CN112442591B - Copper-nickel leaching and iron separation method for copper-nickel sulfide ore - Google Patents
Copper-nickel leaching and iron separation method for copper-nickel sulfide ore Download PDFInfo
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- CN112442591B CN112442591B CN201910814901.7A CN201910814901A CN112442591B CN 112442591 B CN112442591 B CN 112442591B CN 201910814901 A CN201910814901 A CN 201910814901A CN 112442591 B CN112442591 B CN 112442591B
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
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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
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
- C22B15/0069—Leaching or slurrying with acids or salts thereof containing halogen
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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
- C22B23/0423—Halogenated acids or salts thereof
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- 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
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Abstract
The invention discloses a copper-nickel leaching and iron separating method for copper-nickel sulfide ores. According to the method, the oxidant chlorine oxyacid salt is added into the copper nickel sulfide ore, so that copper and nickel elements are leached, and iron elements generate precipitation. According to the invention, the chlorine oxyacid salt is used as an oxidant, harmful ions are not additionally introduced, the complete leaching of copper and nickel ions can be realized through a simple process, meanwhile, iron is directly separated in a precipitation form, the reaction condition is mild, the reaction time is short, the equipment is simple, the operation is simple, the cost is low, and the method is suitable for popularization and application.
Description
Technical Field
The invention belongs to the technical field of hydrometallurgy, and particularly relates to a copper-nickel leaching and iron separation method for copper-nickel sulfide ores.
Background
Nickel and copper elements are essential basic materials and important strategic materials for national economy, social development, national defense industry construction and scientific technology development, copper-nickel sulfide ore is a main nickel source, copper is an important source, and copper-nickel ore smelting is an important step for producing nickel and copper simple substances. Smelting of copper-nickel sulfide ore is divided into two kinds of pyrometallurgy and wet method, and pyrometallurgy is widely used. Hydrometallurgy solves the problems of energy consumption and environment in the pyrometallurgy to a certain extent, and the leaching process is an important step in hydrometallurgy.
The copper nickel sulfide ore leaching process can be mainly divided into acid leaching, ammonia leaching, chlorine leaching and bacterial leaching according to the difference of leaching agents. The oxidant for ammonia leaching and acid leaching is oxygen, the oxidant for chlorine leaching is chlorine, and the oxidant for bacterial leaching is oxidase produced by bacteria. In addition, the use of dichromate, ozone, potassium permanganate and other oxidizing agents as leaches has also been studied. Depending on the raw material to be leached, concentrate leaching and high nickel matte leaching can be classified. The chlorine leaching method of the high-nickel matte is a forming process in industry, is used as a subsequent process of pyrometallurgy, has high efficiency and high recovery rate of the chlorine leaching of the high-nickel matte, and can realize the effective separation of copper and nickel. However, at the same time, chlorine is expensive, and has high requirements on corrosion resistance of equipment, so that the production cost is high. The leaching process using oxygen and bacterial oxidase as oxidants has low efficiency, and the process using dichromate, potassium permanganate and the like as oxidants introduces other ions such as chromate, manganese ions and the like, so that the difficulty in subsequent treatment is increased.
Therefore, there is a need to find a simple leaching process that is efficient in leaching, cost-effective, and does not produce harmful ions.
Disclosure of Invention
The invention aims to provide a copper-nickel leaching and iron separating method for copper-nickel sulfide ores, which is convenient to operate, mild in reaction condition and low in cost, does not additionally introduce harmful ions, can completely leach copper and nickel, and simultaneously realizes direct separation by fixing iron elements in a precipitation form.
In order to solve the technical problems, the invention provides the following technical scheme:
a method for leaching copper-nickel ions from copper-nickel sulfide ore is provided, wherein an oxidant chlorooxonate is added into the copper-nickel sulfide ore to leach copper and nickel, and iron generates precipitation.
