WO2006000880A1 - Method for producing nickelic hydroxide - Google Patents

Method for producing nickelic hydroxide Download PDF

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Publication number
WO2006000880A1
WO2006000880A1 PCT/IB2005/001756 IB2005001756W WO2006000880A1 WO 2006000880 A1 WO2006000880 A1 WO 2006000880A1 IB 2005001756 W IB2005001756 W IB 2005001756W WO 2006000880 A1 WO2006000880 A1 WO 2006000880A1
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WO
WIPO (PCT)
Prior art keywords
electrolyte
hydroxide
process according
nickel
impurities
Prior art date
Application number
PCT/IB2005/001756
Other languages
French (fr)
Inventor
Douglas Charles Alexander
Jacobus Schulze-Messing
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Anglo Operations Limited
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 Anglo Operations Limited filed Critical Anglo Operations Limited
Publication of WO2006000880A1 publication Critical patent/WO2006000880A1/en

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/04—Oxides
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
    • C25C1/06—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese
    • C25C1/08—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese of nickel or cobalt

Definitions

  • This invention relates to a method of preparing nickelic hydroxide from nickelous hydroxide through reaction with gas mixture of sulphur dioxide and oxygen.
  • a conventional method for the removal of cobalt from a nickel electrolyte solution is through the electrolytic production of nickelic hydroxide, which is able to precipitate the cobalt from solution.
  • the nickelic hydroxide is obtained by a two- step process that entails first preparing a nickelous hydroxide compound and then oxidising the nickelous hydroxide compound through an electrolytic cell to form nickelic hydroxide. This nickelic hydroxide is then used to purify the nickel electrolyte by oxidising and precipitating the soluble cobalt from the electrolyte.
  • a process for producing nickelic hydroxide from nickelous hydroxide including the step of oxidising the nickelous hydroxide in the presence of oxygen and sulphur dioxide.
  • the oxygen source may be air.
  • a gas mixture of less than about 15% sulphur dioxide in oxygen, or less than about 3% sulphur dioxide in air, may be used to oxidise the nickelous hydroxide to nickelic hydroxide. More particularly, the gas mixture may comprise about 6% sulphur dioxide in oxygen, or about 1% sulphur dioxide in air.
  • the pH of the process may be in the range of from about pH 6 to about pH 10.
  • a neutralising agent may be used to control the pH of the process.
  • the neutralising agent may be a basic solution, such as sodium hydroxide.
  • the temperature of the process may be in the range of from about 20 to about 90 0 C, and more particularly about 30 0 C.
  • the nickelous hydroxide may be produced from a substantially pure nickel electrolyte, and preferably from a nickel electrolyte having a cobalt concentration of less than one part per million.
  • a process for removing impurities from a nickel electrolyte including the steps of: adding nickelic hydroxide to the electrolyte, to oxidise impurities, prepared according to the above process; causing the oxidised impurities to precipitate out of the electrolyte; and separating the precipitate from the electrolyte.
  • the impurities in the electrolyte may be cobalt, such as Co 2+ and/or Co 3+ ions.
  • the precipitate is preferably formed from Co 3+ ions.
  • a process for electrowinning nickel from a nickel electrolyte including the steps of: (a) oxidising nickelous hydroxide to nickelic hydroxide in the presence of sulphur dioxide and oxygen; (b) adding the nickelic hydroxide to the nickel electrolyte; (c) oxidising at least some of the impurities; (d) precipitating the impurities out of the electrolyte; (e) separating the precipitate from the electrolyte; and (T) electrowinning nickel from the nickel electrolyte.
  • the impurities in the electrolyte may be cobalt.
  • Figure 1 shows a schematic outline for producing nickelic hydroxide from nickelous hydroxide and using the nickelic hydroxide to remove cobalt from a cobalt containing electrolyte according to the invention.
  • the invention provides a process for producing nickelic hydroxide.
  • the nickelic hydroxide (Ni(OH) 4 ) is produced by oxidising nickelous hydroxide (Ni(OH) 2 ) in the presence of a gas mixture of sulphur dioxide and oxygen.
  • the nickelic hydroxide is typically used to remove impurities such as cobalt from a nickel electrolyte.
  • the process is illustrated in Figure 1. While the nickel in nickelic hydroxide is referred to herein as being in the +4 oxidation state, in the art it is sometimes illustrated as being in the +3 oxidation state, i.e. Ni(OH) 3 , where it is understood that the active component in the nickelic compound is Ni(OH) 4 .
  • a cobalt-free nickel electrolyte is treated in a reactor to produce a nickelous hydroxide precipitate.
  • This step can be performed using standard processes which are known to those skilled in the art.
