US3432410A - Method of producing pure nickel by electrolytic refining - Google Patents

Method of producing pure nickel by electrolytic refining Download PDF

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US3432410A
US3432410A US414091A US3432410DA US3432410A US 3432410 A US3432410 A US 3432410A US 414091 A US414091 A US 414091A US 3432410D A US3432410D A US 3432410DA US 3432410 A US3432410 A US 3432410A
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nickel
catholyte
anolyte
cathodic
cathode
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US414091A
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Charles Cuenot
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Societe Le Nickel SLN SA
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
    • C25C7/06—Operating or servicing
    • 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

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  • This invention relates in general to the manufacture of high-purity (about 99.95 by weight) nickel from ferronickel and more particularly to a method of producing high-purity nickel cathodes by electrolytic refining from ferronickel anodes.
  • Patented Mar. 11, 1969 iron, cobalt, etc., and an anode slime comprising mainly iron, cobalt, etc.
  • a cathode deposit the nickel being electrodeposited on metal plates such as stainless or nickel plates in cathodic compartments from the aforesaid catholyte, the nickelimpoverished catholyte being transferred into the anodic cells by dilfusion through pervious cloths bounding the cathodic compartment.
  • one fraction of the catholyte must be recirculated with a high output at least equal to 0.66 to 0.8 gallon per hour per amp/hr. and the nickel concentration in the electrolyte must be relatively high in order to yield a satisfactory homogeneous deposit.
  • Ferronickel anodes contain mainly nickel and iron. The method is applicable irrespective of the nickel contents of the anodes; however, for the sake of economy it is desirable to use ferronickel anodes having a nickel content higher than 80% by weight.
  • the anode corrosion takes place regularly and uniformly.
  • the weight of the noncorroded anode portion may be as low as about '4 to 5% of the initial weight, without taking into account the anode portion emerging from the bath.
  • This invention provides a method of forming cathode deposits of electrolytic nickel and notably av method of producing electrolytic nickel plates.
  • the method of this invention is applicable under both low and high current density values; however, a high cathode current density (of the order of 2,000 to 3,000 amps/sq. ft.) permits of increasing appreciably the production rate of electrolytic cells and, therefore, of reducing the corresponding investments.
  • This invention proposes the use of an aqueous electrolyte affording a satisfactory anode corrosion and a proper cathode deposit.
  • the present invention provides a method of producing high-purity electrolytic nickel by electrolytic refining from ferronickel anodes, this method comprising the following steps:
  • An anodic corrosion of ferronickel anodes in anodic compartments containing a nickel-chloride aqueous electrolyte to form a high-nickel impure anolyte including
  • the anode slime comprises a light fraction and a heavy fraction.
  • Light slime (about 92% of the slimes) is reddish and has a high iron content.
  • Heavy slime is black (about 8% of the slimes).
  • the slimes showed the following compositions:
  • Anode slimes The surface area of the electrodes used in these examples, whether anodes or cathodes, may range from 2 to 13 sq. ft.
  • the original cathode may be a stainless mother plate the surfaces of which are properly prepared for example by sandblasting so as to be slightly but very regularly rough, the electrodeposition of nickel forming on both faces of this plate a commercial nickel cathode having a thickness ranging from A" to A which is separated from the mother plate after the electrolysis.
  • the original cathode may also consist of a nickel mother sheet having a thickness ranging from about 0.02" to 0.04", obtained by electrodeposition of nickel on a stainless-steel mother plate and separation of the thus deposited nickel sheets when their thickness attains a value of about 0.02" to 0.04"; the internal texture and the surface of these mother sheets are carefully prepared for example by effecting the following sequence of operation:
  • the thus treated sheets are used as mother sheets for producing commercial nickel cathodes of a thickness ranging from about 0.35 to 0.47" and incorporating the mother sheet constituting the intermediate portion of the commercial cathode.
  • This invention is also concerned with commercial nickel cathodes obtained by carrying out the method described hereinabove.
  • electrolytic cells may be used for carrying out the method of this invention.
  • FIGURE 1 is a diagrammatic vertical section showing a specific form of embodiment of an electrolytic cell
  • FIGURE 2 is a similar vertical section but taken at right angles to the former in the cathode compartment portion of the assembly
  • FIGURE 3 is a block diagram showing the various steps of an electrolysis carried out according to the method of this invention.
  • the ferronickel anodes are corroded anodically in electrolytic cells 2 filled with a nickel-chloride electrolyte to produce a high-nickel impure anolyte 3.
  • the impure liquid anolyte produced with a pH approximating 4 contains about 70 to 85 grams per liter of nickel, 30 to 60 grams per liter of calcium, to grams per liter of sodium, about 0.5 to 1 gram per liter of iron, 0.10 to 0.20 gram per liter of cobalt, 0.010 to 0.020 g am per liter of copper.
  • This concentrated solution is at a temperature of the order of 45 to 60 (113 F. to 140 F.).