According to the scheme, when the oxidant is sodium chlorate, the specific steps are as follows:
(1) Mixing copper nickel sulfide ore, sodium chlorate and distilled water for ball milling;
(2) Drying the ball-milled sample obtained in the step (1) at room temperature until the dehydration is 60-80%;
(3) Heating the dried sample in the step (2) to react; the method comprises the steps of carrying out a first treatment on the surface of the
(4) Putting the sample reacted in the step (3) into distilled water, leaching copper and nickel, dissolving the copper and nickel into the distilled water, and generating precipitated NaFe by iron 3 (SO 4 ) 2 (OH) 6 。
The oxidant sodium chlorate and the copper nickel sulfide ore are mixed and ball-milled, so that the tight contact of the oxidant sodium chlorate and the copper nickel sulfide ore after being fully crushed can be promoted, and the existence of water reduces the oxidability of the sodium chlorate and avoids direct reaction after the sodium chlorate and the copper nickel sulfide ore are mixed; evaporating at room temperature to remove 60% -80% of water to convert the mixture from slurry into quasi-solid with low water content, and reversely removing the residual waterThe presence of a reactant; oxidation-reduction reaction occurs in the heating process, S element is oxidized, copper ions and nickel ions are directly leached in distilled water, and iron ions are used for precipitating NaFe 3 (SO 4 ) 2 (OH) 6 The form is fixed.
According to the scheme, the mass ratio of the copper nickel sulfide ore to distilled water in the step (1) is 1: (1-1.5); the mass ratio of the copper nickel sulfide ore to the sodium chlorate is 1: (0.85-1.30).
According to the scheme, the ball milling conditions in the step (1) are as follows: the rotating speed is 200-400 rpm, and the time is 50-100 min.
According to the scheme, the heating reaction conditions in the step (3) are as follows: the temperature is 100-400 ℃ and the time is 100-150 min.
According to the scheme, the leaching time in the step (4) is 20-40 min.
According to the scheme, in the leaching process in the step (4), an ultrasonic wave, oscillation or stirring mode is selected.
According to the scheme, when the oxidant is sodium chlorite, the specific steps are as follows:
(1) Preparing sodium chlorite solution with the concentration of 0.1-0.5 mol/L;
(2) Mixing copper nickel sulfide ore with the sodium chlorite solution prepared in the step (1) at normal temperature for reaction, leaching copper and nickel into the water solution after the reaction is finished, and generating precipitated ferroferric oxide by iron.
Regulating and controlling the concentration of sodium chlorite solution, allowing sodium chlorite to react with copper nickel sulfide ore mildly, oxidizing S element, directly leaching copper ions and nickel ions in distilled water, and fixing iron ions in the form of precipitated ferroferric oxide.
According to the scheme, the mass ratio of the copper-nickel sulfide ore to the sodium chlorite is 1 (1.35-4.45).
According to the scheme, in the step (2), the reaction process selects an ultrasonic wave, oscillation or stirring mode.
According to the scheme, the reaction time in the step (2) is 10-30 min.
The beneficial effects of the invention are as follows:
according to the invention, the oxidant chlorine-oxygen salt is added into the copper-nickel sulfide ore concentrate, so that complete leaching of copper and nickel elements can be realized, and meanwhile, the iron element is fixed by a precipitate, so that the separation of the copper-nickel element and the iron element is directly realized. The method has the advantages of mild reaction conditions, short reaction time, simple equipment, simple operation, low cost, no additional introduction of harmful ions in the reaction process, and suitability for popularization and application.
Drawings
FIG. 1 is an XRD pattern of the leached residue obtained from the copper nickel sulfide ore of example 1 after treatment with sodium chlorate as an oxidizer.
Fig. 2 is an XRD pattern of the leached slag obtained after the copper-nickel sulfide ore of example 3 is treated with sodium chlorite as an oxidizing agent.
The specific embodiment is as follows:
the present invention will be described in further detail with reference to examples for better understanding of the technical scheme of the present invention to those skilled in the art.
Example 1:
some copper-nickel sulphide ore has the main component of nickel pyrite ((Ni, fe) 9 S 8 ) Chalcopyrite (CuFeS) 2 ) And pyrite (FeS) 2 ). The contents of Ni, cu and Fe in the sample were 4.97%, 4.73% and 30.24%, respectively. 1g of a mineral sample and 1.01g of sodium chlorate are taken and added into a ball milling tank, 1g of water is added, and ball milling is carried out for 60min under the condition of low rotation speed of 300 rpm. Taking out the ground sample, drying the sample in a dryer at room temperature for 24 hours, removing 60% of water, heating the sample at 200 ℃ in a muffle furnace for 2 hours, taking out the heated sample, quantitatively placing the sample in a conical flask, adding distilled water, leaching the sample in a water bath oscillator at normal temperature and normal pressure for 30 minutes, wherein Ni and Cu are leached into the distilled water, leaching residues are Fe precipitates, and directly separating Fe from Ni and Cu. The leaching rates were measured as follows: 99.63% of Ni, 99.74% of Cu and 0% of Fe.
