US3769002A - Reduction of nickel and cobalt oxides in a molten metal bath of controlled oxygen content - Google Patents

Reduction of nickel and cobalt oxides in a molten metal bath of controlled oxygen content Download PDF

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Publication number
US3769002A
US3769002A US00155354A US3769002DA US3769002A US 3769002 A US3769002 A US 3769002A US 00155354 A US00155354 A US 00155354A US 3769002D A US3769002D A US 3769002DA US 3769002 A US3769002 A US 3769002A
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bath
nickel
cobalt
oxygen
compound
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Neill C O
J Warner
M Bell
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Huntington Alloys Corp
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International Nickel Co Inc
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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
    • C22B23/02—Obtaining nickel or cobalt by dry processes

Definitions

  • the metal bath is maintained in the molten state by burning above the bath carbon monoxide generated in situ and hydrocarbon fuels with an excess of free oxygen. Impurities. oxidizable to volatile oxides can be eliminated by subjecting the oxygencontaining bath, or a part thereof, to subatmospheric pressures, or the metal bath can be surface blown with a free oxygen-containing gas to adjust the oxygen content of the bath before subatmospheric treatment.
  • This invention pertains to reducingmetaloxides and more particularly to reducing and refining metal oxides, including nickel and nickel-containing materials, by pyrometallurgical and vapometallurgical techniques.
  • Nickel oxide is frequently an intermediate product in the commercial recovery of nickel from its ores, whether oxide or sulfide.
  • nickel oxide is obtained by calcining precipitated basic nickel carbonate.
  • nickel sulfide concentrate obtained by matte separation including slow cooling and subsequent comminution, is roasted to nickel oxide.
  • Nickel oxide produced by either of these processes can be employed, if it is sufficiently pure, for alloying purposes. Often, however, a more pure form of nickel is required, and nickel oxide must be reduced for further refining. Sulfur contamination problems are frequently encountered during reduction of nickel oxide, unless more expensive fuels, deficient in sulfur, are employed.
  • metal oxides including nickel oxides, cobalt oxides and compounds heat decomposable thereto, can be directly and continuously melted and refined by a combination of pyrometallurgical and vapometallurgical operations.
  • the combination of processes allows the use of fuels containing substantial amounts of sulfur and also provides a process for lowering the content of impurities such as lead, zinc, cadmium, bismuth, antimony and other impurities which are volatile or have volatile oxides.
  • the product obtained by the process has a low content of dissolved gases and is particularly suitable for continuous casting.
  • a further object of the present invention is to provide a pyrometallurgical process for the direct and continuous production of metals, including nickel and cobalt from their oxides and compounds heat decomposable to their oxides.
  • the present invention contemplates a process for reducing metal oxides.
  • a turbulent bath of at least one metal selected from the group consisting of nickel and cobalt is established, which bath contains at least about 0.01 percent dissolved oxygen but not saturated therewith.
  • At least one compound selected from the group consisting of nickel oxide, cobalt oxide and compounds heat decomposable thereto and a carbonaceous reductant are fed to the turbulent bath while the dissolved oxygen content of the bath is maintained at at least 0.01 percent but less than saturation whereby the carbonaceous reductant-reacts with the dissolved oxygen in the bath to generate carbon monoxide.
  • the generated carbon monoxide and a fuel are burnt above the bath with a free-oxygen-containing gas to produce heat for maintaining the bath at operating temperatures.
  • feeding of the compound to the bath is terminated so that the dissolved oxygen content of the bath is reduced by the carbonaceous reductant.
  • a portion of the oxygen-containing bath can be teemed from the. furnace and then subjected to a subatmospheric pressure treatment for final impurity elimination.
  • the oxygen-containing bath can be directly subjected to a subatmospheric pressure treatment so that the oxidized impurities are more effectively volatized from the bath.
  • dissolved oxygen can be incorporated into the bath by surface blowing the bath with a free-oxygen-containing gas before the subatmospheric pressure treatment or by passing a free-oxygencontaining gas through the metal bath during the subatmo spheric pressure treatment.
  • Oxides, compounds heat decomposable to the oxides of nickel and cobalt, and materials containing these compounds can be treated in accordance with the process of the present invention.
  • Compounds heat decomposable to the oxides include, but are not limited thereto, hydroxides, carbonates, basic carbonates and nitrates of nickel and cobalt. These compounds are often produced by hydrometallurgical techniques and are contaminated by various impurities, most of which can be eliminated by practice of the process in accordance with the present invention.
  • Impurities which can be volatilizedor oxidizedand volatilized include antimony, bismuth, cadmium, lead, sulfur and zinc.
  • the total content of the aforementioned metallic impurities can amount to as much as about 0.5 percent while sulfur can amount to as much as about 3 percent, e.g, about 2 percent.
  • Compounds produced by hydrometallurgical techniques frequently contain nuisance amounts of gangue such as alumina, calcium, magnesia and silica and the process of the present invention provides a highly effective mode for separating these constituents from nickel and/or cobalt.
  • a highly important feature of the present invention is the exceptionally high production rates that are achieved by maintaining the oxygen content of theturbulent bath at at least about 0.01 percent, or about 0.02 percent and even higher, when the metal oxide and the reductant are being added to the bath.
  • high temperatures e.g., about 50C. or even C. above the melting point of the metal bath, and turbulence of the metal bath are the two factors that aremost important in controlling the oxygen content in the metal bath.
  • the metal bath is established in a top blown rotary furnace in which the bath can be independently agitated and maintained at high temperatures.
