US3656940A - Process for the purification of nickel containing solutions - Google Patents

Process for the purification of nickel containing solutions Download PDF

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Publication number
US3656940A
US3656940A US830883A US3656940DA US3656940A US 3656940 A US3656940 A US 3656940A US 830883 A US830883 A US 830883A US 3656940D A US3656940D A US 3656940DA US 3656940 A US3656940 A US 3656940A
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US
United States
Prior art keywords
nickel
cobalt
solution
chloride
iron
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Expired - Lifetime
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US830883A
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English (en)
Inventor
Louis Gandon
Roger Jean
Philippe Lenoble
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Societe Le Nickel SLN SA
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Individual
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/01—Preparation or separation involving a liquid-liquid extraction, an adsorption or an ion-exchange
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J41/00—Anion exchange; Use of material as anion exchangers; Treatment of material for improving the anion exchange properties
    • B01J41/04—Processes using organic exchangers
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/0009—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C01G51/01—Preparation or separation involving a liquid-liquid extraction, an adsorption or an ion-exchange
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • This invention relates to a hydrometallurgical process for the separation of metals and more particularly to a process for purifying nickel solutions containing in admixture small quantitles of metals such as cobalt, iron, and, optionally, molybdenum, copper, aluminum, manganese, and zinc.
  • the nickeliferous ores generally contain relatively large quantities of iron and cobalt, and for industrial applications it is desirable to carry out treatments with a view to separately obtaining high-purity nickel and, where appropriate, high-purity cobalt.
  • anodes are usually cast from an iron/nickel/cobalt alloy orfrom matte, i.e., sub-sulphides of these metals.
  • the anodic corrosion of these cast ingots in anode compartments containing an aqueous electrolyte based on nickel chloride forms on the one hand an impure anolyte rich in nickel and containing iron, cobalt and optionally other metals, and on the other hand an insoluble anodic sludge consisting mainly of metalloids, sulphur and arsenic or certain metal compounds thereof.
  • the impure anolyte has to be subjected to a chemical treatment in order to completely remove the iron and cobalt present therein and thus provide a purified electrolyte which can be used as a catholyte.
  • the nickel is electrodeposited on metal plates, for example consisting of stainless steel or nickel, in cathode compartments.
  • the catholyte poor in nickel is then transferred to the anode compartments by diffusion through porous fabric partitions which limit the cathode compartment.
  • chlorides of cobalt and nickel could be separated by equivalent means, such as for example by means of certain amines or carboxylic acids.
  • these processes cannot be applied to purification by electrolysis because they involve conditions of acidity that are incompatible with the process of electro-deposition.
  • the nickel-cobaltiferous material has to be dissolved in a solution of ammonium chloride to obtain solutions containing nickel cations and complex cobalt chloride anions.
  • Ammonia is given off during this reaction, with the result that the technique is not suited to the conditions under which electrolytic purification is carried out, i.e., generally in an acid medium and in the presence of completely dissociated salts such as sodium chloride.
  • the quantities of ammonium salts required for the treatment are prohibitive because they lie between concentrations of 4N and ION, usually at sixto eight-times molar.
  • the present invention provide an efficient process which is easy to carry out in that it involves very few manual operations whilst at the same time enabling a certain number of metals, in particular nickel, iron and cobalt, to be almost completely separated from mixtures containing them.
  • the present invention relates to a process for purifying solutions containing nickel in admixture with metals capable of forming anionic complex chlorides, wherein the anionic complex chlorides of these metals are formed by addition to the solution of an alkaline or alkali earth metal chloride, the chloride concentration of the solution being from 2 to 6N and the temperature above 20 C, after which the solution is contacted with an anion exchange resin to adsorb the complex anions of the metals capable of forming anionic complex chlorides and the nickel solution thus treated is recovered.
  • the solution will generally then be treated to remove from it all metals other than those emanating from the supply of the dissociated chloride.
  • the metals capable of forming complex chlorides include in particular cobalt and iron and also molybdenum, manganese, aluminum, and zinc.
  • the process according to the invention is particularly applicable to the treatment of anolytes such as those emanating from the electrolytic refinement of ferro-nickel or mattes. However, it may also be used for separating cobalt, iron and nickel from mixtures emanating from the direct dissolution of materials containing them. Thus, the process may be used with particular advantages for the purification of nickel salts obtained by the action of hydrochloric acid on such substances as industrial waste, spent catalysts and carbonates and hydroxides emanating from the precipitation of spent nickel-plating baths with soda.
