CN111187922B - Method for selectively leaching nickel from high-nickel copper matte under normal pressure - Google Patents
Method for selectively leaching nickel from high-nickel copper matte under normal pressure Download PDFInfo
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- CN111187922B CN111187922B CN202010099224.8A CN202010099224A CN111187922B CN 111187922 B CN111187922 B CN 111187922B CN 202010099224 A CN202010099224 A CN 202010099224A CN 111187922 B CN111187922 B CN 111187922B
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- C—CHEMISTRY; METALLURGY
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- 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
- C22B23/043—Sulfurated acids or salts thereof
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- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
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- C22B7/007—Wet processes by acid leaching
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Abstract
The method comprises the steps of grinding the high-nickel copper matte, adding dilute sulfuric acid solution and catalyst, performing selective leaching under normal pressure to obtain nickel sulfate solution and leaching slag, returning leaching liquor to leach enriched nickel, performing iron removal, concentrating and crystallizing to obtain a crude nickel sulfate product, recovering nickel, and returning the leaching slag to a copper smelting process when the leaching slag is low-nickel copper matte. The method can effectively separate the copper and the nickel in the high-nickel copper matte under normal pressure, and can produce a crude nickel sulfate product. The method is simple and easy to implement, short in flow, free of waste gas and waste water generation and discharge, energy-saving and environment-friendly.
Description
Technical Field
The invention belongs to the technical field of hydrometallurgy, and particularly relates to a method for treating high-nickel copper matte.
Background
Matte is an intermediate product produced in the smelting process of non-ferrous metals such as copper, nickel and the like. In the copper smelting process, nickel enters copper matte in the form of sulfide, and sometimes high-nickel copper matte containing about 60% of copper and more than 2% of nickel is produced. Nickel is an impurity which is difficult to remove in copper fire refining, and most of nickel enters electrolyte in the form of ions and is continuously enriched. The nickel has great influence on the electrolytic refining of copper, and the problems of anode passivation, high anode mud rate, difficult anode mud sedimentation, more cathode copper surface grains, easy oxidation and blackening and the like are easily caused in the electrolytic process of high-nickel anode copper. Therefore, measures are taken to separate copper and nickel in the nickel-copper matte in production. The existing copper-nickel separation method comprises a pyrogenic process and a wet process. Wherein, the pyrometallurgical process, namely the layered smelting method, is to mix and melt nickel-copper-matte and sodium sulfide, and the copper sulfide is very soluble in Na in a molten state2In S, nickel sulfide is not easily dissolved in Na2In S, most of the copper sulfide enters Na2The S phase floats on the top layer due to its low density, while the nickel sulfide remains on the bottom layer due to its high density. When the temperature drops to the freezing temperature, the two are separated more thoroughly. The method has complicated processPoor dynamic condition, high production cost and low metal recovery rate. The wet process can be divided into acid selective leaching, chlorination leaching and pressurized ammonia leaching. The acid selective leaching adopts a leaching method combining normal pressure and pressurization, the reaction is carried out at high temperature and high pressure, high-pressure equipment is required, and the equipment investment is large. The chlorination leaching method has high requirements on equipment corrosion resistance, and the potential of a leaching system needs to be controlled in order to reduce the dissolution of noble metals in the leaching process. The pressurized ammonia leaching process flow is short, but the problem of ammonia nitrogen wastewater is prominent.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provides a treatment method for selectively leaching nickel from high-nickel copper matte, which can effectively separate copper and nickel in the high-nickel copper matte under normal pressure and can produce a crude nickel sulfate product.
The purpose of the invention is realized by the following technical scheme:
a method for selectively leaching nickel from high-nickel copper matte under normal pressure comprises the following steps of (1) selectively leaching the nickel from the high-nickel copper matte, wherein the high-nickel copper matte contains 55-60% of copper, 2-6% of nickel, 10-15% of iron and 20-25% of sulfur; the method comprises the following steps:
(1) selective leaching: grinding the high-nickel copper matte, leaching the high-nickel copper matte by using a dilute sulfuric acid solution and a catalyst at normal pressure, reacting for 2-6 hours at the temperature of 60-95 ℃, allowing nickel in the high-nickel copper matte to enter the solution, inhibiting copper in the slag, filtering to obtain a leaching solution and leaching slag, wherein the leaching solution is a nickel sulfate solution, and washing and filtering the leaching slag by using water to obtain low-nickel copper matte; the catalyst is copper sulfate;
(2) removing iron from the leaching solution: adding hydrogen peroxide and potassium sulfate into the leachate, and filtering to obtain iron-removed liquid and iron-removed slag, wherein the iron-removed liquid is a nickel sulfate solution, and the iron-removed slag is washed by water and filtered to obtain iron vitriol slag;
(3) enriching nickel in the leaching solution: returning the iron-removed liquid to the step (1) for continuous leaching until the nickel in the iron-removed liquid is enriched to 35-40 g/L;
(4) evaporation cooling crystallization: and (3) evaporating and concentrating the iron-removed solution enriched with nickel, cooling and crystallizing, and filtering to obtain crude nickel sulfate and crystallization mother liquor.
