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WO1998056482A1 - Preequilibrage d'un agent d'extraction cationique - Google Patents

Preequilibrage d'un agent d'extraction cationique Download PDF

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Publication number
WO1998056482A1
WO1998056482A1 PCT/AU1998/000457 AU9800457W WO9856482A1 WO 1998056482 A1 WO1998056482 A1 WO 1998056482A1 AU 9800457 W AU9800457 W AU 9800457W WO 9856482 A1 WO9856482 A1 WO 9856482A1
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WO
WIPO (PCT)
Prior art keywords
magnesium
magnesia
extractant
acidic organic
organic cationic
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/AU1998/000457
Other languages
English (en)
Inventor
Serge Lallenec
David Honey
David Muir
John O'callaghan
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
WMC Resources Ltd
Original Assignee
WMC Resources Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by WMC Resources Ltd filed Critical WMC Resources Ltd
Priority to AU80039/98A priority Critical patent/AU739497B2/en
Publication of WO1998056482A1 publication Critical patent/WO1998056482A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00—Obtaining nickel or cobalt
    • C22B23/04—Obtaining nickel or cobalt by wet processes
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the present invention relates generally to a process for pre-equilibration of an acidic organic cationic extractant suitable for use in solvent extraction and relates particularly, though not exclusively, to pre-equilibration of a carboxylic acid cationic extractant with magnesia, magnesium hydroxide, or magnesium carbonate.
  • the extraction pH is controlled by the addition of an alkali solution, such as a sodium hydroxide or ammonium hydroxide solution.
  • an alkali solution such as a sodium hydroxide or ammonium hydroxide solution.
  • Milk of Magnesia and lime have been unsuccessfully trialled in a solvent extraction circuit for maintaining the extraction pH at the required level .
  • the relatively fine solid particles of magnesia and lime combine with an aqueous and an organic phase in the solvent extraction circuit to form crud or an emulsion layer which usually collects at an interface between the aqueous and organic phases. This crud or emulsion layer hinders disengagement of the aqueous and organic phases increasing the phase disengagement time and can result in organic phase losses in the aqueous phase waste stream.
  • Australian Patent No. 667539 in the name of Outokumpu describes a method of forming a magnesium salt of a cationic extractant and preventing the formation of jarosite and ammonium and alkali based nickel double salts during solvent extraction.
  • the method involves pre-neutralisation of a cationic extractant such as CYANEX 272 with ammonium to form a CYANEX 272 ammonium salt and thereafter a pre-extraction or exchange of the CYANEX 272 salt with magnesium sulphate in an aqueous solution to produce a CYANEX 272 magnesium salt.
  • the CYANEX 272 magnesium salt is then, in a solvent extraction circuit, contacted with an aqueous solution containing valuable metals such as cobalt and nickel so as to extract the metal.
  • the nickel solution which is stripped from the solvent extractant is then electrowon.
  • An intention of the present invention is to provide a process for pre-equilibrating an acidic organic cationic extractant to be used in a solvent extraction circuit, said process being relatively inexpensive and having a minimal adverse effect on the solvent extraction circuit.
  • a process for pre-equilibration of an acidic organic cationic extractant suitable for use in a solvent extraction circuit involving the step of: (a) adding chemically reactive magnesia, magnesium hydroxide, or magnesium carbonate to a kerosene solution of the acidic organic cationic extractant so as to form a pre-equilibrated magnesium salt of the solvent extractant which can then be used in the solvent extraction circuit for effective loading of one or more metal cations contained in an aqueous mineral feed liquor.
