WO2006113944A1 - Separation of nickel from cobalt by using chloridizing solution and cobalt-selective resin - Google Patents

Separation of nickel from cobalt by using chloridizing solution and cobalt-selective resin Download PDF

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Publication number
WO2006113944A1
WO2006113944A1 PCT/ZA2006/000054 ZA2006000054W WO2006113944A1 WO 2006113944 A1 WO2006113944 A1 WO 2006113944A1 ZA 2006000054 W ZA2006000054 W ZA 2006000054W WO 2006113944 A1 WO2006113944 A1 WO 2006113944A1
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WO
WIPO (PCT)
Prior art keywords
cobalt
nickel
solution
chloride
bed
Prior art date
Application number
PCT/ZA2006/000054
Other languages
French (fr)
Inventor
Edmund Kevin Hardwick
Original Assignee
Edmund Kevin Hardwick
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 Edmund Kevin Hardwick filed Critical Edmund Kevin Hardwick
Publication of WO2006113944A1 publication Critical patent/WO2006113944A1/en

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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
    • C22B23/00—Obtaining nickel or cobalt
    • C22B23/04—Obtaining nickel or cobalt by wet processes
    • C22B23/0476—Separation of nickel from cobalt
    • C22B23/0484—Separation of nickel from cobalt in acidic type solutions
    • 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
    • C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
    • 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
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
    • 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

  • This invention relates generally to a method of separating nickel from cobalt in a nickel-cobalt mixture.
  • Nickel and cobalt are commonly found together in ore or scrap form.
  • the effective separation of the two metals, from such sources, can have a significant economic benefit due to the increased price obtainable for relatively pure cobalt and pure nickel products.
  • increasing levels of contamination of one metal with the other lead to a proportionate decrease in price.
  • a separation theory has been developed making use of cobalt's propensity to complex with chloride ions, when contacted with a chloride solution of high concentration, to form an anionic cobalt chloride complex [CoCI 4 ] 2" .
  • Nickel has no such affinity and does not complex with chloride.
  • a solution containing the cobalt chloride complex and nickel can then be passed through an anion exchange resin. Due to its negative charge the cobalt complex is retained on me resin whilst the nickel passes through.
  • the present invention at least partially addresses the afore-mentioned problem.
  • the invention provides a method of separating nickel from cobalt in a nickel- cobalt mixture which includes the step of dissolving the mixture in a mixed chloride solution to form an anionic cobalt chloride complex in a resultant solution, and wherein the chloride content of the mixed chloride solution originates from at least two different chloride sources.
  • Each chloride source may be selected from any suitable chloride salt and hydrochloric acid.
  • the resultant solution may be heated to enhance the formation of the cobalt chloride complex.
  • the cobalt chloride complex may be separated from the resultant solution by allowing the resultant solution to percolate through a bed of resin having an affinity for anions so that the cobalt chloride complex is absorbed by a resin in the bed and allowing a remaining solution, which is substantially cobalt-free, to pass through the bed.
  • Nickel may be removed from the remaining solution by any appropriate method such as through the use of a precipitation, crystallization or electrowinning technique.
  • nickel may be removed by passing the remaining solution through a nickel selective resin bed so that the nickel is adsorbed by a resin in the resin bed, thus allowing the remainder of the remaining solution, which is a substantially nickel-free solution, to pass through the resin bed.
  • the nickel-free solution may be recycled to a chloride salt source.
  • the nickel may be eluted and recovered from the nickel selective resin by a suitable wash method.
  • a chloride wash solution may be applied to the bed resulting in a cobalt eluate.
  • Cobalt may be recovered from the cobalt eluate by any appropriate method such as through the use of precipitation, crystallization or electrowinning technique.
  • cobalt may be recovered by passing the cobalt eiuate through a cobalt selective resin bed so that the cobalt is adsorbed by a resin in the selective resin bed, and allowing the remaining eiuate, a substantially cobalt-free eiuate, to pass through the selective resin bed.
  • the cobalt-free eiuate may be recycled to a chloride salt source.
  • the cobalt may be eluted and recovered from the cobalt selective resin by a suitable wash method.
  • the apparatus 10 includes a tank 12, a chloride salt source 14, a source 16 of a nickel-cobalt mixture and a source 18 of hydrochloric acid.
  • a resultant solution 20 from the tank 12 is directed to an anionic affinity bed 22
  • a remaining solution 24 from the bed 22 flows to a nickel selective resin bed 26.
  • a cobalt eluate 34 is released from the affinity bed 22 after washing the bed 22 with a chloride solution 36 from the chloride salt source 14.
  • the cobalt eluate 34 reports to a cobalt selective resin bed 38. Washing the bed 38 with an acid from the source 28 of acid elutes a cobalt product 40. A substantially cobalt-free eluate 42 leaves the bed 38.
  • a finely divided nickel-cobalt mixture from the source 16 is fed at a controlled rate to the tank 12, subsequent to the controlled introduction of a hydrochloric acid solution from the source 18 and a saturated chloride salt solution from the source
  • the saturated chloride salt solution can be produced from any suitable chloride salt.
  • Sodium chloride is preferably used as it is easily obtainable and cheap.
  • the resultant solution 20 reports to and percolates through the anionic affinity resin bed 22 which contains a resin that can work either by an anion exchange or an anion chelating action.
  • the resin is a commercially available strong base anion exchange resin in a polystyrenic or acrylic matrix.
  • the remaining solution 24 then reports to the nickel selective resin bed 26.
  • a specific nickel selecting chelating resin is contained within the nickel selective resin bed 26.
  • nickel is adsorbed to the nickel selective resin and a remainder of the remaining solution 24, now a substantially nickel- free solution 32, is relinquished from the bed 26.
  • a chloride solution 36 is used to wash the bed 22.
  • the added water facilitates the dilution of the chloride solution 36 to a less than seven molar chloride solution.
  • the chloride solution 36 is drawn from the chloride salt source 14 prior to entry of the saturated chloride salt solution to the tank 12.
  • a cobalt eluate 34 issues from the bed 22.
  • the chloride solution 36 needs to be less than a seven molar solution to reverse the complexing of chloride with cobalt.
  • the cobalt eluate 34 reports to a cobalt selective resin bed 38.
  • a strong acid cation exchange resin is preferably used as a cobalt selective resin within the cobalt selective resin bed 38.
  • cobalt is adsorbed to the cobalt selective resin and the remainder of the eluate 34, now a substantially cobalt-free eluate 42, passes through the bed 38.
  • the use of a chloride salt allows an additional recycle step to be incorporated into the method of the invention.
  • the substantially nickel-free solution 32 which is also substantially devoid of cobalt, and the substantially cobalt-free solution 42 which is also substantially devoid of nickel, can be recycled to the chloride salt source 14.
  • the nickel product 30 can be neutralized with a sodium hydroxide solution before being pressed and filtered to recover nickel in a substantially pure metallic form.
  • the cobalt product 40 can be neutralized with sodium carbonate before being pressed and filtered to recover the cobalt in a substantially pure metallic form.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