Further, in the selective leaching of the step (1), the high nickel copper matte is ground to-100 meshes.
Further, in the selective leaching in the step (1), the obtained leachate is returned to be continuously leached until the concentration of iron ions in the leachate is 30-36 g/L, and then hydrogen peroxide and potassium sulfate are added into the leachate to remove iron according to the step (2).
Further, in the selective leaching in the step (1), the initial concentration of the dilute sulfuric acid is 30-100 g/L, the volume-to-mass ratio of the dilute sulfuric acid solution to the high-nickel copper matte is 3-10: 1 in terms of ml/g, and the addition amount of the catalyst is 0.05-0.2 times of the mass of the high-nickel copper matte.
Further, removing iron from the leachate obtained in the step (2), wherein the dosage of hydrogen peroxide is 2 times of the theoretical amount required by reaction with iron, the dosage of potassium sulfate is 1.2 times of the theoretical amount required by reaction with iron, the iron removal temperature is 90-95 ℃, and the iron removal time is 2-4 hours.
The main purpose of the selective leaching of the invention is to convert nickel sulfide in the high-nickel copper matte into nickel sulfate to enter the leaching solution. The nickel in the high-nickel copper matte is mainly NiS and Ni7S6、Ni3S2In the form of copper sulfide, the copper is mainly in the form of sulfide, and under the condition of acid copper sulfate solution leaching, nickel sulfide passes through Cu2+Substituted or by Cu2+Oxidizing the copper to solution, separating the copper from the leached slag, and returning the nickel-removed copper matte to the copper smelting process. The main reaction formula is as follows:
Ni7S6+2CuSO4→Cu2S+5NiS+2NiSO4 (1)
Ni3S2+3CuSO4+3Cu2S→Cu9S5+3NiSO4 (2)
NiS+CuSO4→CuS+NiSO4 (3)
the invention has the following beneficial effects:
(1) the reaction process does not need to be carried out at high temperature and high pressure, the copper and the nickel in the high-nickel copper matte can be effectively separated by leaching at normal pressure, the process is simple and easy to implement, the flow is short, no waste gas or waste water is generated and discharged, and the energy is saved and the environment is protected.
(2) The leaching rate of nickel is up to more than 85 percent, and copper is not leached and is enriched in the leaching slag and can be used as low-nickel copper matte to return to the copper smelting process.
(3) Can effectively open the way of nickel in the copper smelting process, control the amount of nickel entering the blister copper and the anode copper, and simultaneously recover the blister nickel sulfate by-product, thereby creating benefits.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
A method for selectively leaching nickel from high-nickel copper matte comprises 55-60% of copper, 2-6% of nickel, 10-15% of iron, 20-25% of sulfur and a small amount of other elements and impurities. As shown in fig. 1, the method is as follows:
(1) selective leaching: grinding the high-nickel copper matte to-100 meshes, leaching with a dilute sulfuric acid solution and a catalyst at normal pressure, reacting at 60-95 ℃ for 2-6 hours to enable nickel in the high-nickel copper matte to enter the solution, inhibiting copper in slag, filtering to obtain a leaching solution and leaching slag, wherein the leaching solution is a nickel sulfate solution, the leaching slag is low-nickel copper matte, washing and filtering with water to obtain the low-nickel copper matte, and the washing water can be returned for continuous washing. The initial concentration of dilute sulfuric acid used for selective leaching is 30-100 g/L, the volume mass ratio of dilute sulfuric acid solution to high-nickel copper matte is 3-10: 1 in terms of ml/g, the concentration of catalyst copper sulfate is 3-10 g/L, and the addition amount of the catalyst is 0.05-0.2 time of the weight of the high-nickel copper matte;
(2) removing iron from the leaching solution: and (2) returning the leachate obtained in the step (1) to continuously leach until the concentration of iron ions in the leachate is 30-36 g/L, then adding hydrogen peroxide and potassium sulfate into the leachate, and filtering to obtain a liquid after iron removal and iron-removing residues, wherein the liquid after iron removal is a nickel sulfate solution, and the liquid after iron removal is washed by water and filtered to obtain iron vitriol residues. The dosage of hydrogen peroxide is 2 times of the theoretical amount required by the reaction with iron, the dosage of potassium sulfate is 1.2 times of the theoretical amount required by the reaction with iron, the iron removal temperature is 90-95 ℃, and the iron removal time is 2-4 hours;
(3) enriching nickel in the leaching solution: returning the iron-removed liquid to the step (1) for continuous leaching until the nickel in the iron-removed liquid is enriched to 35-40 g/L;
(4) evaporation cooling crystallization: and (3) evaporating and concentrating the iron-removed liquid enriched with nickel until the specific gravity is 1.45-1.5, cooling to 35 ℃, and filtering and separating to obtain crude nickel sulfate and a crystallization mother liquor. And (3) after the washing water and the sulfuric acid are supplemented to the crystallization mother liquor, returning to the step (1) for continuous selective leaching.
