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US3656937A - Process for treatment of mattes and sulphurated nickel concentrates - Google Patents

Process for treatment of mattes and sulphurated nickel concentrates Download PDF

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Publication number
US3656937A
US3656937A US3656937DA US3656937A US 3656937 A US3656937 A US 3656937A US 3656937D A US3656937D A US 3656937DA US 3656937 A US3656937 A US 3656937A
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nickel
solution
cobalt
percent
treatment
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Louis Gandon
Roger Jean
Philippe Lenoble
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Societe Le Nickel SLN SA
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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
    • C22B23/0407—Leaching processes
    • C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
    • 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
    • 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

  • ABSTRACT Nickel containing concentrates particularly nickel matte, containing by weight 55 to 75 percent nickel, 10 to 40 percent sulphur and a minor proportion of secondary metals in powder or pulp form are subjected to an oxidizing lixiviation with nitric acid preferably in the presence of oxygen, nitrous vapors formed being regenerated to nitric acid and recycled.
  • the solution from the oxidizing lixiviation is sulphated to substantially replace nitrate by sulphate; secondary metals, in particular iron, copper and cobalt are removed and pure hydrated nickel sulphate is crystallized from the solution.
  • nickel hydroxide and carbonate are precipitated from the mother liquor from the crystallization of nickel sulphate and are used in the removal of iron and cobalt.
  • Sulphurated nickel concentrates to which the treatment according to the invention is applicable include those which generally contain from 55 to 75 percent of nickel and from to 40 percent of sulphur, these percentages being given by weight, like all those which will follow in the present specificatron.
  • Examples of mattes capable of undergoing the treatment according to the invention include the mattes produced by the pyrometallurgical process worked at the DONIAMBO factory of LE NICKEL, NOUMEA (New Caledonia), emanating from the sulfurizing fusion in a low-shaft furnace of a nickel oxide ore called garnierite.
  • the crude matter thus obtained is refined in converters of the BESSEMER type wherein the iron is burnt out by an air blast and scorified by the silica introduced during blasting.
  • the mattes in question generally contain from 22 to 28 percent of sulphur, from 71 to 73 percent of nickel, from 1.5 to 5 percent of iron and from 2 to 5 percent of cobalt, in addition to small quantities of other elements including copper, manganese, aluminum, magnesium and silica.
  • hydrometallurgically sulphurized concentrates lending themselves to the treatment according to the invention include those obtained by precipitation with hydrogen sulfide from sulphuric solutions which have been used for the lixiviation of laterites, for example, the sulphurized concentrates manufactured in the Cuban MOA-BAY works.
  • a material of this kind usually has the following composition on a dry weight basis:
  • nickel 52 to 68% cobalt 5 to 6% Copper 0.5 to 1% iron 1 to 1.5% zinc l to 1.5% sulphur 30 to 38%
  • the other impurities consist of manganese, magnesia, alkaline-earth metals, silica, in a total quantity not exceeding 1 percent.
  • the initial products capable of being treated in accordance with the invention are not necessarily intermediate products obtained by an initial concentration of ores.
  • they can be mixtures emanating by precipitation with hydrogen sulfide from impure nickel solutions as are obtained in processes for regenerating nickel-plating baths or hydrogenation catalysts, or even materials emanating from the pyrometallurgical treatment of slags with sulphur with a view to concentrating the metals present in them.
  • the ammonical lixiviation method also has the disadvantage of converting the sulphur present into complexes which are all the more difficult to separate if they consist of thionates or polythionates. A second stage of oxidation under pressure or of hydrolysis by prolonged boiling is necessary for the reconversion of these complexes.
  • the metals are extracted in the form of amines and have to be collected in ammonia recovery and distillation systems which use up a considerable amount of energy.
  • the sulphuric lixiviation process does not lead to high yields and the lixiviation stages have to be increased in number if it is desired to obtain economically acceptable yields.
  • the present invention provides an improved process for the hydrometallurgical treatment of mattes and concentrates of the aforementioned type which obviates the disadvantages affecting conventional processes, is easier and less expensive to carry into operation and gives a higher yield.
  • the process according to the invention comprises the steps of:
  • the nickel containing concentrate is subjected to an initial physical treatment to convert it to the finely comminuted form suitable for the oxidizing lixiviation.
  • the most important aspect of the invention is the oxidizing lixiviation with nitric acid in which the nitric acid performs the simple function of an oxygen-transfer agent. This stage is preferably carried out in the presence of a free-oxygen containing gas.
  • the main advantage of this method is embodied in the fact that the oxidation reactions involving the nitric acid are exothermic with the result that the process only requires a minimum supply of energy from outside so that it is particularly economic to operate.