Nickel is recovered from a nickel-cobalt mixture by dissolving the mixture in a chloride solution which originates from at least two different chloride sources, to form an anionic cobalt chloride complex which is separated from the solution using a suitable resin having an affinity for anions. The nickel in the remaining solution passed through the bed of resin is separated therefrom using a nickel selective resin.

Description

SEPARATION OF NICKEL FROM COBALT BY USING CHLORIDIZING SOLUTION AND
COBALT-SELECTIVE RESIN
BACKGROUND OF THE INVENTION
[0001] This invention relates generally to a method of separating nickel from cobalt in a nickel-cobalt mixture.
[0002] Nickel and cobalt are commonly found together in ore or scrap form. The effective separation of the two metals, from such sources, can have a significant economic benefit due to the increased price obtainable for relatively pure cobalt and pure nickel products. Conversely, increasing levels of contamination of one metal with the other lead to a proportionate decrease in price.
[0003] Due to the similar chemistries of nickel and cobalt, prior art separation methods have cost and efficiency disadvantages. In one such method a selective ion exchanger is employed. Because of the similar chemistries of the two metals, selectively exchanging and retaining one metal ion in preference to the other, on an ion exchange resin, requires a number of recycle steps through the ion exchanger to achieve sufficient separation.
[0004] A separation theory has been developed making use of cobalt's propensity to complex with chloride ions, when contacted with a chloride solution of high concentration, to form an anionic cobalt chloride complex [CoCI4]2". Nickel has no such affinity and does not complex with chloride. [0005] A solution containing the cobalt chloride complex and nickel can then be passed through an anion exchange resin. Due to its negative charge the cobalt complex is retained on me resin whilst the nickel passes through.
[0006] The theory has no history of industrial application, as the chloride solution is derived from hydrochloric acid. The use of hydrochloric acid has a number of disadvantages including the high cost of the acid and the high cost involved in neutralizing excess acid, the problem associated with the disposal of a highly saline effluent and corrosion of equipment caused by the acid.
[0007] The present invention at least partially addresses the afore-mentioned problem.
SUMMARY OF INVENTION
[0008] The invention provides a method of separating nickel from cobalt in a nickel- cobalt mixture which includes the step of dissolving the mixture in a mixed chloride solution to form an anionic cobalt chloride complex in a resultant solution, and wherein the chloride content of the mixed chloride solution originates from at least two different chloride sources.
[0009] Each chloride source may be selected from any suitable chloride salt and hydrochloric acid.
[0010] The resultant solution may be heated to enhance the formation of the cobalt chloride complex. [0011] The cobalt chloride complex may be separated from the resultant solution by allowing the resultant solution to percolate through a bed of resin having an affinity for anions so that the cobalt chloride complex is absorbed by a resin in the bed and allowing a remaining solution, which is substantially cobalt-free, to pass through the bed.
[0012] Nickel may be removed from the remaining solution by any appropriate method such as through the use of a precipitation, crystallization or electrowinning technique.
[0013] Alternatively nickel may be removed by passing the remaining solution through a nickel selective resin bed so that the nickel is adsorbed by a resin in the resin bed, thus allowing the remainder of the remaining solution, which is a substantially nickel-free solution, to pass through the resin bed.
[0014] The nickel-free solution may be recycled to a chloride salt source.
[0015] The nickel may be eluted and recovered from the nickel selective resin by a suitable wash method.
[0016] To release cobalt from the cobalt chloride complex and allow it to elute from the bed a chloride wash solution may be applied to the bed resulting in a cobalt eluate.
[0017] Cobalt may be recovered from the cobalt eluate by any appropriate method such as through the use of precipitation, crystallization or electrowinning technique. [0018] Alternatively cobalt may be recovered by passing the cobalt eiuate through a cobalt selective resin bed so that the cobalt is adsorbed by a resin in the selective resin bed, and allowing the remaining eiuate, a substantially cobalt-free eiuate, to pass through the selective resin bed.
[0019] The cobalt-free eiuate may be recycled to a chloride salt source.
[0020] The cobalt may be eluted and recovered from the cobalt selective resin by a suitable wash method.
BRIEF DESCRIPTION OF THE DRAWING
[0021] The invention is further described by way of example with reference to the accompanying drawing which schematically illustrates a method of separating nickel from cobalt in a nickel-cobalt mixture using the principles of the invention.
DESCRIPTION OF PREFERRED EMBODIMENT
[0022] The accompanying drawing illustrates apparatus 10 for the separation of nickel from cobalt in accordance with the method of the invention.