  • these anolytes In the case of impure anolytes emanating from the attack of ferro-nickel anodes, these anolytes generally have a pH value of around 4 and contain from 70 to 85 g/liter of nickel, from 0.5 to l g/liter of iron and from 0.10 to 0.20 g/liter of cobalt, and also quantities of sodium chloride of the order of 60 g/liter and more generally between 60 and 180 g/liter.
  • the dissociated hydrochloric acid salts are preferably alkali metal chlorides and more particularly sodium chloride and potassium chloride.
  • the chloride concentration of the solution is preferably 3N to 4N.
  • the temperature employed, in excess of 20 C, is preferably in a range from about 60 to about 80 C, these being the temperatures at which the anionic exchange resin has a maximum effect and does not undergo any deterioration.
  • resins that are known to have strongly basic outline groups, such as quaternary amines.
  • a preferred resin is polystyrene with active groups of the quaternary ammonium type, this resin working in the form of its chloride which is its most stable form.
  • IMAC S 540 One example of such a resin is commercially available under the name IMAC S 540.
  • AMBERLITE IRA 400 which is a polystyrene resin containing groups
  • DOWEX l which is a polystyrene resin containing groups
  • weakly basic resins such as that commercially available under the name lMAC A 20 P, of which the active groups consist of primary, secondary and tertiary amines, may be satisfactorily used in the specific case of anolytes with the concentration indicated previously, because the pH and temperature conditions correspond ideally to the range of activity of these types of base.
  • the process comprises anodically attacking nickeliferous, cobaltiferous and ferruginous substances in a hot concentrated solution of a nickel chloride and sodium chloride and continuously treating this solution be percolation on an anion-exchange resin in the form of its chloride, so as to absorb the iron and the cobalt and give a solution of nickel chloride and sodium chloride which is directly recycled to the cathode compartment for the electrodeposition of the nickel in a pure form.
  • the impure solution issuing from the anode compartment passes at a predetermined rate through an anion-exchange resin column (such as the resin lMAC S 540).
  • the nickel cations pass through the column without being retained whilst the complex cobalt/iron anions are adsorbed by the resin. This results in a complete separation of all the iron and cobalt from the nickel.
  • the invention also relates to a process for recovering metals other than nickel retained in complex anionic form by the ion exchanger, comprising desorbing the aforementioned exchanger with optionally acidulated water or even with an aqueous solution of dissociated salts at such a concentration that the aforementioned complex is destroyed.
  • the cobalt is preferably extracted with a semi-normal solution of dissociated chlorides, the iron, aluminum, zinc and so on preferably being eliminated with a decinormal to normal hydrochloric acid solution.
  • the desorbed metals are directly recovered in the form of chlorides. Elution with the chlorides simultaneously regenerates the resin which is reavailable for continuing the purification cycle.
  • the column has a double jacket enabling a temperature of C: 5 C to be maintained during the experiment. Percolation is carried out at an average speed of 4,500 liters per hour.
  • the resin On completion of the cycle, the resin is washed with 3 liters of saturated sodium chloride solution in order to entrain the nickel retained, and the cobalt is eluted by percolating hot water through the resin.
  • the following table confirms the path along which the various operations progress.
  • EXAMPLE 2 Six liters of an anolyte which is produced by the electrolytic purification of a nondeferrized matte and having the following composition:
  • Example 2 are brought into contact in a manner substantially similar to that described in Example 1 in the same ion-exchange column which was used for treating the anolyte containing only very small quantities of impurities other than cobalt.
  • the first 6 liters of effluent contained less than 50 mg per liter of cobalt and less than mg per liter of nickel.
  • almost all the cobalt, i.e., 11.27 g, is recovered in pure fon'n, the iron being desorbed from the resin on completion of the cycle by washing with water at a high rate, i.e., at a rate of four times the volume of resin per hour.
  • the initial NirNi-l-Co weight ratio is 83.8%. After treatment, it reaches 99.1 percent.
  • the cobalt complex is released during desorption in the form of a solution of cobalt chloride in which the weight ratio of NizCo is lower than 2 percent.
  • aqueous solution at least one chloride selected from the group comprising the alkali and alkaline earth metal chlorides in an amount such that said aqueous solution has a chloride concentration in the range from 2N to 6N;
  • an eluant selected from the group consisting of water, acidulated water and aqueous solutions of alkali and a1- kaline earth metal chlorides at such a concentration that the said metal is removed from said anion exchange resin.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Treatment Of Water By Ion Exchange (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
US830883A 1968-06-21 1969-06-05 Process for the purification of nickel containing solutions Expired - Lifetime US3656940A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR156168A FR1583920A (fr) 1968-06-21 1968-06-21 Procede de purification de solutions de nickel