  • the impure anolyte is treated at 4, outside the electrolytic cell, to remove the greater portion of its iron and cobalt contents, notably in order to produce a pure catholyte 5 from which electrodeposited nickel cathodes 6 are formed which contain at least 99.85% nickel, less than 0.1% cobalt, less than 0.01% iron, less than 0.01% copper.
  • the iron precipitation takes place under a pH value ranging from 1.8 to 3.5 by chlorine peroxidation in the presence of a precipitation agent which should be a basic nickel material such as hydrate or carbonate of nickel.
  • hydrate of nickel is used (a product which can be prepared by electrolysis) an amount of hydrate of nickel which corresponds to the stoichiometric quantity of iron dissolved in the electrolyte should be introduced. Copper and arsenic are eliminated with iron. The precipitation of cobalt takes place under a pH value of 3.5 to 4.5 in the presence for example of milk of lime and chlorine; calcium and sodium remain in the solution.
  • the catholyte that is, the electrolyte of purified aqueous chloride, has a pH value ranging from 4 to 5 set preferably at 4.5, and contains not more than 0.005 gram/liter of iron, 0.010 gram/liter of cobalt and 0.003 gram/liter of copper.
  • the nickel and chlorine radical concentrations are practically the same as in the impure anolyte.
  • the catholyte is electrolyzed in the cathodic compartment 7 at a temperature ranging from 50 C. to 60 C. (122 F. to 140 F.) by causing electric current to flow therethrough.
  • the current density may be variable; however,
  • high-density current that is, above 1,500 amps/sq. ft. and notably from 2,000 to 4,500 amps/sq. ft. for electrodepositing nickel implies the stirring of the catholyte in the cathodic compartment to facilitate the diffusion through the cathodic film of the nickel ions to be discharged.
  • This stirring is obtained by resorting to a forced circulation of the catholyte along the path 8 in the cathodic compartment 7 by means of a circulation pump (not shown).
  • the recirculated catholyte is perferably reheated along its path outside the cathodic cell to a temperature ranging from 50 C. to 60 C. (122 F. to 140 F.).
  • the pure catholyte 5 from the anolyte purification is fed at 9 to the recirculated catholyte 8 and the mixture 12 of the two catholyte streams is reintroduced into the cathodic compartment 7.
  • the catholyte circulation output should be at least from 0.66 to 0.8 gallon per hr. and per amp/hr. Of course, the catholyte circulation output should be adjusted as a function of the actual density of the current utilized.
  • EXAMPLE The electrolysis is carried out in cells 11 (FIGURE 3) comprising sixty-one electrodes, that is, thirty-one anodes 1 and thirty cathodes 6; the rectangular anode dimensions are 30" x 40" with an initial thickness of 2.16"; the rectangular cathode consists of 32" x 42" x 0.2 stainless steel plates.
  • the anodes constitute the raw material to be treated.
  • Each cathode 6 is disposed in a cathodic cell 7 consisting of a cathodic box of polyester reinforced with glass fabric, the two lateral faces of this box which register with the anode being hollowed and comprising cathodic cloths 10 permitting the gravity of a 4.8 cu. in. per hour output per amp/hr. of catholyte towards the anolyte.
  • the inner dimensions of the electrolytic cells are 51" x 227" x 55". These cells are lined internally with a corrosion-resistant material also adapted to withstand mechanical shocks and heat surges, such as polyester resin reinforced with glass fabric.
  • the electrolysis is carried out under a current density of 3,000 amps. per sq. ft., thus giving 450 amperes admitted for each electrode or 13,600 amperes per electrolytic cell.
  • the catholyte 12 is distributed along the cathodes 6 by diffusers in the form of perforated plates 13 (see FIGURE 2) disposed in the cathodic boxes and adapted regularly to sweep the cathodes in the direction of the arrows i with an hourly output of 0.66 gallon/hr. per amp/hr.
  • One fraction of the catholyte (0.0211 gallon/hr. per amp/hr.) is diffused through the cathodic cloths in the direction of the arrows f to the anolyte 3, the remaining catholyte fraction 8 being recirculated to the cathodic boxes 7 after an intermediate reheating in 14 at the rate of 0.66 gallon/ hr. per amp/hr.
  • the catholyte is heated at a temperature of about 50 C. to 60 C. (122 F. to 140 F.) for example in a steam-heated graphite-type heat transfer device.
  • the 50 to 60 C. (122 F. to 140 F.) temperature of the catholyte is one of the factors ensuring a proper deposit of nickel on the cathode.
  • the anolyte 3 is taken from the electroiytic cells and delivered to the purifying system at the above-mentioned rate of 4.8 cu. in./hr. per amp/hr.
  • a cascade set of purifying cells operating continuously permits of precipitating iron at 15 (by means of chlorine 16 and hydrate of nickel 17) and cobalt at 18 (by means of chlorine 16 and hydrate of lime 19).
  • the reactions with due regard for the stirrings and recirculations, re quire a total residence time of about half an hour.
  • By Way of indication therefore, given an anolyte output of 15,850 gallons per hour, the reactions take place in six precipitation cells of 158 gallons useful capacity each.
  • the filtration is effected at 20 for example by using filter presses without washing the cakes.
  • filter presses By way of example, given the above-mentioned output and an iron concentration of 1.8 lb. per cu. in. (or 0.5 gram/liter) in the anolyte 3 issuing from the electrolytic cells, the filtration requires three filter presses having a useful surface of 750 sq. ft. each, one filter press commencing the filling, the second being unclogged and the third completing the filling.
  • the purified anolyte 5 is fed at 9 to the catholyte circuit and the resulting mixture 12 is reintroduced with an hourly output of 0.682 gallon per amp/hr. into the cathodic cells 7 from which it flows by gravity from one to the other end of the cathodic boxes.