  • top blown rotary furnace has many advantages with the foremost being the independent control of temperature, atmosphere and agitation. Further advantages flowing from the use of top blown rotary converters include high thermal and chemical efficiencies provided by the rotating refractories and by the turbulence of the bath.
  • a carbonaceous reductant such as coal, coke, charcoal or even liquid hydrocarbons, is added to the oxygen-containing metal bath to reduce the dissolved oxygen.
  • the reduction reaction is so extremely rapid, particularly when conducted in a top blown rotary converter, that nickel oxide or cobalt oxide and the carbonaceous reductant can be added to the bath in a continuous or semicontinuous manner.
  • the reduction reaction is so rapid and energetic that a carbon monoxide boil can be observed.
  • Carbonaceous reductant is added to the oxygencontaining metalbath in amounts necessary to substantially satisfy the reduction stoichiometry and to provide carbon monoxide to at least partially satisfy the heat requirements. Greater amounts of reductant can be added to insure complete reduction and to act as a source of fuel which can be burned by reaction with free-oxygen-containing gases.
  • agglomeration reductant and fuel either liquid or solid, can be incorporated in the briquettes or pellets.
  • a highly advantageous embodiment is to incorporate into the pellets liquid hydrocarbons, such as Bunker C fuel oil during briquetting, so that at least part of the reductant and/or fuel can be added via the pellets.
  • the incorporation of liquid hydrocarbons during the briquetting operation has the further addition of lowering, or even eliminating, the use of water as a binder, thereby lowering fuel costs attributable to drying and vaporizing such water.
  • liquid hydrocarbon such as Bunker C oil
  • the amount of reductant incorporated in the pellets can vary within wide limits. Less than stoichiometric amounts of reductant can be incorporated in the briquettes with difference being made up by the addition of coke or other solid reductant to the bath. If more than stoichiometric amounts of reductant are incorporated in the briquetted nickel oxide or other compounds heat decomposable thereto, the oxygen content of the molten nickel bath can be maintained above about 0.01 percent by surface blowing the bath with a free-oxygen-containing gas to burn the excess reductant and to incorporate oxygen in the bath, or by the addition of reductant-free briquetted oxide. The presence of excess reductant is readily ascertained since the vigor of the carbon monoxide boil rapidly diminishes.
  • Heat can be supplied by burning above the bath carbon monoxide generated in situ or the carbonaceous reductant with a free-oxygen-containing gas and- /or by burning a fuel with a free-oxygen-containing gas in a burner provided for this purpose.
  • The'fuel can be the same as the reductant or can be gaseous (e.g., natural gas) and does not have to be sulfur free. Sufficient heat is generated by any or all of these methods to maintain the metal bath at a temperature of at least about 50C. or even C. above its melting point to promote dissolution of the oxide and to increase reduction kinetics.
  • An important feature of the present invention is the subatmospheric pressure treatment for final impurity elimination.
  • a bath containing the requisite amounts of dissolved oxygen can be produced in the vacuum unit and is advantageously so done during final impurity elimination.
  • the starting material contains large quantities, e.g., about 4 percent, of impurities which are volatile or oxidized to volatile species, the demands placed on the vacuum unit render such a procedure commercially impractical. Therefore, it is preferred, in most instances, to incorporate oxygen into the molten bath by other means.
  • the oxygen content of the bath can be controlled by terminating the addition of carbonaceous reductant to the bath while continuing the addition of oxides or by surface blowing the surface of the bath with a free-oxygencontaining gas.
  • a turbulent bath of at least one metal selected from the group consisting of nickel and cobalt and having at least 0.01 percent oxygen but not saturated therewith is established in a rotary converter that is provided with means for partially combusting hydrocarbon fuel above the bath to generate heat and means for surface blowing the metal bath with a gas containing free oxygen.
  • the rotary converter is rotated to maintain the metal bath in a turbulent state and briquetted oxides, or compounds heat decomposable to oxides, of nickel and cobalt are fed to the turbulent metal bath to maintain the dissolved oxygen in the bath at the aforedescribedlevels.
  • Carbonaceous reductants are added to the oxygen-containing metal bath to rapidly and energetically reduce the oxide fed to the bath.
  • the amounts of oxide and reductant added to the bath are proportioned to insure that the bath contains at least about 0.01 percent oxygen and does not reach saturation levels. Precautions need not be taken to insure that the fuel has a low sulfur content since sulfur absorbed by the bath will be subsequently removed by the subatmospheric pressure treatment.
  • Carbon monoxide generated by the reduction reactions, the carbonaceous reductant and fuel introduced via the burner are burned with an excess of free oxygen to maintain the bath at a temperature at least about 50C. above its melting point.
  • the additions of agglomerated oxide and solid reductants can be simultaneousor can be repeatedly alternated until the furnace capacity is approached. When the capacity of the furnace is approached, the oxygen content of the bath can be adjusted so that the metal can be cast into product form. Alternatively, the oxygen content of the bath can be adjusted for final impurity elimination during a subatmospheric pressure treatment.
  • the bath is subjected to a vacuum treatment for final impurity elimination. It is advantageous for thermodynamic and kinetic reasons to subject the metal bath to a vacuum of less than about 0.1 atmosphere and advantageously to a pressure less thanabout 0.01 atmosphere "or evenless than about 0.001 atmosphere. If the bath is deficient in oxygen, additional oxygen can be added thereto.
  • gaseous oxygen is introduced into the molten bath to overcome any oxygen deficiencies. The addition of oxygen during the low pressure treatment is advantageous in that it lessens the need to incorporate all the oxygen required for final impurity elimination by surface blowing during the smelting operation and thereof avoids the problems associated with possible formation of undesirable and inactive metal oxide dross. Gaseous oxygen can be added as air, oxygen-enriched air, preheated air or commercial oxygen.