[0023] The apparatus 10 includes a tank 12, a chloride salt source 14, a source 16 of a nickel-cobalt mixture and a source 18 of hydrochloric acid. A resultant solution 20 from the tank 12 is directed to an anionic affinity bed 22 [0024] A remaining solution 24 from the bed 22 flows to a nickel selective resin bed 26.
Washing the bed 26 with an acid from a source 28 of acid elutes a nickel product 30 and a substantially nickel-free solution 32 is relinquished from the bed 26.
[0025] A cobalt eluate 34 is released from the affinity bed 22 after washing the bed 22 with a chloride solution 36 from the chloride salt source 14.
[0026] The cobalt eluate 34 reports to a cobalt selective resin bed 38. Washing the bed 38 with an acid from the source 28 of acid elutes a cobalt product 40. A substantially cobalt-free eluate 42 leaves the bed 38.
[0027] In use a finely divided nickel-cobalt mixture from the source 16 is fed at a controlled rate to the tank 12, subsequent to the controlled introduction of a hydrochloric acid solution from the source 18 and a saturated chloride salt solution from the source
14.
[0028] The saturated chloride salt solution can be produced from any suitable chloride salt. Sodium chloride is preferably used as it is easily obtainable and cheap.
[0029] The addition of the hydrochloric acid solution to the saturated chloride salt solution in the tank 12 generates a chloride solution of at least a seven molar chloride concentration, which is necessary for chloride to complex with cobalt, in the nickel- cobalt mixture, to form an anionic cobalt-chloride complex [CoCU]2". [0030] Heating and stirring of the mixture of nickel-cobalt, hydrochloric acid and chloride salt in the tank 12, yields a resultant solution 20. The heating and stirring enhances the formation of the anionic cobalt-chloride complex.
[0031] The resultant solution 20 reports to and percolates through the anionic affinity resin bed 22 which contains a resin that can work either by an anion exchange or an anion chelating action. In the preferred embodiment the resin is a commercially available strong base anion exchange resin in a polystyrenic or acrylic matrix.
[0032] The cobalt-chloride complex, due to its anionic nature, is retained on the resin in the bed 22 whilst the remaining solution 24, now a substantially cobalt-free solution, passes from the bed 22.
[0033] The remaining solution 24 then reports to the nickel selective resin bed 26. A specific nickel selecting chelating resin is contained within the nickel selective resin bed 26. As the remaining solution 24 permeates the bed 26, nickel is adsorbed to the nickel selective resin and a remainder of the remaining solution 24, now a substantially nickel- free solution 32, is relinquished from the bed 26.
[0034] Washing the bed 26, with any suitable acid from the acid source 28, releases the nickel adsorbed to the nickel selective resin and a nickel product 30 is eluted.
[0035] To release cobalt from the chloride complex, retained in the bed 22, a chloride solution 36, with the addition of water, is used to wash the bed 22. The added water facilitates the dilution of the chloride solution 36 to a less than seven molar chloride solution. The chloride solution 36 is drawn from the chloride salt source 14 prior to entry of the saturated chloride salt solution to the tank 12. A cobalt eluate 34 issues from the bed 22. The chloride solution 36 needs to be less than a seven molar solution to reverse the complexing of chloride with cobalt.
[0036] The cobalt eluate 34 reports to a cobalt selective resin bed 38. A strong acid cation exchange resin is preferably used as a cobalt selective resin within the cobalt selective resin bed 38. As the cobalt eluate 34 flows through the bed 38, cobalt is adsorbed to the cobalt selective resin and the remainder of the eluate 34, now a substantially cobalt-free eluate 42, passes through the bed 38.
[0037] Washing the bed 38, with any suitable acid from the acid source 28, releases the cobalt adsorbed to the cobalt selective resin and a cobalt product 40 is eluted.
[0038] It is advantageous to use the apparatus 10 with the method of invention, with its reliance on a chloride salt as a source of chloride, as the chloride solution of at least a seven molar concentration is produced without need to revert to a strong solution of hydrochloric acid. Hydrochloric acid is expensive, it cannot be practically recycled, and it is difficult to dispose of when taking environmental considerations into account. A strong solution of hydrochloric acid is highly corrosive, produces toxic fumes and is hazardous to use.
[0039] The use of a chloride salt allows an additional recycle step to be incorporated into the method of the invention. The substantially nickel-free solution 32 which is also substantially devoid of cobalt, and the substantially cobalt-free solution 42 which is also substantially devoid of nickel, can be recycled to the chloride salt source 14.
[0040] Additionally, the nickel product 30 can be neutralized with a sodium hydroxide solution before being pressed and filtered to recover nickel in a substantially pure metallic form. Similarly the cobalt product 40 can be neutralized with sodium carbonate before being pressed and filtered to recover the cobalt in a substantially pure metallic form.