  • magnesia, magnesium hydroxide, or magnesium carbonate is in a substantially dry condition when added to the acidic organic cationic extractant.
  • magnesia, magnesium hydroxide, or magnesium carbonate is slurried with just sufficient water prior to its addition to the acidic organic cationic extractant.
  • Dry magnesia, magnesium hydroxide, or magnesium carbonate is preferred to slurried magnesia, magnesium hydroxide, or magnesium carbonate which exhibits relatively high levels of unreacted or entrained magnesia, magnesium hydroxide, or magnesium carbonate during pre-equilibration at process step (a) . It is understood that this unreacted or entrained magnesia, magnesium hydroxide, or magnesium carbonate then results in the formation of crud when water is also present.
  • the acidic organic cationic extractant comprises a high molecular weight organic carboxylic, phosphoric, phosphonic, or phosphinic acid such as the proprietary products VERSATIC 10, D2EPHA, PC88A, or CYANEX 272 respectively.
  • the acidic organic cationic extractant may comprise a dithiophosphoramide or dithiophosphinic acid such as the proprietary products ZENECA DS 6001 or CYANEX 301, respectively.
  • the acidic organic cationic extractant is dissolved or diluted in kerosene to give solutions typically containing between 5 to 50% w/v of said extractant.
  • magnesia, magnesium hydroxide, or magnesium carbonate is derived from a technical or commercial grade calcined magnesite or dolomite.
  • the invention is not restricted to magnesia, magnesium hydroxide, or magnesium carbonate of a specific particle size distribution it will be appreciated that a relatively fine particle size is preferred so as to minimise the reaction time required to pre-equilibrate the acidic organic cationic extractant in process step (a) .
  • the step of adding magnesia, or magnesium hydroxide, or magnesium carbonate to the acidic organic cationic extractant involves adding a stoichiometric quantity of magnesia, magnesium hydroxide, or magnesium carbonate.
  • a stoichiometric quantity of magnesia, magnesium hydroxide, or magnesium carbonate is considered to be that required to achieve the following reaction:
  • R ⁇ H + represents an acidic organic cationic extractant
  • MgO represents the equivalent reactive MgO content of basic magnesium minerals containing magnesia, magnesium hydroxide, or magnesium carbonate
  • R ⁇ 2 Mg 2+ represents a pre-equilibrated magnesium salt of the solvent extractant .
  • a quantity of between 30% to 150% of the stoichiometric requirement of magnesia, magnesium hydroxide, or magnesium carbonate is added to the acidic organic cationic extractant. More typically, the process further involves subsequent to step (a) filtering of the pre-equilibrated magnesium salt of the solvent extractant so as to remove unreacted magnesia, magnesium hydroxide, or magnesium carbonate prior to solvent extraction.
  • phase modifier is an alcohol phase modifier such as isodecanol or iso-tridecanol .
  • the step of adding magnesia, magnesium hydroxide, or magnesium carbonate is carried out with sub-stoichiometric levels to minimise the filter demand and crud formation.
  • the step of adding magnesia, magnesium hydroxide, or magnesium carbonate is conducted at a temperature of between approximately ambient to 95°C. More typically, the temperature of pre-equilibration is from between approximately 50° to 60°C.
  • the step of adding magnesia, magnesium hydroxide, or magnesium carbonate is performed under conditions of agitation at a stirring rate of at least approximately 60 rpm.
  • process step (a) involving the pre-equilibration of the acidic organic cationic extractant is relatively fast occurring in less than approximately five (5) minutes, typically when using finely ground magnesia, magnesium hydroxide, or magnesium carbonate at approximately 50°C.
  • process step (b) involving loading of the pre-equilibrated magnesium salt of the solvent extractant in the solvent extraction circuit is also relatively fast, equilibrium being established in less than approximately two (2) minutes.
  • the mineral feed liquor is a metal sulphate leach liquor.