  • the above-mentioned fraction of 4.8 cu. in./hr. per amp/hr. flows through the pervious cloths 7 to the anolyte and the remaining fraction 8 of the catholyte is fed to a circuit from which it is pumped for reheating and eventually recycled.
  • the recirculation circuit comprises a 3,500 cu. ft. (or 26,400 gallon) storage vat, three pumps having a capacity of 105,000 gaL/hr. each, and a reheated catholyte stocking vat having a capacity of 3,500 cu. ft. (or 26,400 gallons).
  • the anode slirnes accumulate in the bottom of cell 11. They are removed periodically during the idle time period of the cell and collected at 21. The anode wastes at the end of the electrolytic process are collected at 22.
  • the electrolytic nickel is deposited on 0.2" stainless steel cathodic plates. After height to ten days deposit under a current density of 3,000 amps/sq. ft. the cathodic plates coated on each face with a layer of electrolytic nickel having a thickness ranging from A to are extracted from the bath at 23, scoured and washed at 24; the nickel plates are separated from their supporting plates at 25, reannealed in neutral atmosphere to degasify same at 26, and cut to standard dimensions at 27 to yield the final product 28.
  • a method of producing high-purity nickel by electrolytic refining which comprises the steps of corroding ferronickel anodes in an aqueous nickel-chloride electrolyte contained in the anodic compartment of a divided electrolytic cell for producing a high-nickel impure anolyte containing impurities, and applying a chemical treatment to said impure anolyte outside said electrolytic cell with a view to form a purified electrolyte fed as a catholyte into the cathodic compartment of said electrolytic cell, said cathodic compartment comprising walls of pervious cloths, electrodepositing the nickel from said catholyte on the cathode, and causing said nickel-impoverished catholyte to pass into said anodic compartment by diffusion through said pervious cloths, the improvements consisting in that said ferronickel anodes have a nickel content greater than by weight, that said nickel-chloride anolyte contains per liter about 70 to grams of nickel ions, about 30
  • catholyte has the same nickel, calcium, sodium and chloride ion contents as said anolyte, a pH value ranging from 4 to 5 and a temperature ranging from 50 C. to 60 C. (122 F. to 140 F.).
  • said electrolytic cell comprises a plurality of anodes and a plurality of cathodes disposed in as many cathodic compartments.
  • said original cathode is a nickel mother sheet having a thickness of about 0.02 to 0.04", obtained by electrodepositing nickel on a stainless steel mother plate and separating the deposited nickel sheets when their thickness attains from 0.02" to 0.04", said sheets being used as mother sheets for producing commercial nickel cathodes of a thickness of about 0.35" to 0.47" incorporating the mother sheet constituting the intermediate portion of said commercial cathode.
  • a method of producing high-purity nickel by electrolytic refining which comprises the steps of corroding ferronickel anodes in an aqueous nickel-chloride electrolyte contained in the anodic compartment of :a divided electrolytic cell for producing a high-nickel impure anolyte containing impurities, and applying a chemical treatment to said impure anolyte outside said electrolytic cell with a view to form a purified electrolyte fed as a catholyte into the cathodic compartment of said electrolytic cell, said cathodic compartment comprising walls of pervious cloths, electrodepositing the nickel from said catholyte on the cathode, and causing said nickel-impoverished catholyte to pass into said anodic compartment by diffusion through said pervious cloths, the improvements consisting in that said ferronickel anodes have a nickel content greater than 80% by weight, that said nickel-chloride anolyte contains per liter about 70 to 85 grams of nickel
  • catholyte has the same nickel, calcium, sodium and chloride ion contents as said anolyte, a pH value ranging from 4 to 5 and a temperature ranging from 50 C. to 60 C. (122 F. to 140 F.), that said catholyte is recycled in said cathodic compartment whereby it will sweep the cathode faces, is reheated during its recycling to a temperature ranging from 50 to 60 (122 to 140 F.) and electrolyzed in said cathodic compartment with a current density ranging from about 1,500 to about 4,500 amps/ sq. ft.
  • said electrolytic cell comprises a plurality of anodes and a plurality of cathodes disposed in as many cathodic compartments.
  • said electrolytic cell comprises a plurality of anodes and a plurality of cathodes disposed in as many cathodic compartments.
  • said original cathode is a nickel mother sheet having a thickness of about 0.02 to 0.04, obtained by electrodepositing nickel on a stainless steel mother plate and separating the deposited nickel on a stainless steel mother plate and separating the deposited nickel sheets when their thickness attains from 0.02" to 0.04", said sheets being used as mother sheets for producing commercial nickel cathodes of a thickness of about 0.35" to 0.47" incorporating the mother sheet constituting the intermediate portion of said commercial cathode.
  • An aqueous catholyte for producing high-purity electrolytic nickel containing about 70 to 85 grams of nickel ions, about 30 to 60 grams of calcium ions and about 15 to 20 grams of sodium ions per liter, the anions of said catholyte consisting essentially of chloride ions, said catholyte having a pH value ranging from 4 to 5.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrolytic Production Of Metals (AREA)
US414091A 1963-11-27 1964-11-27 Method of producing pure nickel by electrolytic refining Expired - Lifetime US3432410A (en)