  • the nickelous hydroxide precipitate is then oxidised to nickelic hydroxide by sparging with a mixture of oxygen and sulphur dioxide, or with a mixture of air and sulphur dioxide.
  • the oxygen may be in either essentially pure form, or may be obtained from air.
  • the gas mixture generally includes less than about 15% sulphur dioxide in oxygen, or less than about 3% sulphur dioxide in air. More particularly, the gas mixture includes less than about 6% sulphur dioxide in oxygen, or less than about 1% sulphur dioxide in air.
  • the pH of the process typically is maintained in the range of from about pH 6 to about pH 10 so as to achieve adequate precipitation of the nickel. This can be achieved by using a neutralising agent, such as a solution of sodium hydroxide.
  • the temperature of the process is generally in the range of from about 20 to about 90 0 C, and more particularly about 30 0 C, depending on considerations such as the gas solubility at higher temperatures and the kinetics of the nickelic hydroxide formation.
  • the nickelic hydroxide produced according to the process described above may then be added to a reactor containing an impure nickel electrolyte so as to remove cobalt from the electrolyte prior to an electrowinning step.
  • the nickelic hydroxide will oxidise the Co 2+ in the electrolyte to Co 3+ , which precipitates as a cobaltic hydroxide (Co(OH) 3 ).
  • a solid-liquid separation step such as filtration, is then carried out to separate the cobalt precipitate (cake) from the nickel electrolyte.
  • the cobalt-containing cake can be treated in a conventional manner to recover the cobalt and any nickel residues therein.
  • a 90 g/l nickel sulphate solution was heated to 30 degrees Celsius in a reactor, and the pH of this solution was adjusted with a solution of NaOH to pH 9.5. This produced a nickelous hydroxide slurry.
  • a gas mixture of 6% SO 2 and 94% oxygen was then sparged into the nickelous hydroxide slurry, whilst maintaining the pH at 9.5 with a sodium hydroxide solution.
  • a nickelic hydroxide precipitate was formed due to the oxidative properties of the gas mixture.
  • the nickelic hydroxide produced was transferred into a second reactor containing a solution of cobalt (500 mg/l) at a pH of 6.0 and a temperature of 45 degrees Celsius.
  • the nickelic hydroxide oxidised the soluble cobalt into the Co 3+ state, which readily formed an insoluble cobaltic hydroxide.
  • the pH of this cobalt containing solution was not controlled.
  • the cobalt in solution decreased from 500 mg/l to less than 0.5 mg/l in 60 minutes.
  • a 90 g/l nickel sulphate solution was heated to 45 degrees Celsius in a reactor, and the pH of this solution was adjusted with a solution of NaOH to pH 9.5. This produced a nickelous hydroxide slurry.
  • a gas mixture of 6% SO 2 and 94% oxygen was then sparged into the nickelous hydroxide slurry, whilst maintaining the pH at 9.5 with a sodium hydroxide solution.
  • a nickelic hydroxide precipitate was formed due to the oxidative properties of the gas mixture.
  • the nickelic hydroxide produced was transferred into a second reactor containing a solution of cobalt (500 mg/l) at a pH of 6.0 and a temperature of 50 degrees Celsius.
  • the nickelic hydroxide oxidised the soluble cobalt into the Co 3+ state, which readily formed an insoluble cobaltic hydroxide.
  • the pH of this cobalt containing solution was not controlled.
  • the cobalt in solution decreased from 500 mg/l to less than 1 mg/I in 60 minutes.
  • the invention is advantageous in that it provides a process for removing cobalt that is simpler and more energy efficient than the known electrolytic process.
  • the electrolytic cells used to generate nickelic hydroxide may be converted to nickel electro-winning cells to boost nameplate nickel production capacity at minimal capital expense.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention provides a process for producing nickelic hydroxide from nickelous hydroxide, wherein the nickelous hydroxide is oxidised in the presence of oxygen and sulphur dioxide. A gas mixture of less than about 15% sulphur dioxide in oxygen, or less than about 3% sulphur dioxide in air, is typically used. The invention extends to a process for removing impurities from a nickel electrolyte, the process including the steps of oxidising impurities in the electrolyte by adding nickelic prepared according to the invention; causing the oxidised impurities to precipitate out of the electrolyte; and separating the precipitate from the electrolyte. The impurities in the electrolyte may be cobalt, such as Co2+ and/or Co3+ ions. The invention also extends to a process for electrowinning nickel from a nickel electrolyte, by adding nickelic hydroxide prepared according to the invention to the nickel electrolyte; oxidising at least some of the impurities, such as cobalt; precipitating the impurities out of the electrolyte; separating the precipitate from the electrolyte; and electrowinning nickel from the nickel electrolyte.

