US2793936A - Method of separating nickel and cobalt compounds from each other - Google Patents

Method of separating nickel and cobalt compounds from each other Download PDF

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Publication number
US2793936A
US2793936A US521837A US52183755A US2793936A US 2793936 A US2793936 A US 2793936A US 521837 A US521837 A US 521837A US 52183755 A US52183755 A US 52183755A US 2793936 A US2793936 A US 2793936A
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United States
Prior art keywords
nickel
cobalt
trivalent
hydroxides
hydroxide
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Expired - Lifetime
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US521837A
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English (en)
Inventor
Voos Walter
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Lonza Electric and Chemical Works Ltd
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Lonza Electric and Chemical Works Ltd
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    • 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
    • C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C01G51/04—Oxides
    • 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
    • C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
    • 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
    • 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
    • C22B3/262—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds using alcohols or phenols
    • 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
    • C22B3/30—Oximes
    • 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 to a method of separating nickel and cobalt compounds from each other, and more particularly to the separation of nickel and cobalt which are in the form of divalent and trivalent mixed hydroxides thereof from each other.
  • the present invention mainly consists in a method of separating nickel and cobalt compounds from each other, comprising the Steps of oxidizing a mixture of nickel and cobalt hydroxides, at least a portion of which are in divalent form, so as to form a mixture of trivalent nickel hydroxide and trivalent cobalt hydroxide, and extracting the thus-formed mixture of trivalent nickel and cobalt hydroxides with an aqueous chlorine-containing liquor in an amount suiicient to cause dissolution of substantially all of the trivalent nickel hydroxide, the trivalent cobalt hydroxide remaining undissolved, thereby separating the nickel hydroxide from the cobalt hydroxide.
  • the oxidation is preferably carried out in a liquid medium in which the mixtureof divalent ,and trivalent-nickel landcobalt hydroxides is insoluble.
  • the liquid ice medium is an aqueous medium and in such case the amount of the aqueous medium with reference to the amount of the mixed hydroxides should be such that a slurry or pasty mixture is formed.
  • the oxidation is most preferably carried out by means of a chlorine-containing solution or a solution which gives up chlorine, e. g., by an aqueous solution containing chlorine, a soluble chlorate or hypochlorite.
  • any other suitable oxidation agent may be utilized provided no undesirable residue from the oxidation remains.
  • the oxidation is preferably carried out at room temperature, although higher temperatures may be utilized within practical limits; for example, inthe case of utilizing chlorine as the oxidizing agent a temperature of C. should not be exceeded in order to prevent the chlorine from volatilizing. Temperatures of 40-50 C. are most suitable.
  • the oxidized hydroxides e. g., trivalent nickel and cobalt hydroxides
  • the oxidized hydroxides are separated from the liquid medium by filtration or, preferably, centrifugation.
  • the mixture of trivalent nickel and cobalt hydroxides are then subject to extraction by means of a large amount of a chlorine-containing aqueoussolution whereby substantially all of the trivalent nickel hydroxide goes into solution while substantially all of the trivalent cobalt ⁇ hydroxide remains undissolved.
  • the nickel hydroxide and the cobalt hydroxide may then be recovered separately by any suitable means.
  • the extracting agent must be an aqueous solution of chlorine.
  • the aqueous solution is preferably saturated with chlorine and, in order to increase the amount of chlorine which the solution may contain and thereby to increase the dissolving ability for trivalent nickel hydroxide of the solution, the aqueousl solution should also contain a carrier salt which has the property of permitting the aqueous solution to Ihold more chlorine and simultaneously aid in the extraction of the trivalent nickel hydroxide.