Example 1
The method for selectively leaching nickel from high-nickel copper matte comprises the following steps:
(1) grinding nickelic copper matte containing 57.5% of copper, 2.1% of nickel, 10.3% of iron and 22% of sulfur and containing a small amount of other elements and impurities to-100 meshes, adding dilute sulfuric acid and copper sulfate for selective leaching, wherein the leaching conditions are as follows: the initial concentration of dilute sulfuric acid is 30g/L, the liquid-solid volume mass ratio of dilute sulfuric acid to high-nickel copper matte is 3:1(ml: g), the concentration of copper sulfate is 10g/L, the addition amount of copper sulfate is 0.05 times of the weight of high-nickel copper matte, the leaching reaction temperature is 60 ℃, the reaction time is 6 hours, a nickel sulfate solution and leaching residues are obtained, the leaching residues are washed by water, and low-nickel copper matte containing 64.5% of copper, 0.27% of nickel and 7.97% of iron is obtained after filtration; the washing water for washing the leaching residue can be returned for washing continuously;
(2) the leachate returns to the step (1) for leaching, when the concentration of iron ions in the leachate is enriched to 33.5g/L, hydrogen peroxide and potassium sulfate are added for removing iron, the dosage of hydrogen peroxide is 2 times of the theoretical quantity required for reacting with iron, the dosage of potassium sulfate is 1.2 times of the theoretical quantity required for reacting with iron, the iron removal temperature is 90-95 ℃, the iron removal time is 2 hours, the iron-removed liquid containing 0.5g/L of iron and iron removal slag are obtained after filtering and separation, and the iron removal slag is washed and filtered to obtain iron vitriol slag containing 0.11% of nickel;
(3) and (3) returning the liquid after iron removal to the step (1) for continuous leaching, when the concentration of nickel ions in the leaching solution is enriched to 35g/L, removing iron according to the step (2), evaporating and concentrating the liquid after iron removal to the specific gravity of 1.45-1.5, cooling to 35 ℃, and filtering and separating to obtain a crystallization mother liquor containing 74.6g/L nickel and crude nickel sulfate containing 19.4% nickel. And (4) adding washing water and sulfuric acid into the crystallization mother liquor, and returning to the step (1) for continuous selective leaching.
Example 2
The method for selectively leaching nickel from high-nickel copper matte comprises the following steps:
(1) high-nickel copper matte containing 59.5% of copper, 3.25% of nickel, 13.6% of iron and 25% of sulfur is ground to-100 meshes, dilute sulfuric acid and a catalyst are added for selective leaching, and the leaching conditions are as follows: the initial concentration of dilute sulfuric acid is 50g/L, the liquid-solid volume mass ratio of dilute sulfuric acid to high-nickel copper matte is 6:1(ml: g), the concentration of copper sulfate is 6g/L, the addition amount of copper sulfate is 0.1 time of the weight of high-nickel copper matte, the leaching reaction temperature is about 92 ℃, the reaction time is 4 hours, a nickel sulfate solution and leaching residues are obtained, the leaching residues are washed by water, and low-nickel copper matte containing 65.3% of copper, 0.51% of nickel and 9.14% of iron is obtained after filtration; the washing water for washing the leaching residue can be returned for washing continuously;
(2) the leachate returns to the step (1) for leaching, when the concentration of iron ions in the leachate is enriched to 35.5g/L, hydrogen peroxide and potassium sulfate are added for removing iron, the dosage of hydrogen peroxide is 2 times of the theoretical quantity required for reacting with iron, the dosage of potassium sulfate is 1.2 times of the theoretical quantity required for reacting with iron, the iron removal temperature is 90-95 ℃, the iron removal time is 3 hours, the iron-removed liquid containing 0.25g/L of iron and iron removal slag are obtained after filtering and separation, and the iron removal slag is washed and filtered to obtain iron alum slag containing 0.08% of nickel;
(3) and (3) returning the liquid after iron removal to the step (1) for continuous leaching, when the concentration of nickel ions in the leaching solution is enriched to 37.2g/L, removing iron according to the step (2), evaporating and concentrating the liquid after iron removal to the specific gravity of 1.45-1.5, cooling to 35 ℃, and filtering and separating to obtain a crystallization mother liquor containing 73.2g/L nickel and crude nickel sulfate containing 19.1% nickel. And (3) adding washing water and sulfuric acid into the crystallization mother liquor, and returning to the step (1) for continuous selective leaching.