Claims

1. A< methΘd of separating nickel from cobalt in a nickel-cobalt mixture which includes the step of dissolving the mixture in a mixed chloride solution to form an anionic cobalt chloride complex in a resultant solution, and wherein the chloride content of the mixed chloride solution originates from at least two different chloride sources.
2. A method according to claim 1 which includes the step of selecting each chloride source from a suitable chloride salt and hydrochloride acid.
3. A method according to claim 1 or 2 which includes the step of heating the resultant solution to enhance the formation of the cobalt chloride complex.
4. A method according to any one of claims 1 to 3 which includes the step of separating the cobalt chloride complex from the resultant solution by allowing the resultant solution to percolate through a bed of resin having an affinity for anions so that the cobalt chloride complex is absorbed by a resin in the bed and allowing a remaining solution, which is substantially cobalt-free, to pass through the bed.
5. A method according to claim 4 wherein a chloride wash solution is applied to the resin bed to produce a cobalt eluate from which cobalt is recovered.
6. A method according to claim 5 wherein cobalt is recovered by passing the cobalt eluate through a cobalt selective resin bed so that the cobalt is adsorbed by a resin in the selective resin bed, and allowing the remaining eluate, a substantially cobalt-free eluate, to pass through the selective resin bed.
7. A method according to claim 6 which includes the step of recycling the cobalt free eluate to a chloride salt source.
8. A method according to any one of claims 4 to 7 which includes the step of removing nickel from the remaining solution thereby to produce a substantially nickel-free solution.
9. A method according to claim 8 which includes the step of recycling the substantially nickel-free solution to a chloride salt source.
10. A method according to claim 8 or 9 wherein the nickel is removed by passing the remaining solution through a nickel selective resin bed so that the nickel is adsorbed by a resin in the resin bed. And the nickel is then eluted and recovered from the nickel selective resin.
PCT/ZA2006/000054 2005-04-18 2006-04-13 Separation of nickel from cobalt by using chloridizing solution and cobalt-selective resin WO2006113944A1 (en)