Description

METHOD FOR PRODUCING NICKELIC HYDROXIDE
BACKGROUND OF THE INVENTION
This invention relates to a method of preparing nickelic hydroxide from nickelous hydroxide through reaction with gas mixture of sulphur dioxide and oxygen.
When electro-winning nickel from nickel electrolytes, cobalt contained in the electrolyte will co-deposit with the nickel, thereby affecting the grade of the nickel metal deposited. It is therefore important to remove cobalt from the nickel bearing solution (electrolyte) prior to the electrolyte entering the electro-winning cells so as to ensure that the cobalt concentration in the nickel metal deposited will meet required specifications, typically metal containing greater than 99.98% nickel.
Both Co2+ and Ni2+ ions precipitate as hydroxides at pH values of 6.8, but Co3+ precipitates at pH 3. Therefore, to precipitate cobalt selectively from a nickel electrolyte, it is necessary first to oxidise the Co2+ ions to Co3+ (Habashi, 1999).
A conventional method for the removal of cobalt from a nickel electrolyte solution is through the electrolytic production of nickelic hydroxide, which is able to precipitate the cobalt from solution. The nickelic hydroxide is obtained by a two- step process that entails first preparing a nickelous hydroxide compound and then oxidising the nickelous hydroxide compound through an electrolytic cell to form nickelic hydroxide. This nickelic hydroxide is then used to purify the nickel electrolyte by oxidising and precipitating the soluble cobalt from the electrolyte.
A considerable disadvantage of using the electrolytic cell to oxidise the nickelous hydroxide, however, is the poor use of power. Current efficiency in this process is typically below 30%. The applicant has therefore identified a need for an alternative, simpler and more efficient process for removing cobalt from a nickel electrolyte solution.
SUMMARY OF INVENTION
According to a first embodiment of the invention, there is provided a process for producing nickelic hydroxide from nickelous hydroxide, the process including the step of oxidising the nickelous hydroxide in the presence of oxygen and sulphur dioxide.
The oxygen source may be air.
A gas mixture of less than about 15% sulphur dioxide in oxygen, or less than about 3% sulphur dioxide in air, may be used to oxidise the nickelous hydroxide to nickelic hydroxide. More particularly, the gas mixture may comprise about 6% sulphur dioxide in oxygen, or about 1% sulphur dioxide in air.
The pH of the process may be in the range of from about pH 6 to about pH 10. A neutralising agent may be used to control the pH of the process. The neutralising agent may be a basic solution, such as sodium hydroxide.
The temperature of the process may be in the range of from about 20 to about 900C, and more particularly about 300C.
The nickelous hydroxide may be produced from a substantially pure nickel electrolyte, and preferably from a nickel electrolyte having a cobalt concentration of less than one part per million.
According to a second embodiment of the invention, there is provided a process for removing impurities from a nickel electrolyte, the process including the steps of: adding nickelic hydroxide to the electrolyte, to oxidise impurities, prepared according to the above process; causing the oxidised impurities to precipitate out of the electrolyte; and separating the precipitate from the electrolyte.
The impurities in the electrolyte may be cobalt, such as Co2+ and/or Co3+ ions. The precipitate is preferably formed from Co3+ ions.
According to a third embodiment of the invention, there is provided a process for electrowinning nickel from a nickel electrolyte, the process including the steps of: (a) oxidising nickelous hydroxide to nickelic hydroxide in the presence of sulphur dioxide and oxygen; (b) adding the nickelic hydroxide to the nickel electrolyte; (c) oxidising at least some of the impurities; (d) precipitating the impurities out of the electrolyte; (e) separating the precipitate from the electrolyte; and (T) electrowinning nickel from the nickel electrolyte.
The impurities in the electrolyte may be cobalt.
BRIEF DESCRIPTION OF THE DRAWINGS
Figure 1 shows a schematic outline for producing nickelic hydroxide from nickelous hydroxide and using the nickelic hydroxide to remove cobalt from a cobalt containing electrolyte according to the invention.
DETAILED DESCRIPTION OF THE INVENTION
The invention provides a process for producing nickelic hydroxide. The nickelic hydroxide (Ni(OH)4) is produced by oxidising nickelous hydroxide (Ni(OH)2) in the presence of a gas mixture of sulphur dioxide and oxygen. The nickelic hydroxide is typically used to remove impurities such as cobalt from a nickel electrolyte. The process is illustrated in Figure 1. While the nickel in nickelic hydroxide is referred to herein as being in the +4 oxidation state, in the art it is sometimes illustrated as being in the +3 oxidation state, i.e. Ni(OH)3, where it is understood that the active component in the nickelic compound is Ni(OH)4.