FIG. 1 is an XRD pattern of the leached residue after the reaction in this example, showing that the main component of the leached residue is sodium-iron-vanadium (NaFe) 3 (SO 4 ) 2 (OH) 6 )。
The sodium chlorate has excellent leaching effect on copper nickel sulfide ores, and the leaching effect can be realized for 30min at normal temperature and normal pressure, so that complete leaching of copper and nickel elements and fixation of iron elements can be realized, and the iron elements completely form yellow sodium ettringite insoluble salts to be fixed in solid insoluble matters.
Example 2:
some copper-nickel sulphide ore contains chalcopyrite (CuFeS) 2 ) Pyrite (FeS) 2 ) Purple sulfur nickel ore (FeNi 2 S 4 ). The contents of Ni, cu and Fe in the sample are 4.72%, 4.40% and 26.55%, respectively. 1g of a mineral sample and 1.2g of sodium chlorate are taken and added into a ball milling tank, 1g of water is added, and ball milling is carried out for 80 minutes under the condition of low rotation speed of 200 rpm. Taking out the ground sample, drying in a dryer at room temperature for 24h, removing 80% of water, heating at 150 ℃ in a muffle furnace for 2h, taking out the heated sample, quantitatively placing the sample into a conical flask, adding distilled water, leaching at normal temperature and normal pressure in a water bath oscillator for 30min, wherein Ni and Cu are leached into the distilled water, and Fe is NaFe 3 (SO 4 ) 2 (OH) 6 The precipitate form was separated. The leaching rates were measured as follows: 99.49% of Ni, 99.65% of Cu and 0% of Fe.
Example 3:
the main component of the test sample of the main component of a certain copper-nickel sulfide ore is chalcopyrite (CuFeS 2 ) Pyrite (FeS) 2 ) Purple sulfur nickel ore (FeNi 2 S 4 ). The contents of Ni, cu and Fe are 4.72%, 4.40% and 26.55%, respectively. 100mL of sodium chlorite solution with the concentration of 0.3mol/L is prepared, the sodium chlorite solution is placed in an conical flask, and 1g of mineral sample is placed in the solution to form a reaction system, so that the excessive oxidant is ensured. The reaction system is placed in a water bath oscillator (250 rpm) to oscillate for 10min at normal temperature and normal pressure to complete the reaction, wherein Ni and Cu are leached into distilled water, leaching slag is a precipitate of Fe, and Fe is directly separated from Ni and Cu. The leaching rates were measured as follows: 99.99% of Ni, 99.80% of Cu and 0% of Fe.
FIG. 2 is an XRD pattern of the leached residue after the reaction in this example, showing that the main component of the leached residue is ferroferric oxide (Fe 3 O 4 )。
The dilute sodium chlorite solution has excellent leaching effect on copper-nickel sulfide ores, can be leached for 10min at normal temperature and normal pressure to realize complete leaching of copper and nickel elements and fixation of iron elements, and the iron elements are completely fixed in insoluble ferroferric oxide, and in addition, the sodium chlorite is prepared into the dilute solution, so that harmful gas ClO generated in the reaction process can be avoided as much as possible 2 Into the air.
Example 4:
some copper-nickel sulphide ore has the main component of nickel pyrite ((Ni, fe) 9 S 8 ) Chalcopyrite (CuFeS) 2 ) Pyrite (FeS) 2 ). The contents of Ni, cu and Fe in the sample were 4.97%, 4.73% and 30.24%, respectively. 100ml of 0.3mol/L sodium chlorite solution is prepared and put into a conical flask, and 1.5g of ore sample is put into the solution to form a reaction system, so that the excessive oxidant is ensured. The reaction was completed by shaking the reaction system in a water bath shaker (250 rpm) at normal temperature and pressure for 20 minutes, wherein Ni and Cu were leached into distilled water and Fe was separated as a precipitate of ferroferric oxide. The leaching rates were measured as follows: 99.79% of Ni, 99.36% of Cu and 0% of Fe.