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ZA2005/03095 2005-04-18
ZA200503095 2005-04-18

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2514242C1 (en) * 2012-09-27 2014-04-27 Лидия Алексеевна Воропанова Sorption extraction of cobalt ions from acidic chloride solutions
CN110819800A (en) * 2019-12-07 2020-02-21 怀化炯诚新材料科技有限公司 Method for recovering metal from laterite-nickel ore leaching solution by resin

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3650688A (en) * 1968-10-23 1972-03-21 Metalimpex Acel Es Femkulkeres Industrial process for separation of nickel
US3656940A (en) * 1968-06-21 1972-04-18 Nickel Le Process for the purification of nickel containing solutions
JPS52144319A (en) * 1976-05-28 1977-12-01 Pacific Metals Co Ltd Separating and removing method of cobalt and zinc from chloride solution
SU592859A1 (en) * 1976-02-04 1978-02-15 Ордена Трудового Красного Знамени Институт Физической Химии Ан Ссср Method of separating metal salts
NL8403683A (en) * 1984-12-04 1986-07-01 Tno Recovering heavy metals from sediments and sludges - by acidifying and adjusting chloride ion content to solubilise the metals as chloride complexes, and passing over anion exchanger
US5667665A (en) * 1995-03-14 1997-09-16 Japan Energy Corporation Process of producing high purity cobalt
JP2001020021A (en) * 1999-07-02 2001-01-23 Kojundo Chem Lab Co Ltd Manufacture of high purity cobalt

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3656940A (en) * 1968-06-21 1972-04-18 Nickel Le Process for the purification of nickel containing solutions
US3650688A (en) * 1968-10-23 1972-03-21 Metalimpex Acel Es Femkulkeres Industrial process for separation of nickel
SU592859A1 (en) * 1976-02-04 1978-02-15 Ордена Трудового Красного Знамени Институт Физической Химии Ан Ссср Method of separating metal salts
JPS52144319A (en) * 1976-05-28 1977-12-01 Pacific Metals Co Ltd Separating and removing method of cobalt and zinc from chloride solution
NL8403683A (en) * 1984-12-04 1986-07-01 Tno Recovering heavy metals from sediments and sludges - by acidifying and adjusting chloride ion content to solubilise the metals as chloride complexes, and passing over anion exchanger
US5667665A (en) * 1995-03-14 1997-09-16 Japan Energy Corporation Process of producing high purity cobalt
JP2001020021A (en) * 1999-07-02 2001-01-23 Kojundo Chem Lab Co Ltd Manufacture of high purity cobalt

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
DATABASE WPI Section Ch Week 197803, Derwent World Patents Index; Class M25, AN 1978-05338A, XP002396034 *
DATABASE WPI Section Ch Week 197901, Derwent World Patents Index; Class A91, AN 1979-01590B, XP002395997 *
DATABASE WPI Section Ch Week 198631, Derwent World Patents Index; Class D15, AN 1986-202748, XP002395998 *
PATENT ABSTRACTS OF JAPAN vol. 2000, no. 16 8 May 2001 (2001-05-08) *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2514242C1 (en) * 2012-09-27 2014-04-27 Лидия Алексеевна Воропанова Sorption extraction of cobalt ions from acidic chloride solutions
CN110819800A (en) * 2019-12-07 2020-02-21 怀化炯诚新材料科技有限公司 Method for recovering metal from laterite-nickel ore leaching solution by resin

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