A cobalt-free nickel electrolyte is treated in a reactor to produce a nickelous hydroxide precipitate. This step can be performed using standard processes which are known to those skilled in the art. The nickelous hydroxide precipitate is then oxidised to nickelic hydroxide by sparging with a mixture of oxygen and sulphur dioxide, or with a mixture of air and sulphur dioxide.
The oxygen may be in either essentially pure form, or may be obtained from air. Thus, the gas mixture generally includes less than about 15% sulphur dioxide in oxygen, or less than about 3% sulphur dioxide in air. More particularly, the gas mixture includes less than about 6% sulphur dioxide in oxygen, or less than about 1% sulphur dioxide in air.
The pH of the process typically is maintained in the range of from about pH 6 to about pH 10 so as to achieve adequate precipitation of the nickel. This can be achieved by using a neutralising agent, such as a solution of sodium hydroxide.
The temperature of the process is generally in the range of from about 20 to about 900C, and more particularly about 300C, depending on considerations such as the gas solubility at higher temperatures and the kinetics of the nickelic hydroxide formation.
The nickelic hydroxide produced according to the process described above may then be added to a reactor containing an impure nickel electrolyte so as to remove cobalt from the electrolyte prior to an electrowinning step. The nickelic hydroxide will oxidise the Co2+ in the electrolyte to Co3+, which precipitates as a cobaltic hydroxide (Co(OH)3).
A solid-liquid separation step, such as filtration, is then carried out to separate the cobalt precipitate (cake) from the nickel electrolyte. The cobalt-containing cake can be treated in a conventional manner to recover the cobalt and any nickel residues therein.
The present invention is further described by the following examples. Such examples, however, are not to be construed as limiting in any way either the spirit or scope of the invention.
EXAMPLE 1
A 90 g/l nickel sulphate solution was heated to 30 degrees Celsius in a reactor, and the pH of this solution was adjusted with a solution of NaOH to pH 9.5. This produced a nickelous hydroxide slurry. A gas mixture of 6% SO2 and 94% oxygen was then sparged into the nickelous hydroxide slurry, whilst maintaining the pH at 9.5 with a sodium hydroxide solution. A nickelic hydroxide precipitate was formed due to the oxidative properties of the gas mixture.
After a residence time of 300 minutes, the gas flow into the reactor was stopped. The nickelic hydroxide produced was transferred into a second reactor containing a solution of cobalt (500 mg/l) at a pH of 6.0 and a temperature of 45 degrees Celsius. The nickelic hydroxide oxidised the soluble cobalt into the Co3+ state, which readily formed an insoluble cobaltic hydroxide. The pH of this cobalt containing solution was not controlled. The cobalt in solution decreased from 500 mg/l to less than 0.5 mg/l in 60 minutes.
EXAMPLE 2
A 90 g/l nickel sulphate solution was heated to 45 degrees Celsius in a reactor, and the pH of this solution was adjusted with a solution of NaOH to pH 9.5. This produced a nickelous hydroxide slurry. A gas mixture of 6% SO2 and 94% oxygen was then sparged into the nickelous hydroxide slurry, whilst maintaining the pH at 9.5 with a sodium hydroxide solution. A nickelic hydroxide precipitate was formed due to the oxidative properties of the gas mixture.
After a residence time of 300 minutes, the gas flow into the reactor was stopped. The nickelic hydroxide produced was transferred into a second reactor containing a solution of cobalt (500 mg/l) at a pH of 6.0 and a temperature of 50 degrees Celsius. The nickelic hydroxide oxidised the soluble cobalt into the Co3+ state, which readily formed an insoluble cobaltic hydroxide. The pH of this cobalt containing solution was not controlled. The cobalt in solution decreased from 500 mg/l to less than 1 mg/I in 60 minutes.
The applicant believes that the invention is advantageous in that it provides a process for removing cobalt that is simpler and more energy efficient than the known electrolytic process. In addition, in specific applications where the process is converted from using electrolytic cells to using the process of the invention, the electrolytic cells used to generate nickelic hydroxide may be converted to nickel electro-winning cells to boost nameplate nickel production capacity at minimal capital expense.
While the invention has been described in detail with respect to specific embodiments thereof, it will be appreciated by those skilled in the art that various alterations, modifications and other changes may be made to the invention without departing from the spirit and scope of the present invention. It is therefore intended that the claims cover or encompass all such modifications, alterations and/or changes.