  • said one or more valuable metals loaded during solvent extraction in step (b) include nickel, cobalt, copper, zinc, manganese and/or iron.
  • Figure 1 is a flowsheet illustrating an apparatus used for the pre-equilibration of a kerosene solution of VERSATIC 10 with substantially dry magnesia;
  • Figure 2 is a flowsheet illustrating pre-equilibration of VERSATIC 10 solution in kerosene with 100% excess dry magnesia followed by solvent extraction of a nickel sulphate feed and stripping of the nickel with sulphuric acid to provide barren organic which is recycled;
  • Figure 3 is a flowsheet depicting 75% partial pre-equilibration of VERSATIC 10 solution in kerosene with dry magnesia followed by solvent extraction of a nickel sulphate feed and stripping of the nickel with sulphuric acid;
  • Figure 4 is a flowsheet showing 50% partial pre-equilibration of VERSATIC 10 solution in kerosene with dry magnesium hydroxide followed by solvent extraction of a nickel sulphate feed liquor.
  • R " H + represents an acidic organic cationic extractant
  • MgO represents the equivalent reactive MgO content of basic magnesium minerals containing magnesia, magnesium hydroxide, or magnesium carbonate.
  • magnesium was introduced into an acidic organic cationic extractant as magnesia (MgO, dry or slurried) , magnesium hydroxide (slaked from magnesia) , solid magnesium hydroxide Mg(OH) 2 , or magnesium carbonate.
  • acidic organic cationic extractants including the following proprietary products, were pre-equilibrated with magnesium. It will be appreciated that this invention is not limited to particular acidic cationic extractants and that the following serve as examples .
  • VERSATIC 10 (Shell Chemicals Co.) is a mixture of synthetic, saturated carboxylic acid isomers, derived from a highly branched Cio structure.
  • R 3 Ri, R 2 , and R 3 are alkyl groups, of which at least one is methyl .
  • VERSATIC 10 As a carboxylic acid, VERSATIC 10 exhibits low acidic strength due to alkyl substitution at the alpha position, but outstanding solubility in kerosene-type solvents.
  • the physical /chemical characteristics of VERSATIC 10 are as follows :
  • ZENECA DS 6001 is a development solvent extraction reagent based on a tetra-substituted dithiophosphoramide structure.
  • Ri to R may be any of (substituted) alkyl, O-alkyl, aryl, and O-aryl .
  • CYANEX 301 is a dithiophosphinic acid solvent extraction reagent which is an isomer of DS 6001 having the following chemical structure.
  • Ri and R 2 are 2,4,4 trimethyl pentyl .
  • CYANEX 272 is another suitable organic cationic extractant with its active component being bis (2 , 4 , 4-trimethylpentyl) phosphinic acid represented by the following formula.
  • CYANEX 272 extractant is a phosphinic acid
  • metals are extracted through a cation exchange mechanism. Molecular Weight: 290
  • Highly reactive calcined magnesite was produced under closely controlled conditions and then precision milled to superfine requirements to give an especially fine particle size distribution thereby achieving maximum area and high chemical reactivity.
  • Arsenic (As) 0.0004%
  • FIG. 1 illustrates a bench scale apparatus used for pre-equilibrating the acidic organic cationic extractant VERSATIC 10 with dry magnesia (MgO) .
  • the dry magnesia was fed through a screw feeder 10 to a jacketed reactor vessel 12 which contained the barren IM solution of VERSATIC 10 in kerosene at a temperature of approximately 50°C.
  • the pre-equilibrated VERSATIC 10 was then pumped to a solvent extraction circuit with any unreacted magnesia being filtered before solvent extraction.
  • the VERSATIC 10 extractant loading capacity for magnesium from slurried magnesium hydroxide (ie slaked MgO, 24 hours) at 60°C was 10 g/L Mg compared to 11 and 12 g/L Mg achieved from slurried or dry magnesia, respectively. It was found that tests conducted with excess magnesium, in the form of magnesium hydroxide slurry, and unmodified VERSATIC 10 at a temperature of 50°C resulted in the formation of a VERSATIC-magnesium soap or third phase crud.
  • IM VERSATIC 10 in kerosene was stirred with magnesia in a dry and slurried form with and without a phase modifier.
