhexyls) phosphates using the -5- of hydroxyl containing 2- nonylacetophenone oximes, is used for Cu and Ni separation in pH=9.5 Cu/Ni mixing ammonia solutions, wherein, 2- hydroxyl -5- nonylacetophenone oximes and three (2- second Base hexyl) phosphate mol ratio be 4/1.
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