Publications (1)

Publication Number Publication Date
US3656940A true US3656940A (en) 1972-04-18

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Family Applications (1)

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US830883A Expired - Lifetime US3656940A (en) 1968-06-21 1969-06-05 Process for the purification of nickel containing solutions

Country Status (13)

Country Link
US (1) US3656940A (cs)
JP (1) JPS518095B1 (cs)
BE (1) BE734070A (cs)
BR (1) BR6909995D0 (cs)
CS (1) CS179356B2 (cs)
CU (1) CU33395A (cs)
DE (1) DE1931426A1 (cs)
DO (1) DOP1969001630A (cs)
FI (1) FI50328C (cs)
FR (1) FR1583920A (cs)
GB (1) GB1276134A (cs)
NO (1) NO125938B (cs)
YU (1) YU33889B (cs)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3839168A (en) * 1971-05-24 1974-10-01 Nickel Le Method for producing high-purity nickel from nickel matte
US3992270A (en) * 1974-02-05 1976-11-16 Imetal Method of reclaiming nickel values from a nickeliferous alloy
US4069040A (en) * 1973-11-19 1978-01-17 Rhone-Poulenc Industries Method for recovery of platinum and iridium from catalysts
US5368703A (en) * 1992-05-12 1994-11-29 Anco Environmental Processes, Inc. Method for arsenic removal from wastewater
US20040069652A1 (en) * 2001-08-01 2004-04-15 Yuichiro Shindo Method for producing high purity nickle, high purity nickle, sputtering target comprising high purity nickel, and thin film formed by using said spattering target
WO2006113944A1 (en) * 2005-04-18 2006-10-26 Edmund Kevin Hardwick Separation of nickel from cobalt by using chloridizing solution and cobalt-selective resin
US20070122324A1 (en) * 2005-11-25 2007-05-31 Enthone Inc. Method and apparatus for purification of process solutions
AU2004208659B2 (en) * 2003-09-17 2010-05-20 Sumitomo Metal Mining Co., Ltd. Method for refining aqueous nickel chloride solution
CN106283108A (zh) * 2016-08-31 2017-01-04 中南大学 一种用离子交换树脂从镍电解阳极液中深度除铜的方法
WO2023213919A1 (en) * 2022-05-05 2023-11-09 Umicore Process for the oxidative leaching of a metal

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2138332B1 (cs) * 1971-05-24 1975-07-04 Nickel Le
FR2834980B1 (fr) * 2002-01-23 2005-01-14 Sarp Ind Procede de separation du zinc et d'un second metal ne formant pas de complexe anionique en presence d'ions chlorures
JP6602172B2 (ja) * 2015-11-18 2019-11-06 シチズン時計株式会社 金属装飾物及びその製造方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3085054A (en) * 1960-02-25 1963-04-09 Falconbridge Nickel Mines Ltd Recovery of nickel
US3128156A (en) * 1960-02-08 1964-04-07 Dow Chemical Co Recovery and separation of cobalt and nickel
US3235377A (en) * 1962-11-23 1966-02-15 Union Carbide Corp Use of an anion exchange resin to absorb cobalt from a solution containing cobalt and nickel
US3537845A (en) * 1967-04-24 1970-11-03 Dow Chemical Co Separation and recovery of cobalt and zinc