  • VERSATIC 10 was modified with 10% v/v alcohol phase modifier, in this example Isodecanol and Iso-tridecanol , before contacting with dry or slurried magnesia.
  • No significant variations were found in either the extraction capacity or the kinetics of magnesium pre-equilibration with the incorporation of alcohol phase modifiers to VERSATIC 10, in both dry and slurry magnesia addition. Greater than 85% magnesium pre-equilibration was achieved, with the exception of the VERSATIC/magnesia slurry system. It should be noted that the formation of an emulsion occurred with the addition of excess magnesia when no phase modifier was used. Fast kinetics of less than one minute were recorded for the tests .
  • Example 5 A solution of IM VERSATIC 10 in kerosene was stirred with 75% stoichiometric dry magnesia at temperatures from 20 to 60°C and levels of agitation, ranging from 400 to 1200rpm. The kinetics of magnesia loading on VERSATIC 10 were relatively fast at less than approximately two (2) minutes. Furthermore, the loading capacity was not significantly affected by temperature or agitation with between 80 to 90% pre-equilibration of available magnesium being observed in all conditions .
  • Example 8 A solution of 0.6M ZENECA DS6001 reagent in kerosene was reacted with 75% stoichiometric EMAG 45 magnesia at 60°C under similar conditions to tests with CYANEX 272 (see Example 7) . With this reagent, only about 10% of the available magnesium was extracted, with no significant increase upon increasing reaction time or stirring. Up to 18% Mg extraction was achieved by raising the temperature to 100°C and by further grinding the magnesia in-si tu in a ceramic ball mill. It appears that the extent of reaction is limited by the "weak acidity" of the functional group of this reagent.
  • Figure 2 shows that approximately 100% (12 g/L Mg) pre-equilibration was achieved with 100% excess dry magnesia powder addition.
  • the calculated theoretical maximum nickel loading capacity of 30 g/L with IM VERSATIC 10 was achieved at a temperature of 50°C with an extraction O/A of 1.0.
  • Figures 3 and 4 indicate a target of 75% and 50% magnesium pre-equilibration, with 68% and 40% pre-equilibration actually being achieved.
  • the nickel extraction of 22.8 g/L (78%) and 15.1 g/L (50%) was found to be very close to the theoretical maximum extraction of 22 g/L and 15 g/L, respectively. This demonstrated that only the magnesium in the organic phase exchanged for nickel and no protons were exchanged .
  • nickel loading kinetics with magnesium pre-equilibrated VERSATIC 10 are fast, with equilibrium established in less than approximately two minutes. Furthermore, it is believed that the VERSATIC 10 loading capacity for nickel is related to the amount of magnesium pre-equilibration which maintains the pH of extraction and the concentration of magnesium in the organic.
  • the experimental loading capacity of nickel on IM VERSATIC 10 corresponded to the theoretical calculations of 30 g/L Ni for 100%, 22 g/L for 75% and 15 g/L for 50% magnesium pre-equilibration.
  • the amount of calcium remaining in the VERSATIC 10 organic phase increases significantly at pH of greater than approximately 6.9.
  • magnesia, magnesium hydroxide, or magnesium carbonate are relatively inexpensive alkali substances suitable for pre-equilibration of an acidic organic cationic extractant;
  • pre-equilibration of an acidic organic cationic extractant using magnesia, magnesium hydroxide, or magnesium carbonate has a minimal adverse effect on a solvent extraction circuit when carried out separately from the extraction step where water is mixed with the organic extractant;
  • the present invention is not limited to the embodiments described above and numerous variations and modifications can be made to the process for pre-equilibrating an acidic organic cationic extractant which still remain within the ambit of the present invention.
  • the embodiments described relate to solvent extraction of a nickel sulphate leach liquor the invention also extends to cobalt, copper, zinc, or other sulphate leach liquors.