  • the metal bath is maintained at a temperature of at least about 50C. above its melting point during the vacuum treatment. Even better results are obtained by maintaining the metal bath at a temperature of about 100C. above its melting point. Higher temperatures provide better results by increasing the vapor pressure of the volatile impurities, by thermodynamically insuring more complete reactions when impurities are being eliminated as volatile oxides and by the amount of dissolved oxygen to thereby increase the driving force of this oxidizing reaction.
  • impurities such as bismuth and lead can be eliminated to almost undetectable amounts.
  • the subatmospheric pressure treatment is advantageously continued after elimination of impurities without furtheroxygen'additions to degas the metal.
  • the metal bath can be finally deoxidized by the addition of carbon, silicon, aluminum, or calcium silicon.
  • Deoxidation can also be effected by lancing the turbulent bath with methane or other gaseous hydrocarbons or by passing a reducing gas containing carbon monoxide, hydrogen or methane through the molten bath or by surface blowing the bath with such reducing gases.
  • the melt is degassed under subatmospheric pressures to provide a final metal product that has a low content of dissolved gases which product is particularly suitable for continuous casting.
  • Refining and degassing can be conducted in a suitable vacuum chamber in which low pressures are maintained by mechanical pumps, steam ejector systems, or any other system capable of pumping large volumes of gas at low pressures.
  • the vacuum chamber is equipped with means for controlling the temperature of the molten bath.
  • the vacuum unit can be heated by induction or by carbon are or by other means.
  • the molten bath can be maintained in a state of turbulence while undergoing vacuum treatment by electromagnetic stirring or by pneumatic or mechanical means.
  • EXAMPLE I- A charge consisting of 1.5 inches X 1 inch X 1 inch briquettes of basic nickel carbonate analyzing approximately 54 percent nickel plus cobalt on a dry basis, and containing about 20 percent moisture was fed into a rotary converter operating at 20 revolutions per minute.
  • the converter contained a bath of molten nickel maintained at about 2,950F. and containing approximately 0.1 percent dissolved oxygen.
  • the carbonate was added at pounds per minute, and metallurgical coke at the rate of 9.6 pounds per minute. A very vigorous boil was maintained, and the carbonate and coke was almost immediately reacted.
  • the converter was maintained at between 2,900F. and 2,980F. 'by burning natural gas within excess of the stoichiometric requirement of oxygen.
  • the amount of oxygen was such that the gas exiting from the converter was contained between about 0 and 3 percent carbon monoxide.
  • the carbon monoxide from the reduction of nickel oxide by carbon was threfore being largely burned to carbon dioxide in the converter, supplying a significant portion of the heat requirements for the process. Dust losses to the converter stock were negligible.
  • the present invention provides a process for reducing metal compound.
  • the process comprises establishing a bath of at least one metal selected from the group consisting of nickel and cobalt, which bath contains at least about 0.1 percent dissolved oxygen (and advantageously at least about 0.'l
  • At least one compound selected from the group consisting of nickel oxide, cobalt acts with the dissolved oxygen in the bath to generate carbon monoxide.
  • the generated carbon monoxide and a fuel are burned above the bath with free-oxygencontaining gas to heat the bath to operating temperatures. A portion of reduced metal is recovered from the, bath.
  • a process for reducing a metal compound which comprises: establishing a bath of at least one metal selected from the group consisting of nickel and cobalt,
  • bath contains at least about 0.01 percent dissolved oxygen; feeding at least one compound selected from the group consisting of nickel oxide, cobalt oxide, and compounds heat decomposable thereto and a carbonaceous reductant to the bath while the dissolved oxygen content of the bath is maintained at at least about 0.01 percent whereby the carbonaceous reductant reacts with the dissolved oxygen in the bath to generate carbon monoxide; burning the generated carbon monoxide .and a fuel with a free-oxygen-containing gas above the bath to produce heat for maintaining the bath at operating temperatures; and recovering a portion of reduced metal from the bath.
  • a process for reducing a nickel compound which comprises: establishing a turbulent nickel bath which contains at least about 0.01 percent dissolved oxygen but not saturated therewith; feeding at least one nickel compound selected from the group consisting of nickel oxide and compounds heat decomposable thereto and a carbonaceous reductant to the nickel bath while maintaining the dissolved oxygen level of the nickel bath at at least about 0.01 percent but less than saturation whereby the carbonaceous reductant reacts with the dissolved oxygen content in the nickel bath to generate carbon monoxide; burning the generated carbon monoxide and a fuel with a free-oxygen-containing gas above the nickel bath to produce heat for maintaining the bath at operating temperatures; and recoverng nickel from the nickel bath.
  • a process for reducing a cobalt compound which comprises: establishing a turbulent cobalt bath containing at least about 0.01 percent dissolved oxygen but not saturated therewith; feeding at least one cobalt compound selected from the group consisting of cobalt oxide and compounds heat decomposable thereto and a carbonaceous reductant to the cobalt bath whereby the carbonaceous reductant reacts with the dissolved oxygen in the cobalt bath to generate carbon monoxide; burning the generated carbon monoxide and a fuel with a free-oxygen-containing gas above the cobalt bath to produce heat for maintaining the cobalt bath at operating temperatures; and recovering cobalt metal from the cobalt bath.
  • liquid hydrocarbon is incorporated in the briquettes in amounts in excess of that required to satisfy the stoichiometry of the reduction reactions and the surface of the metal bath is surface blown with a free-oxygencontaining gas to maintain the dissolvedoxygen content of the bath at at least about 0.01 percent.
  • nickel compound is nickel hydroxide 21.
  • nickel compound is basic nickel carbonate.