Claims

1. A process for producing nickelic hydroxide from nickelous hydroxide, the process including the step of oxidising the nickelous hydroxide in the presence of oxygen and sulphur dioxide.
2. A process according to claim 1 , wherein the oxygen source is air.
3. A process according to either of claims 1 or 2, wherein a gas mixture of less than about 15% sulphur dioxide in oxygen is used to oxidise the nickelous hydroxide to nickelic hydroxide.
4. A process according to claim 3, wherein the gas mixture includes about 6% sulphur dioxide in oxygen.
5. A process according to either of claims 1 or 2, wherein a gas mixture of less than about 3% sulphur dioxide in air is used to oxidise the nickelous hydroxide to nickelic hydroxide.
6. A process according to claim 5, wherein the gas mixture includes about 1% sulphur dioxide in air.
7. A process according to any one of claims 1 to 6, which is carried out at a pH in the range from about pH 6 to about pH 10.
8. A process according to any one of claims 1 to 7, wherein a neutralising agent is used to control the pH of the process.
9. A process according to claim 8, wherein the neutralising agent is a basic solution.
10. A process according to claim 9, wherein the neutralising agent is sodium hydroxide.
11. A process according to any one of claims 1 to 10, which is carried out at a temperature in the range of from about 20 to about 90°C.
12. A process according to claim 11 , wherein the temperature is about 300C.
13. A process according to any one of claims 1 to 12, wherein the nickelous hydroxide is produced from a substantially pure nickel electrolyte.
14. A process according to any one of claims 1 to 13, wherein the nickelous hydroxide is produced from a nickel electrolyte having a cobalt concentration of less than one part per million.
15. A process for removing impurities from a nickel electrolyte, the process including the steps of: adding nickelic hydroxide to the electrolyte to oxidise impurities, the nickelic hydroxide having been prepared by oxidising nickelous hydroxide in the presence of oxygen and sulphur dioxide; causing the oxidised impurities to precipitate out of the electrolyte; and separating the precipitate from the electrolyte.
16. A process according to claim 15, wherein the impurities in the electrolyte are cobalt.
17. A process according to claim 16, wherein the cobalt impurities are selected from Co2+ and Co3+ ions.
18. A process according to claim 17, wherein the precipitate is formed from Co3+ ions.
19. A process for electrowinning nickel from a nickel electrolyte, the process including the steps of: (a) oxidising nickelous hydroxide to nickelic hydroxide in the presence of sulphur dioxide and oxygen; (b) adding the nickelic hydroxide to the nickel electrolyte; (c) oxidising at least some of the impurities; (d) precipitating the impurities out of the electrolyte; (e) separating the precipitate from the electrolyte; and (f) electrowinning nickel from the nickel electrolyte.
20. A process according to claim 19, wherein the impurities in the electrolyte are cobalt.
21. A process according to claim 1 , substantially as herein described with reference to either of the illustrative examples.
22. A process according to claim 15, substantially as herein described with reference to either of the illustrative examples.
23. A process according to claim 19, substantially as herein described with reference to either of the illustrative examples.
PCT/IB2005/001756 2004-06-21 2005-06-21 Method for producing nickelic hydroxide WO2006000880A1 (en)

Applications Claiming Priority (2)

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ZA200404884 2004-06-21
ZA2004/4884 2004-06-21

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3933976A (en) * 1974-02-08 1976-01-20 Amax Inc. Nickel-cobalt separation
US4006216A (en) * 1975-07-28 1977-02-01 The International Nickel Company, Inc. Preparation of nickel black

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3933976A (en) * 1974-02-08 1976-01-20 Amax Inc. Nickel-cobalt separation
US4006216A (en) * 1975-07-28 1977-02-01 The International Nickel Company, Inc. Preparation of nickel black

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
DATABASE CA [online] CHEMICAL ABSTRACTS SERVICE, COLUMBUS, OHIO, US; 1995, ZHAN, HUIFANG: "Study on the technology of cobalt removal with Ni(OH)3", XP002345512, retrieved from STN Database accession no. 124:122648 *
DATABASE CA [online] CHEMICAL ABSTRACTS SERVICE, COLUMBUS, OHIO, US; 2001, PROKOPCIKAS, A.: "Physicochemical properties of Ni(OH)3 and Ni(OH)4", XP002345513, retrieved from STN Database accession no. 58:11505 *
KUANGYE (BEIJING) , 4(3), 49-54 CODEN: KUANEN; ISSN: 1005-7854, 1995 *
LIETUVOS TSR MOKSLU AKAD. DARBAI, SER. B , (NO. 2), 31-6, 1962 *

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