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Application Number Priority Date Filing Date Title
FR955190A FR1384780A (fr) 1963-11-27 1963-11-27 Procédé de raffinage électrolytique d'un alliage de nickel, en vue de l'obtention de nickel pur électrolytique

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US (1) US3432410A (de)
AT (1) AT255779B (de)
BE (1) BE654820A (de)
CH (1) CH440725A (de)
DK (1) DK124413B (de)
DO (1) DOP1964001139A (de)
ES (1) ES306422A1 (de)
FI (1) FI44300B (de)
FR (1) FR1384780A (de)
GB (1) GB1045630A (de)
LU (1) LU47209A1 (de)
NL (1) NL6413729A (de)
SE (1) SE305326B (de)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4288305A (en) * 1979-10-10 1981-09-08 Inco Limited Process for electrowinning nickel or cobalt
US4786386A (en) * 1984-07-19 1988-11-22 Universite des Sciences et Techniques du Languedoc (Montpelier I) Process and apparatus for the treatment of water and effluents by ultra-filtration and electrolysis
US5458745A (en) * 1995-01-23 1995-10-17 Covofinish Co., Inc. Method for removal of technetium from radio-contaminated metal
US20040124097A1 (en) * 2000-09-01 2004-07-01 Sarten B. Steve Decontamination of radioactively contaminated scrap metals from discs
EP1413651A4 (de) * 2001-08-01 2006-10-25 Nippon Mining Co Verfahren zur herstellung von hochreinem nickel, hochreines nickel, das hochreine nickel enthaltendes sputtertarget und unter verwendung des sputtertargets gebildeter dünner film
RU2503748C2 (ru) * 2011-10-10 2014-01-10 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Тамбовский государственный технический университет" (ФГБОУ ВПО ТГТУ) Способ получения ультрамикродисперсного порошка оксида никеля на переменном токе
RU2550070C1 (ru) * 2014-02-04 2015-05-10 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Тамбовский государственный технический университет" Способ получения ультрамикродисперсного порошка оксида никеля