  • the nitric lixiviation is preferably carried out at atmospheric pressure with stirring in air at a temperature below the boiling temperature of nitric acid. All these features contribute to the economy of the process according to the invention from a practical point of view.
  • the cobalt may be precipitated in the form of cobalt (Ill) hydroxide by treatment with an alkali metal or alkaline-earth metal hypochlorites or with chlorine in the presence of nickel (II) hydroxide or nickel carbonate.
  • the secondary metals are preferably separated by operations which do not totally reduce the nickel content of the sulphated brine, namely separation of the iron by the action of nickel (II) carbonate obtained from the mother liquors, separation of the copper by cementation through the addition of nickel powder, and separation of the cobalt by the addition of nickel (III) hydroxide obtained by treating the residual mother liquors.
  • the process according to the invention may be referred to as a loop process in which the nickel which is not recovered in the form of pure sulphate is continuously recycled, which is a factor of economic significance.
  • the starting material is initially crushed to convert it into a relatively fine powder. Crushing should not be over done because on the one hand the oxidizing lixiviation with nitric acid is extremely effective and on the other hand introduction of an excessively fine material into the nitric acid gives rise to the formation of a foam or froth which interferes with the normal operation of any installation. It has been found that the best results are obtained with a powder percent of whose grains are between and 200 microns in size.
  • the preparatory phase merely comprises dispersion in water to convert them into a homogeneous pulp which is fluent enough to be continuously introduced into the reaction medium.
  • the accompanying drawing shows a flow-sheet illustrating the process according to the invention in its preferred embodiment in which the nickel from the residual mother liquors is recycled in the form of nickel carbonate and nickel (III) hydroxide.
  • the process comprises the following stages:
  • the compounds to be treated are introduced into a nitric acid solution whose concentration may vary within certain limits, although the best results are obtained with solutions whose concentration is around 50 percent.
  • the reactor is kept at a temperature above 60 C., and below the boiling point of nitric acid, preferably 80 C. A vigorous current of air bubbles through the reaction medium being necessary to accelerate elimination of the nitrous gases.
  • the nitrous gases are introduced into an absorption and oxidation tower which reconverts them into a nitric acid solution which is returned to the circuit. This installation is similar to that used in nitric acid manufacturing plants.
  • the brine resulting from this treatment is subjected to a hydration treatment and, optionally to a, sulphuration treatment.
  • This treatment comprises adding the sulphuric acid required to neutralize the basic sulphates if an initial material unsaturated with sulphur is used, for example the nickel mattes from New Caledonia.
  • the effect of the sulphuric acid is instantaneous when the temperature is around the boiling point.
  • This sulphation treatment also has a secondary function, namely to displace the nitrates because they are not very stable at the temperature at which this treatment is carried out. 1
  • Ni S 26.7 percent of sulphur
  • the filtrate is then delivered into a tank where its pI-I-value is adjusted with a view to precipitating the ferric iron. This operation is best carried out by adding nickel carbonate and the iron which was in the ferric state precipitates completely at about pH 4.
  • the reaction can be formulated as follows:
  • the ferric compound thus formed is then separated by filtration.
  • the resulting solution is then treated with nickel (Ill) hydroxide to precipitate the cobalt (III) hydroxide in accordance with the following reaction:
  • filtration of the cobalt (III) hydroxide leaves a saline solution whose cation is solely nickel whilst the anions consist of a mixture of nitrate and sulphate in which it is substantially the sulphate component which predominates.
  • the final purification stage comprises a selective crystallization following evaporation of the brine. In effect, the nickel sulphate remains much more insoluble than the corresponding nitrate and almost all the nickel is readily separated in the form of a pure hydrated sulphate.
  • Ni(NO Na CO 2NaNO NiCO t The insoluble nickel carbonate is filtered and washed until the sodium ions have been removed. 2. 2Ni(NO NaOCl-l-4NaOl-I H O 2Ni(OH) NaCl 4NaNO3
  • the nickel (III) hydroxide is filtered and washed in boiling water until the chlorine and sodium ions have disappeared. It is then used to precipitate the cobalt.
  • the cycle is completely in the form of a loop.
  • the nickel sulphate obtained in a perfectly pure form can be converted into pure nickel by conventional processes.
  • EXAMPLE 1 The apparatus used consists of a three-liter-capacity glass reactor equipped with a stirrer and a thermometer and also surmounted by a condenser which opens into a column packed with Raschig rings comprising several stages separated by nozzles for the introduction of air.
  • the reactor is also provided with means for introducing the reactants.
  • the reactor itself is placed in a thermostatically controlled cabinet by means of which the reacting mixture can be heated and cooled.
  • the packed column is continuously washed with a recycled solution, the downward circulation of the liquid being ensured by means of a pump.