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US00155354A 1970-07-08 1971-06-21 Reduction of nickel and cobalt oxides in a molten metal bath of controlled oxygen content Expired - Lifetime US3769002A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3877933A (en) * 1973-09-21 1975-04-15 Int Nickel Co Metallurgical addition product
US5017220A (en) * 1989-02-21 1991-05-21 Nkk Corporation Method for smelting reduction of Ni ore
US5324341A (en) * 1992-05-05 1994-06-28 Molten Metal Technology, Inc. Method for chemically reducing metals in waste compositions
WO2009100495A1 (en) * 2008-02-12 2009-08-20 Bhp Billiton Innovation Pty Ltd Production of nickel
US20090249921A1 (en) * 2008-02-08 2009-10-08 Vale Inco Limited Process for production of nickel and cobalt using metal hydroxide, metal oxide and/or metal carbonate
US20110103998A1 (en) * 2007-10-26 2011-05-05 Ivan Ratchev Production of Nickel
FR3008426A1 (fr) * 2013-07-15 2015-01-16 Eramet Procede d'elaboration de nickel metallique a partir d'oxyde de nickel par fusion-reduction
US20220048790A1 (en) * 2018-09-26 2022-02-17 Panasonic Intellectual Property Management Co., Ltd. Method for producing nickel particles, method for producing nickel sulfate, and method for producing positive electrode active material for secondary batteries