  • Such carrier salt is preferably the chloride of a metal, the hydroxide of which is water soluble.
  • a metal the hydroxide of which is water soluble.
  • sodium chloride, calcium chloride are suitable for this purpose.
  • Sodium chloride is, of course, most preferred for reasons of ready availability and economy.
  • the aqueous extracting solution preferably contains between 50 and 500g. per liter of sodium chloride, most preferably between 200 and 300 g. per liter.
  • the solution is further preferably saturated with chlorine.
  • the amount of the aqueous chlorine-containing solu-' tion can be varied within rather Wide limits. Generally at least 500 liters of the aqueous solution per 30 kg. of the hydroxides is needed in order to assure dissolution of all of the trivalent nickel hydroxide, although the amount of course depends upon the amount of trivalent nickel hydroxide in the mixture of trivalent nickel and cobalt hydroxides. There is actually no maximum amount of solution which may be used, although as a practical matter, in order to avoid the necessity of extremely large apparatus, the amount of solution should not exceed 3,000 liters per kg. of the hydroxides. Most preferably, between 1500 and 2000 liters per 180 kg. is
  • the extraction is preferably carried out at a temperature between 50-l00 C., rand most preferably between 90-95 C.
  • the extraction results in dissolving of the, trivalent nickel hydroxide in the chlorine-containing so- 1ution,'while the trivalent cobalt hydroxide remains undissolved.
  • the leaching or extraction of the mixed hydroxides can be so carried out until the regular control of thebottom residue, depending upon the requirements of the operation, shows only traces of the nickel, or until the leached product is free of nickel.
  • the separation o f the nickel from the cobalt can be carried out to a degree of 100% so that in the nickel solution no cobalt is'present as shown by means of a-nit'roso--naphthol, while in the cobalt residue no nickel is present as can be shown by means of dimethylglyoxime.
  • the oxidation is preferably carried out in a vessel provided with a stirrer in which the mixed hydroxide is stirred with the small amount of oxidizing solution in the form of a slurry until lthe desired conversion of thenickel and cobalt into the trivalent form is achieved.
  • the leaching or extracting of the trivalent nickel hydroxide from the trivalent cobalt hydroxide is carried out in suspensions in larger amounts of liquid and can also be carried out in vessels provided with stirrers, although to improve the extraction it is also possible to operate in an autoclave under pressure.
  • the extracted most pure nickel solution or the remainingmost pure cobaltic hydroxide can by any suitable 'means be worked up into pure salts, oxides, catalysts, reducing metals, hard metals, electrolyte metals, or metal powders, while the aqueous chlorine-containing solution which would generally also contain a carrier salt, such as the sodium chloride, can be recovered and/or recirculated for further extraction.
  • a carrier salt such as the sodium chloride
  • Example 1 180 kg. of mixed hydroxide of cobalt and nickel including divalent and trivalent hydroxides of each (the ratio of cobalt to nickel being :1) are introduced into a container and 90 kg. of tap water, e. g., an amount sufcient to form only a slurry, is added.
  • the thus obtained slurry is subjected to an oxidizing treatment in which, while stirring atvroom temperature, chlorine gas in fine subdivision is introduced into the slurry until the metal hydroxide mixture has a black color through and through indicating that both the nickel and the cobalt are in trivalentform.
  • the oxidized slurry is then introduced into a centrifuge and there the solid particles are separated from the liquid by centrifugation.
  • the spent liquor can serve for the treatment of fresh raw material.
  • the extraction is then carried out as follows: The mixture of trivalent cobalt and nickel obtained by the oxidation of the 180 kg. of the mixed hydroxides, which trivalent compounds are in the form of a 180 kg. cake, are added to the solution slowly while stirring. After the introduction is completed the leaching is continued for 30 minutes at 90-95 C. and thereafter the aqueous solution content of chlorine gas is renewed. Alternate periods of 30 minutes extraction and renewed addition of chlorine gas are continued until the desired purity of the cobalt hydroxide is achieved. The separation of the nickel and mother liquor or the later precipitated wash water from the liquor residue from the cobaltic hydroxide is carried out by centrifugation. The nickel containing liquor and the cobaltic hydroxide can be further worked up to the desired end product while the wash water can be utilized .for treatment of additionalA raw material.