  • 919.5 g of 10.95N nitric acid of specific gravity 1.30 are introduced into the reactor. After the acid has been introduced, 20 liters of air per hour are bubbled through it.
  • the temperature is raised to C. and 300 g of nickel matte are introduced over a period of 1 hour and 40 minutes, the temperature being kept at C. throughout the entire operation.
  • the matte treated has the following weight analysis:
  • a portion of the preceding solution 1815 ml) is neutralized to pH 5.9 by the addition of 230 g of nickel carbonate weighed dry but dispersed in 694 g of water. Accordingly the iron is precipitated out as Fe(OI-I) and removed by filtration. This operation is carried out at a temperature of 50 to 60 C. with vigorous stirring. It is completed by the addition of 99.6 mg of ultra-fine nickel powder (98.7 percent pure) in order to precipitate the copper. In addition the oxidation-reduction potential is adjusted by the addition of 8.25 ml of N/50 1(Mn0. so as to eliminate every risk of leaving iron or manganese in solution.
  • the dispersion obtained is filtered in a Buchner funnel at room temperature. There is obtained on the one hand a clear green solution of nickel and cobalt in the form of sulfates weighing 2,500 g with a specific gravity of 1.210 and on the other hand a precipitate weighing 791 g. The precipitate is washed with 1,576 g of boiling water and is then filtered which leads to two fractions:
  • the concentrated solution emanating from the first filtration issubjected for a period of 45 minutes at 95 C. to vigorous stirring in the presence of 240 g of nickel (Ill) hydrate pulp containing 6.57 percent of nickel.
  • the pI-I-value is kept at about 4 by the addition of 300 ml of normal sulphuric acid.
  • the final precipitate weighs 568 g and contains 3.45 percent of nickel.
  • Oxidation is carried out in 3 /2 hours with 49.42 liters of exactly llN commercial nitric acid. Air is bubbled through the reactor at a rate of 6 cubic meters per hour whilst its contents are stirred with a 3-blade propellor agitator turning at 600 rpm. The temperature at the beginning of introduction of the matte was 54 C. It rises quickly, i.e., in less than 15 minutes, to around 75 C. and is kept at this value throughout the introduction period. After all the sulphurated compound has been introduced, the contents of the reactor are boiled for 30 minutes, followed by the addition of 30 liters of boiling water to dilute the reaction product. The residue weighing 1,290 g is filtered. It has the following weight analysis:
  • mother liquors can be converted by precipitation with sodium carbonate, caustic soda and hypochlorite into carbonate and nickelous and nickelic hydroxide available for an operation of the same type, these reactants being used to eliminate the iron and the cobalt.
  • the temperature recording curves indicate that the temperature varies between 80 and 90 C.
  • the gases are delivered to the bottom of a three stage tower filled with Raschig rings in which the washing liquid circulates downwards, the admission of air required for reoxidizing the nitrous vapours being ensured by inlets arranged at intervals along the tower which is placed under a slightly reduced pressure.
  • Ten to eleven liters per hour of a 4446 percent nitric acid solution are taken from this nitric acid regeneration system and returned to the reactor after the addition of enough fresh concentrated acid to restore the original concentration.
  • the brine which results from the oxidation regularly overflows into the second reactor in which concentrated sulphuric acid (66 B) is introduced at a rate of 1.5 liters per hour by means of a metering pump.
  • the temperature is regulated to 105 C.
  • the reddish fumes escaping from this reactor are delivered to a main collector leading to the nitric acid regeneration tower.
  • the highly concentrated solution thus obtained is hydrated by the introduction of 10 liters per hour of cold water and brought to the boil in a third reactor before being separated in a continuous centrifuge.
  • the yield from the treatment is thus above 98 percent while the recovery of nitric acid varies between 70 and percent.
  • the iron is removed as follows: the solution is adjusted to pH 5.5 by the addition of a basic nickel carbonate pulp and is then filtered in a press. The amount of iron left in the solution is less than 5 ml per litre.
  • the filter cake which is rich in nickel is used for the initial removal of iron from the solution to be worked up this treatment being carried out at pH 4 and at a temperature of 60 C.
  • the iron-free solution is subjected in two reactors whose temperature is regulated to 100 C. to intensive stirring by means of turbine impeller rotating at 2,200 r.p.m. in the presence of trivalent nickel hydroxide.
  • the first reactor receives the cake emanating from the centrifuging of the reaction product issuing from the second reactor, while a large excess of the oxidizing reactant is introduced into the second reactor.
  • the following distribution is observed, calculated on an average of 1 hours operation:
  • the solution is concentrated and crystallized in a continuous-cycle crystallizer/evaporator.
  • the crystal paste is centrifuged and the crystallizate is clarified by spraying it with water.
  • the invention is not limited to the examples described above and in particular although the presence of free oxygen during the oxidizing lixiviation phase is preferred it is not indispensable and the presence of nitric acid alone is entirely sufi'rcient to convert the sulphides into sulphates.
  • a process for hydrometallurgically treating a nickel concentrate containing from 55 to 75 weight percent of nickel, from 10 to 40 weight percent of sulphur and minor proportions of secondary metals which process comprises the steps of:

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  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
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  • Materials Engineering (AREA)
  • Metallurgy (AREA)
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  • General Life Sciences & Earth Sciences (AREA)
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US3656937D 1968-10-21 1969-10-03 Process for treatment of mattes and sulphurated nickel concentrates Expired - Lifetime US3656937A (en)

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US (1) US3656937A (fi)
JP (1) JPS5013214B1 (fi)
BE (1) BE740061A (fi)
CS (1) CS184306B2 (fi)
DE (1) DE1952751B2 (fi)
FI (1) FI50639C (fi)
FR (1) FR1597569A (fi)
GB (1) GB1287920A (fi)
NO (1) NO126744B (fi)
YU (1) YU33670B (fi)

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3965239A (en) * 1973-11-16 1976-06-22 International Ore Technology, Inc. Recovery of nitric acid soluble transition metals from sulfur and iron containing ores of the same
US3966462A (en) * 1975-04-18 1976-06-29 International Ore Technology, Inc. Recovery of nitric acid soluble transition metals from sulfur and iron containing ores of the same
US3992270A (en) * 1974-02-05 1976-11-16 Imetal Method of reclaiming nickel values from a nickeliferous alloy
US4038361A (en) * 1975-04-18 1977-07-26 International Ore Technology, Inc. Recovery of nitric acid soluble transition metals from sulfur and iron containing ores of the same
EP1945571A2 (en) * 2005-11-08 2008-07-23 Ovonic Battery Company, Inc. Method of producing a nickel salt solution
US20150078972A1 (en) * 2012-03-29 2015-03-19 Sumitomo Metal Mining Co., Ltd. Method for producing high-purity nickel sulfate
EP2949626A4 (en) * 2013-01-25 2016-12-21 Sumitomo Metal Mining Co METHOD FOR PRODUCING HIGH-PURITY NICKEL SULPHATE AND METHOD FOR REMOVING POLLUTION ELEMENTS FROM A NICKEL-BASED SOLUTION
CN108844949A (zh) * 2018-08-28 2018-11-20 长春黄金研究院有限公司 一种准确高效的矿石中铂钯含量的测定方法
US20200109462A1 (en) * 2017-06-14 2020-04-09 Nmr 360 Inc Method for the production of cobalt and associated oxides from various feed materials
CN114015872A (zh) * 2022-01-06 2022-02-08 矿冶科技集团有限公司 复杂硫化镍矿低温活化加压浸出的方法
EP3945068B1 (en) 2020-07-10 2024-01-17 Northvolt AB Process and method for producing crystallized metal sulfates

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1150787A (en) * 1909-07-17 1915-08-17 Rankin Process Company Method of treating metalliferous materials and recovering solvents used.
US1212334A (en) * 1915-08-24 1917-01-16 Frederic A Eustis Treatment of nickel ores.
US1756092A (en) * 1927-12-27 1930-04-29 Lathe Frank Eugene Method of refining nickel-copper matte
US2367239A (en) * 1942-10-16 1945-01-16 Int Nickel Co Purification of cobalt precipitates containing iron and other impurities
US2377832A (en) * 1941-11-28 1945-06-05 Int Nickel Co Precipitation of cobaltic hydroxide
US2959467A (en) * 1956-03-22 1960-11-08 Yusuf Mehmed Process for treating arseniuretted or sulfarsenidic cobalt, nickel or cobalt and nickel ores