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  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
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Abstract

La présente invention concerne de manière générale l'observation selon laquelle le prééquilibrage d'un agent d'extraction cationique organique acide avec du magnésium évite d'avoir à régler le pH dans un circuit d'extraction par solvant. Selon divers modes de réalisation de cette invention, du magnésium est introduit dans un agent d'extraction cationique organique acide sous forme de magnésie (MgO, sous forme sèche ou pâteuse) d'hydroxyde de magnésium (schiste de magnésie), d'hydroxyde de magnésium solide, ou de carbonate de magnésium. Divers agents d'extraction cationiques organiques acides comprenant VERSATIC 10, ZENECA DS 6001, CYANEX 301 et CYANEX 272 peuvent être prééquilibrés avec du magnésium. Le prééquilibrage dudit agent d'extraction à l'aide de magnésie, d'hydroxyde de magnésium ou de carbonate de magnésium, a un effet nocif minime sur un circuit d'extraction par solvant lorsqu'il est réalisé séparément de l'étape d'extraction où l'eau est mélangée avec l'agent organique d'extraction.
PCT/AU1998/000457 1997-06-12 1998-06-12 Preequilibrage d'un agent d'extraction cationique Ceased WO1998056482A1 (fr)

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Application Number Priority Date Filing Date Title
AU80039/98A AU739497B2 (en) 1997-06-12 1998-06-12 Pre-equilibration of a cationic extractant

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AUPO7327 1997-06-12
AUPO7327A AUPO732797A0 (en) 1997-06-12 1997-06-12 Pre-equilibration of a cationic extractant

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001048252A1 (fr) * 1999-12-24 2001-07-05 Wmc Resources Limited Extraction par solvant de metaux impurs presents dans une solution de sulfate de metal precieux
WO2001096621A1 (fr) * 2000-06-13 2001-12-20 Wmc Resources Limited Extraction par solvant des impuretes presentes dans des solutions de sulfate metallique concentrees
AU2001273737B2 (en) * 2000-06-13 2005-06-09 Wmc Resources Limited Solvent extraction of impurities from concentrated metal sulphate solutions
EP1330555A4 (fr) * 2000-09-15 2005-08-31 Commw Scient Ind Res Org Procede d'extraction de solvant destine a extraire le nickel et le cobalt de solutions de lixiviation
WO2008015582A3 (fr) * 2006-06-15 2008-07-10 Cognis Ip Man Gmbh Procédé pour améliorer des séparations de phases dans des circuits d'extraction par solvant
CN111410217A (zh) * 2020-04-10 2020-07-14 吉林吉恩镍业股份有限公司 一种采用萃取分离法去除硫酸镁溶液中镍和钴的方法

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU4126793A (en) * 1992-06-18 1993-12-23 Outokumpu Harjavalta Metals Oy Method for preventing the formation of jarosite and ammonium and alkali based double salts in solvent extraction circuits connected to acidic leaching processes

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU4126793A (en) * 1992-06-18 1993-12-23 Outokumpu Harjavalta Metals Oy Method for preventing the formation of jarosite and ammonium and alkali based double salts in solvent extraction circuits connected to acidic leaching processes

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001048252A1 (fr) * 1999-12-24 2001-07-05 Wmc Resources Limited Extraction par solvant de metaux impurs presents dans une solution de sulfate de metal precieux
US20030064013A1 (en) * 1999-12-24 2003-04-03 O'callaghan John Solvent extraction of impurity metals from a valuable metal sulphate solution
EP1252345A4 (fr) * 1999-12-24 2005-07-13 Wmc Resources Ltd Extraction par solvant de metaux impurs presents dans une solution de sulfate de metal precieux
US7727496B2 (en) 1999-12-24 2010-06-01 Wmc Resources Ltd. Solvent extraction of impurity metals from a valuable metal sulphate solution
WO2001096621A1 (fr) * 2000-06-13 2001-12-20 Wmc Resources Limited Extraction par solvant des impuretes presentes dans des solutions de sulfate metallique concentrees
AU2001273737B2 (en) * 2000-06-13 2005-06-09 Wmc Resources Limited Solvent extraction of impurities from concentrated metal sulphate solutions
EP1330555A4 (fr) * 2000-09-15 2005-08-31 Commw Scient Ind Res Org Procede d'extraction de solvant destine a extraire le nickel et le cobalt de solutions de lixiviation
WO2008015582A3 (fr) * 2006-06-15 2008-07-10 Cognis Ip Man Gmbh Procédé pour améliorer des séparations de phases dans des circuits d'extraction par solvant
US8298510B2 (en) 2006-06-15 2012-10-30 Basf Corporation Process for improving phase separations in solvent extraction circuits
AU2007280103B2 (en) * 2006-06-15 2012-12-20 Cognis Ip Management Gmbh Process for improving phase separations in solvent extraction circuits of metal winning
CN111410217A (zh) * 2020-04-10 2020-07-14 吉林吉恩镍业股份有限公司 一种采用萃取分离法去除硫酸镁溶液中镍和钴的方法

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