  • Example 2 200 kg. of a mixture of cobalt and nickel divalent and trivalent hydroxides (ratio of cobalt to nickel being 1:1) are introduced into a container with only so much tap water as to form a slurry, i. e., with 60 kg. of tapwater.
  • the thus obtained slurry is subjected to an oxidation treatment wherein under stirring at room temperature chlorine gas is introduced in finest subdivision until the metal hydroxide mixture has a black color through and through indicating the trivalent form of the metals.
  • This mass is introduced into centrifuge and there subjected to centrifugation.
  • the spent liquor can servefor the treatment of fresh raw material.
  • the extraction is then carried out by the addition of the mixed trivalent hydroxides to the solution slowly while stirring. After introduction of all of the hydroxides the leaching is continued for 20 minutes at 85-90 C. and thereupon the solution is again saturated with chlorine gas. AlternateV SO-minute extractions and renewed additions of chlorine gas are continued until the desired purity of the cobaltic hydroxide has been obtained.
  • the separation of the nickel mother liquor or the later precipitated wash water from the leaching residue from the cobaltic hydroxide is accomplished by means of a centrifuge.
  • a method of completely separating nickel and cobalt compounds from each other comprising the steps of subjecting a mixture of nickel and cobalt hydroxides at least a portion of which are in divalent form to oxidation in an aqueous medium, said aqueous medium being in an amount of -60% by weight of said mixture of nickel and cobalt hydroxides so that said aqueous medium and said mixture of nickel and coalt hydroxides is in the form of a pasty mass, thereby forming a mixture of 'trivalent nickel hydroxide and trivalent cobalt hydroxide distributed in said aqueous medium; separating said trivalent nickel and cobalt hydroxides from said aqueous medium; and extracting the thus formed mixture of trivalent nickel and cobalt hydroxides with an aqueous chlorine-containing liquor in an amount suflicient to cause dissolution of all of said trivalent nickel hydroxide, said trivalent cobalt hydroxide remaining undissolved, thereby separating said nickel hydroxide from said cobalt hydroxide.
  • a method of completely separating nickel and cobalt compounds from each other comprising the steps of subjecting a mixture of nickel and cobalt hydroxides at least a portion of which are in divalent form to oxidation by means of chlorine in an aqueous medium, said aqueous medium'being in an amount of 10-60% by Weight of said mixture of nickel and cobalt hydroxides so that said aqueous medium and said mixture of nickel and cobalt hydroxides is in the form of a pasty mass, thereby forming a mixture of trivalent nickel hydroxide and trivalent cobalt hydroxide distributed in said aqueous medium; separating said trivalent nickel and cobalt hydroxides from said aqueous medium; and extracting the thus 6 formed mixture of trivalent nickel and cobalt hydroxides with an aqueous solution ot sodium chloride containing y also chlorinein an amount sulcient to cause dissolution of all of said trivalent nickel hydroxide, said trivalent cobalt hydroxide remaining undissolved, thereby separating
  • a method of completely separating nickel and cobalt compounds from each other comprising the steps of subjecting a mixture of nickel and cobalt hydroxides at least a portion of which are in divalent form to oxidation in an aqueous medium, said aqueous medium being in an amount of lO-60% by weight of said mixture of nickel and cobalt hydroxides so that said aqueous medium and said mixture of nickel and cobalt hydroxides is in the form of a pasty mass, thereby forming a mixture of trivalent nickel hydroxide and trivalent cobalt hydroxide; separating said trivalent nickel and cobalt hydroxides from said aqueous medium; and extracting the thus formed mixture of trivalent nickel and cobalt hydroxides with an aqueous solution of sodium chloride saturated with chlorine and containing between 50 and 500 g.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Geology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Manufacture And Refinement Of Metals (AREA)
US521837A 1954-07-19 1955-07-13 Method of separating nickel and cobalt compounds from each other Expired - Lifetime US2793936A (en)