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2134729C1 (ru) * 1998-02-12 1999-08-20 Попов Владимир Максимович Способ переработки окисленных никелевых руд
RU2132400C1 (ru) * 1998-09-03 1999-06-27 Открытое акционерное общество "Серовский металлургический завод" Способ переработки окисленных никелевых руд
RU2621496C2 (ru) * 2015-06-09 2017-06-06 Александр Александрович Веселовский Способ переработки окисленных никелевых руд и отвальных никелевых шлаков химико-термической обработкой

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US1828752A (en) * 1928-05-03 1931-10-27 Int Nickel Co Desulphurizing nickel-containing matte
US2740710A (en) * 1951-03-02 1956-04-03 Johannsen Friedrich Method for the production of iron, nickel, cobalt, manganese, and chromium from their ores
US2815279A (en) * 1953-11-02 1957-12-03 Nat Res Corp Process of preparing high purity nickel
US3030201A (en) * 1960-09-02 1962-04-17 Int Nickel Co Method of producing ferro-nickel from nickel-containing silicate ores
US3157489A (en) * 1961-03-09 1964-11-17 Pullman Inc Method for reducing metal oxides
US3169055A (en) * 1961-10-12 1965-02-09 Stora Kopparbergs Bergslags Ab Process for producing pig iron in rotary furnace
US3188196A (en) * 1963-06-19 1965-06-08 Pullman Inc Method for desiccating and reducing ore
US3188198A (en) * 1962-08-23 1965-06-08 Gen Electric Method for deoxidizing metals
US3326671A (en) * 1963-02-21 1967-06-20 Howard K Worner Direct smelting of metallic ores
US3425824A (en) * 1965-06-23 1969-02-04 Metallgesellschaft Ag Process of reducing metal ores
US3573894A (en) * 1965-03-18 1971-04-06 Pierre Marie Francois Fourt Process and plant for reducing metallic oxides
US3640701A (en) * 1964-04-30 1972-02-08 Creusot Loire Direct reduction of oxides

Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1828752A (en) * 1928-05-03 1931-10-27 Int Nickel Co Desulphurizing nickel-containing matte
US2740710A (en) * 1951-03-02 1956-04-03 Johannsen Friedrich Method for the production of iron, nickel, cobalt, manganese, and chromium from their ores
US2815279A (en) * 1953-11-02 1957-12-03 Nat Res Corp Process of preparing high purity nickel
US3030201A (en) * 1960-09-02 1962-04-17 Int Nickel Co Method of producing ferro-nickel from nickel-containing silicate ores
US3157489A (en) * 1961-03-09 1964-11-17 Pullman Inc Method for reducing metal oxides
US3169055A (en) * 1961-10-12 1965-02-09 Stora Kopparbergs Bergslags Ab Process for producing pig iron in rotary furnace
US3188198A (en) * 1962-08-23 1965-06-08 Gen Electric Method for deoxidizing metals
US3326671A (en) * 1963-02-21 1967-06-20 Howard K Worner Direct smelting of metallic ores
US3188196A (en) * 1963-06-19 1965-06-08 Pullman Inc Method for desiccating and reducing ore
US3640701A (en) * 1964-04-30 1972-02-08 Creusot Loire Direct reduction of oxides
US3573894A (en) * 1965-03-18 1971-04-06 Pierre Marie Francois Fourt Process and plant for reducing metallic oxides
US3425824A (en) * 1965-06-23 1969-02-04 Metallgesellschaft Ag Process of reducing metal ores

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3877933A (en) * 1973-09-21 1975-04-15 Int Nickel Co Metallurgical addition product
US5017220A (en) * 1989-02-21 1991-05-21 Nkk Corporation Method for smelting reduction of Ni ore
US5324341A (en) * 1992-05-05 1994-06-28 Molten Metal Technology, Inc. Method for chemically reducing metals in waste compositions
US20110103998A1 (en) * 2007-10-26 2011-05-05 Ivan Ratchev Production of Nickel
US8557019B2 (en) * 2008-02-08 2013-10-15 Vale Inco Limited Process for production of nickel and cobalt using metal hydroxide, metal oxide and/or metal carbonate
US20090249921A1 (en) * 2008-02-08 2009-10-08 Vale Inco Limited Process for production of nickel and cobalt using metal hydroxide, metal oxide and/or metal carbonate
US20110118100A1 (en) * 2008-02-12 2011-05-19 Ivan Ratchev Production of Nickel
US8460429B2 (en) 2008-02-12 2013-06-11 Bhp Billiton Innovation Pty Ltd Production of nickel
WO2009100495A1 (en) * 2008-02-12 2009-08-20 Bhp Billiton Innovation Pty Ltd Production of nickel
CN101952464B (zh) * 2008-02-12 2013-12-11 Bhp比利顿创新公司 镍的生产
FR3008426A1 (fr) * 2013-07-15 2015-01-16 Eramet Procede d'elaboration de nickel metallique a partir d'oxyde de nickel par fusion-reduction
WO2015007658A1 (fr) * 2013-07-15 2015-01-22 Eramet Procédé d'élaboration de nickel métallique à partir d'oxyde de nickel par fusion-réduction
US20220048790A1 (en) * 2018-09-26 2022-02-17 Panasonic Intellectual Property Management Co., Ltd. Method for producing nickel particles, method for producing nickel sulfate, and method for producing positive electrode active material for secondary batteries

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DE2134161A1 (enrdf_load_html_response) 1972-02-03
CA921708A (en) 1973-02-27
ZA714230B (en) 1972-03-29
JPS5227612B1 (enrdf_load_html_response) 1977-07-21
GB1316200A (en) 1973-05-09
DOP1971001829A (es) 1976-05-12
NO128620B (enrdf_load_html_response) 1973-12-17
FR2098258B1 (enrdf_load_html_response) 1974-04-05
FR2098258A1 (enrdf_load_html_response) 1972-03-10
DE2134161B2 (de) 1972-02-03

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