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3128156A (en) * 1960-02-08 1964-04-07 Dow Chemical Co Recovery and separation of cobalt and nickel
US3085054A (en) * 1960-02-25 1963-04-09 Falconbridge Nickel Mines Ltd Recovery of nickel
US3235377A (en) * 1962-11-23 1966-02-15 Union Carbide Corp Use of an anion exchange resin to absorb cobalt from a solution containing cobalt and nickel
US3537845A (en) * 1967-04-24 1970-11-03 Dow Chemical Co Separation and recovery of cobalt and zinc

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3839168A (en) * 1971-05-24 1974-10-01 Nickel Le Method for producing high-purity nickel from nickel matte
US4069040A (en) * 1973-11-19 1978-01-17 Rhone-Poulenc Industries Method for recovery of platinum and iridium from catalysts
US3992270A (en) * 1974-02-05 1976-11-16 Imetal Method of reclaiming nickel values from a nickeliferous alloy
US5368703A (en) * 1992-05-12 1994-11-29 Anco Environmental Processes, Inc. Method for arsenic removal from wastewater
US7435325B2 (en) * 2001-08-01 2008-10-14 Nippon Mining & Metals Co., Ltd Method for producing high purity nickle, high purity nickle, sputtering target comprising the high purity nickel, and thin film formed by using said spattering target
US20040069652A1 (en) * 2001-08-01 2004-04-15 Yuichiro Shindo Method for producing high purity nickle, high purity nickle, sputtering target comprising high purity nickel, and thin film formed by using said spattering target
US20090004498A1 (en) * 2001-08-01 2009-01-01 Nippon Mining & Metals Co., Ltd. Manufacturing Method of High Purity Nickel, High Purity Nickel, Sputtering Target formed from said High Purity Nickel, and Thin Film formed with said Sputtering Target
AU2004208659B2 (en) * 2003-09-17 2010-05-20 Sumitomo Metal Mining Co., Ltd. Method for refining aqueous nickel chloride solution
WO2006113944A1 (en) * 2005-04-18 2006-10-26 Edmund Kevin Hardwick Separation of nickel from cobalt by using chloridizing solution and cobalt-selective resin
US20070122324A1 (en) * 2005-11-25 2007-05-31 Enthone Inc. Method and apparatus for purification of process solutions
US8202431B2 (en) * 2005-11-25 2012-06-19 Enthone Inc. Method for removing impurities from a metal deposition process solution
EP1803837B1 (de) 2005-11-25 2018-09-12 MacDermid Enthone Inc. Verfahren und Vorrichtung zur Reinigung von Prozesslösungen
CN106283108A (zh) * 2016-08-31 2017-01-04 中南大学 一种用离子交换树脂从镍电解阳极液中深度除铜的方法
CN106283108B (zh) * 2016-08-31 2018-04-03 中南大学 一种用离子交换树脂从镍电解阳极液中深度除铜的方法
WO2023213919A1 (en) * 2022-05-05 2023-11-09 Umicore Process for the oxidative leaching of a metal

Also Published As

Publication number Publication date
YU131969A (en) 1977-12-31
BE734070A (cs) 1969-11-17
FI50328C (fi) 1976-02-10
JPS518095B1 (cs) 1976-03-13
FI50328B (cs) 1975-10-31
FR1583920A (fr) 1969-12-05
CS179356B2 (en) 1977-10-31
NO125938B (cs) 1972-11-27
YU33889B (en) 1978-06-30
GB1276134A (en) 1972-06-01
CU33395A (en) 1981-12-04
BR6909995D0 (pt) 1973-01-11
DE1931426A1 (de) 1970-03-19
DOP1969001630A (es) 1974-07-02

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