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114735765B (zh) * 2022-03-10 2023-09-01 成都盛威兴科新材料研究院合伙企业(有限合伙) 一种电池级硫酸镍的生产工艺

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1251511A (en) * 1917-08-14 1918-01-01 George A Guess Process of electrolytically separating nickel from copper.
US1887037A (en) * 1930-08-15 1932-11-08 Int Nickel Co Process of refining nickel bearing materials
US2066347A (en) * 1932-09-03 1937-01-05 Falconbridge Nickel Mines Ltd Production of nickel by electrolytic deposition from nickel salt solutions
US2394874A (en) * 1942-11-05 1946-02-12 Int Nickel Co Electrorefining of nickel
US2478189A (en) * 1944-03-08 1949-08-09 Falconbridge Nickel Mines Ltd Production of malleable and annealable nickel
US2597296A (en) * 1948-10-01 1952-05-20 Int Nickel Co Forming starting sheets for electrolytic refining of nickel
US2839461A (en) * 1953-10-29 1958-06-17 Internat Nickel Co Inc Electrolytic recovery of nickel
US3114687A (en) * 1961-03-10 1963-12-17 Int Nickel Co Electrorefining nickel

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1251511A (en) * 1917-08-14 1918-01-01 George A Guess Process of electrolytically separating nickel from copper.
US1887037A (en) * 1930-08-15 1932-11-08 Int Nickel Co Process of refining nickel bearing materials
US2066347A (en) * 1932-09-03 1937-01-05 Falconbridge Nickel Mines Ltd Production of nickel by electrolytic deposition from nickel salt solutions
US2394874A (en) * 1942-11-05 1946-02-12 Int Nickel Co Electrorefining of nickel
US2478189A (en) * 1944-03-08 1949-08-09 Falconbridge Nickel Mines Ltd Production of malleable and annealable nickel
US2597296A (en) * 1948-10-01 1952-05-20 Int Nickel Co Forming starting sheets for electrolytic refining of nickel
US2839461A (en) * 1953-10-29 1958-06-17 Internat Nickel Co Inc Electrolytic recovery of nickel
US3114687A (en) * 1961-03-10 1963-12-17 Int Nickel Co Electrorefining nickel

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4288305A (en) * 1979-10-10 1981-09-08 Inco Limited Process for electrowinning nickel or cobalt
US4786386A (en) * 1984-07-19 1988-11-22 Universite des Sciences et Techniques du Languedoc (Montpelier I) Process and apparatus for the treatment of water and effluents by ultra-filtration and electrolysis
US5458745A (en) * 1995-01-23 1995-10-17 Covofinish Co., Inc. Method for removal of technetium from radio-contaminated metal
US20040124097A1 (en) * 2000-09-01 2004-07-01 Sarten B. Steve Decontamination of radioactively contaminated scrap metals from discs
EP1413651A4 (de) * 2001-08-01 2006-10-25 Nippon Mining Co Verfahren zur herstellung von hochreinem nickel, hochreines nickel, das hochreine nickel enthaltendes sputtertarget und unter verwendung des sputtertargets gebildeter dünner film
EP2450474A1 (de) * 2001-08-01 2012-05-09 JX Nippon Mining & Metals Corporation Hochreines Nickel, Sputtertarget mit dem hochreinen Nickel und mit diesem Sputtertarget hergestellter Dünnfilm
RU2503748C2 (ru) * 2011-10-10 2014-01-10 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Тамбовский государственный технический университет" (ФГБОУ ВПО ТГТУ) Способ получения ультрамикродисперсного порошка оксида никеля на переменном токе
RU2550070C1 (ru) * 2014-02-04 2015-05-10 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Тамбовский государственный технический университет" Способ получения ультрамикродисперсного порошка оксида никеля

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Publication number Publication date
FI44300B (de) 1971-06-30
AT255779B (de) 1967-07-25
FR1384780A (fr) 1965-01-08
LU47209A1 (de) 1964-12-28
DOP1964001139A (es) 1970-02-04
NL6413729A (de) 1965-05-28
DK124413B (da) 1972-10-16
BE654820A (de) 1965-02-15
CH440725A (fr) 1967-07-31
SE305326B (de) 1968-10-21
GB1045630A (en) 1966-10-12
ES306422A1 (es) 1965-04-01

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