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1150787A (en) * 1909-07-17 1915-08-17 Rankin Process Company Method of treating metalliferous materials and recovering solvents used.
US1212334A (en) * 1915-08-24 1917-01-16 Frederic A Eustis Treatment of nickel ores.
US1756092A (en) * 1927-12-27 1930-04-29 Lathe Frank Eugene Method of refining nickel-copper matte
US2377832A (en) * 1941-11-28 1945-06-05 Int Nickel Co Precipitation of cobaltic hydroxide
US2367239A (en) * 1942-10-16 1945-01-16 Int Nickel Co Purification of cobalt precipitates containing iron and other impurities
US2959467A (en) * 1956-03-22 1960-11-08 Yusuf Mehmed Process for treating arseniuretted or sulfarsenidic cobalt, nickel or cobalt and nickel ores

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3965239A (en) * 1973-11-16 1976-06-22 International Ore Technology, Inc. Recovery of nitric acid soluble transition metals from sulfur and iron containing ores of the same
US3992270A (en) * 1974-02-05 1976-11-16 Imetal Method of reclaiming nickel values from a nickeliferous alloy
US3966462A (en) * 1975-04-18 1976-06-29 International Ore Technology, Inc. Recovery of nitric acid soluble transition metals from sulfur and iron containing ores of the same
US4038361A (en) * 1975-04-18 1977-07-26 International Ore Technology, Inc. Recovery of nitric acid soluble transition metals from sulfur and iron containing ores of the same
EP1945571A2 (en) * 2005-11-08 2008-07-23 Ovonic Battery Company, Inc. Method of producing a nickel salt solution
JP2009519192A (ja) * 2005-11-08 2009-05-14 オヴォニック バッテリー カンパニー インコーポレイテッド ニッケル塩溶液の製造方法
EP1945571A4 (en) * 2005-11-08 2009-12-30 Ovonic Battery Co PROCESS FOR PRODUCING A NICKEL SALINE SOLUTION
EP2832700A4 (en) * 2012-03-29 2015-12-16 Sumitomo Metal Mining Co METHOD FOR PRODUCING HIGH-PURITY NICKEL SULPHATE
US20150078972A1 (en) * 2012-03-29 2015-03-19 Sumitomo Metal Mining Co., Ltd. Method for producing high-purity nickel sulfate
US9702023B2 (en) * 2012-03-29 2017-07-11 Sumitomo Metal Mining Co., Ltd. Method for producing high-purity nickel sulfate
EP2949626A4 (en) * 2013-01-25 2016-12-21 Sumitomo Metal Mining Co METHOD FOR PRODUCING HIGH-PURITY NICKEL SULPHATE AND METHOD FOR REMOVING POLLUTION ELEMENTS FROM A NICKEL-BASED SOLUTION
US20200109462A1 (en) * 2017-06-14 2020-04-09 Nmr 360 Inc Method for the production of cobalt and associated oxides from various feed materials
CN111278997A (zh) * 2017-06-14 2020-06-12 城市采矿有限公司 由各种供给材料生产钴及相关氧化物的方法
CN108844949A (zh) * 2018-08-28 2018-11-20 长春黄金研究院有限公司 一种准确高效的矿石中铂钯含量的测定方法
EP3945068B1 (en) 2020-07-10 2024-01-17 Northvolt AB Process and method for producing crystallized metal sulfates
CN114015872A (zh) * 2022-01-06 2022-02-08 矿冶科技集团有限公司 复杂硫化镍矿低温活化加压浸出的方法

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FI50639B (fi) 1976-02-02
YU241569A (en) 1977-06-30
BE740061A (fi) 1970-03-16
FI50639C (fi) 1976-05-10
DE1952751B2 (de) 1971-04-08
NO126744B (fi) 1973-03-19
YU33670B (en) 1977-12-31
DE1952751A1 (fi) 1971-04-08
JPS5013214B1 (fi) 1975-05-17
FR1597569A (fi) 1970-06-29
CS184306B2 (en) 1978-08-31
GB1287920A (fi) 1972-09-06

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