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BE (1) BE539910A (enrdf_load_html_response)
CH (1) CH328069A (enrdf_load_html_response)
DE (1) DE1041024B (enrdf_load_html_response)
FR (1) FR1134804A (enrdf_load_html_response)
GB (1) GB785350A (enrdf_load_html_response)

Cited By (4)

* 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
US5855858A (en) * 1993-07-29 1999-01-05 Cominco Engineering Services Ltd. Process for the recovery of nickel and/or cobalt from an ore or concentrate
US6054105A (en) * 1993-07-29 2000-04-25 Cominco Engineering Services Ltd. Process for the solvent extraction of nickel and cobalt values in the presence of magnesium ions from a solution
WO2006056610A1 (en) * 2004-11-29 2006-06-01 Shell Internationale Research Maatschappij B.V. Catalytic process for the conversion of co (ii)hydroxide in co (iii)oxidehydroxide

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1191856B (de) * 1957-04-18 1965-04-29 Sperry Rand Corp Schaltungsanordnung zur Impulsverstaerkung und -verzoegerung
NL7006861A (enrdf_load_html_response) * 1969-05-14 1970-11-17

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1596253A (en) * 1924-09-26 1926-08-17 Harshaw Fuller & Goodwin Compa Method of separating cobalt from nickel
GB570231A (en) * 1941-11-28 1945-06-28 Mond Nickel Co Ltd Improvements in the purification of cobaltic hydroxide
US2488561A (en) * 1943-09-30 1949-11-22 Ferro Enamel Corp Method for the separation of cobalt and nickel from solutions
US2726144A (en) * 1951-07-12 1955-12-06 Int Nickel Co Production of pure cobaltic hydroxide

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1596253A (en) * 1924-09-26 1926-08-17 Harshaw Fuller & Goodwin Compa Method of separating cobalt from nickel
GB570231A (en) * 1941-11-28 1945-06-28 Mond Nickel Co Ltd Improvements in the purification of cobaltic hydroxide
US2488561A (en) * 1943-09-30 1949-11-22 Ferro Enamel Corp Method for the separation of cobalt and nickel from solutions
US2726144A (en) * 1951-07-12 1955-12-06 Int Nickel Co Production of pure cobaltic hydroxide

Cited By (8)

* 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
US5855858A (en) * 1993-07-29 1999-01-05 Cominco Engineering Services Ltd. Process for the recovery of nickel and/or cobalt from an ore or concentrate
US6054105A (en) * 1993-07-29 2000-04-25 Cominco Engineering Services Ltd. Process for the solvent extraction of nickel and cobalt values in the presence of magnesium ions from a solution
US6383460B2 (en) 1993-07-29 2002-05-07 Cominco Engineering Services Ltd. Process for the recovery of nickel and/or cobalt from a concentrate
WO2006056610A1 (en) * 2004-11-29 2006-06-01 Shell Internationale Research Maatschappij B.V. Catalytic process for the conversion of co (ii)hydroxide in co (iii)oxidehydroxide
US20080051474A1 (en) * 2004-11-29 2008-02-28 Dogterom Ronald J Catalytic Process For The Conversion Of Co (II)Hydroxide In Co (III)Hydroxide
AU2005308788B2 (en) * 2004-11-29 2009-04-30 Shell Internationale Research Maatschappij B.V. Catalytic process for the conversion of Co (II)hydroxide in Co (III)oxidehydroxide
US8062620B2 (en) 2004-11-29 2011-11-22 Shell Oil Company Catalytic process for the conversion of Co (II)hydroxide in Co (III)oxidehydroxide

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DE1041024B (de) 1958-10-16
FR1134804A (fr) 1957-04-18
CH328069A (de) 1958-02-28
GB785350A (en) 1957-10-23
BE539910A (enrdf_load_html_response) 1900-01-01

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