Claims (7)
1. A copper-nickel leaching and iron separation method of copper-nickel sulphide ore is characterized in that oxidant chloroxolate is added into the copper-nickel sulphide ore to leach copper and nickel, and iron generates precipitation; wherein:
when the oxidant oxychloride is sodium chlorate, the specific steps are as follows:
(1) Mixing and ball milling copper-nickel sulfide ore, sodium chlorate and distilled water, wherein the mass ratio of the copper-nickel sulfide ore to the distilled water is 1: (1-1.5);
(2) Drying the ball-milled sample obtained in the step (1) at room temperature until the dehydration is 60-80%;
(3) Heating the dried sample in the step (2) to react;
(4) Putting the sample reacted in the step (3) into distilled water, leaching copper and nickel, dissolving the copper and nickel into the distilled water, and forming precipitated NaFe by iron 3 (SO 4 ) 2 (OH) 6 ；
When the oxidant chlorine oxyacid salt is sodium chlorite, the specific steps are as follows:
(1) Preparing sodium chlorite solution with the concentration of 0.1-0.5 mol/L;
(2) Mixing copper nickel sulfide ore with the sodium chlorite solution prepared in the step (1) at normal temperature for reaction, leaching copper and nickel into the water solution after the reaction is finished, and forming precipitated ferroferric oxide by iron.
2. The method for copper-nickel leaching and iron separation of copper-nickel sulfide ore according to claim 1, wherein when the oxidizer chlorine oxyacid salt is sodium chlorate, the mass ratio of copper-nickel sulfide ore to sodium chlorate in the step (1) is 1: (0.85-1.30).
3. The method for copper-nickel leaching and iron separation of copper-nickel sulfide ore according to claim 1, wherein when the oxidizer chlorine oxyacid salt is sodium chlorate, the ball milling conditions in the step (1) are: the rotating speed is 200-400 rpm, and the time is 50-100 min.
4. The method for copper-nickel leaching and iron separation of copper-nickel sulfide ore according to claim 1, wherein when the oxidizing agent chlorine oxyacid salt is sodium chlorate, the heating reaction conditions in the step (3) are: the temperature is 100-400 ℃ and the time is 100-150 min.
5. The method for copper-nickel leaching and iron separation of copper-nickel sulfide ore according to claim 1, wherein when the oxidant chlorine oxyacid salt is sodium chlorate, the leaching time in the step (4) is 20-40 min; the leaching process adopts ultrasonic wave, vibration or stirring mode.
6. The method for leaching copper and nickel from copper and nickel sulfide ores and separating iron according to claim 1, wherein when the oxidant chlorine oxyacid salt is sodium chlorite, the mass ratio of the copper and nickel sulfide ores to the sodium chlorite is 1 (1.35-4.45).
7. The method for copper-nickel leaching and iron separation of copper-nickel sulfide ore according to claim 1, wherein when the oxidant chlorine oxyacid salt is sodium chlorite, the reaction time in the step (2) is 10-30 min; the reaction process is carried out by selecting ultrasonic wave, oscillation or stirring.
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| US20050118081A1 (en) * | 2003-09-30 | 2005-06-02 | Jaguar Nickel Inc. | Process for the recovery of value metals from base metal sulfide ores |
| CN101760611A (en) * | 2010-01-30 | 2010-06-30 | 中南大学 | Method for wet-method oxidative decomposition of metal sulfide ores |
| CN102703693A (en) * | 2012-05-22 | 2012-10-03 | 北京大学 | Method for enriching and recovering metal nickel, copper and cobalt from tailings of copper and nickel mines |
| CN106319228A (en) * | 2016-08-26 | 2017-01-11 | 荆门市格林美新材料有限公司 | Method for recycling nickel, cobalt and manganese synchronously from waste residues containing nickel, cobalt and manganese |
| CN108060301A (en) * | 2017-12-05 | 2018-05-22 | 北京科技大学 | A kind of method that rubidium and by-product active calcium silicate are extracted in the ore from rubidium |
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