Example 3
The method for selectively leaching nickel from high-nickel copper matte comprises the following steps:
(1) high-nickel copper matte containing 55% of copper, 5.8% of nickel, 14.3% of iron and 20.1% of sulfur is ground to-100 meshes, dilute sulfuric acid and a catalyst are added for selective leaching, and the leaching conditions are as follows: the initial concentration of dilute sulfuric acid is 100g/L, the concentration of copper sulfate is 3g/L, the addition amount of copper sulfate is 0.2 times of the weight of high-nickel copper matte, the liquid-solid volume mass ratio of dilute sulfuric acid to high-nickel copper matte is 10:1(ml: g), the leaching reaction temperature is 95 ℃, the reaction time is 2 hours, a nickel sulfate solution and leaching residues are obtained, the leaching residues are washed by water, and low-nickel copper matte containing 67.5% of copper, 0.85% of nickel and 9.74% of iron is obtained after filtration; the washing water for washing the leaching residue can be returned for washing continuously;
(2) the leachate returns to the step (1) for leaching, when the concentration of iron ions in the leachate is enriched to 30g/L, hydrogen peroxide and potassium sulfate are added for removing iron, the amount of hydrogen peroxide is 2 times of the theoretical amount required for reacting with iron, the amount of potassium sulfate is 1.2 times of the theoretical amount required for reacting with iron, the iron removal temperature is 90-95 ℃, the iron removal time is 4 hours, the iron-removed liquid containing 0.15g/L of iron and iron removal slag are obtained after filtering and separation, and the iron removal slag is washed and filtered to obtain iron alum slag containing 0.08% of nickel;
(3) and (3) returning the liquid after iron removal to the step (1) for continuous leaching, when the concentration of nickel ions in the leaching solution is enriched to 40g/L, removing iron according to the step (2), evaporating and concentrating the liquid after iron removal to the specific gravity of 1.45-1.5, cooling to below 35 ℃, and filtering and separating to obtain 78g/L nickel-containing crystallization mother liquor and 18.5% nickel-containing crude nickel sulfate. And (3) adding washing water and sulfuric acid into the crystallization mother liquor, and returning to the step (1) for continuous selective leaching.
Unless otherwise indicated, all the percentage values of the components appearing in the present invention are mass percentages.
Claims (6)
1. A method for selectively leaching nickel from high-nickel copper matte under normal pressure is characterized by comprising the following steps: the high-nickel copper matte contains 55-60% of copper, 2-6% of nickel, 10-15% of iron and 20-25% of sulfur; the method comprises the following steps:
(1) selective leaching: grinding the high-nickel copper matte, leaching the high-nickel copper matte by using a dilute sulfuric acid solution and a catalyst at normal pressure, reacting for 2-6 hours at the temperature of 60-95 ℃, allowing nickel in the high-nickel copper matte to enter the solution, inhibiting copper in the slag, filtering to obtain a leaching solution and leaching slag, wherein the leaching solution is a nickel sulfate solution, and washing and filtering the leaching slag by using water to obtain low-nickel copper matte; the catalyst is copper sulfate;
(2) removing iron from the leaching solution: adding hydrogen peroxide and potassium sulfate into the leachate, and filtering to obtain iron-removed liquid and iron-removed slag, wherein the iron-removed liquid is a nickel sulfate solution, and the iron-removed slag is washed by water and filtered to obtain iron vitriol slag;
(3) enriching nickel in the leaching solution: returning the iron-removed liquid to the step (1) for continuous leaching until the nickel in the iron-removed liquid is enriched to 35-40 g/L;
(4) evaporation cooling crystallization: and (3) evaporating and concentrating the iron-removed solution enriched with nickel, cooling and crystallizing, and filtering to obtain crude nickel sulfate and crystallization mother liquor.
2. A method for the atmospheric selective leaching of nickel from high-nickel matte according to claim 1, characterized in that in the selective leaching of step (1) the high-nickel matte is ground to-100 mesh.
3. The method according to claim 1, wherein in the selective leaching in step (1), the leachate is returned to continue leaching until the concentration of iron ions in the leachate is 30-36 g/L, and then hydrogen peroxide and potassium sulfate with iron removed are added into the leachate according to step (2).
4. The method for selectively leaching nickel from high-nickel copper matte under normal pressure according to claim 1, 2 or 3, wherein in the selective leaching in the step (1), the initial concentration of the dilute sulfuric acid is 30-100 g/L, the volume-mass ratio of the dilute sulfuric acid solution to the high-nickel copper matte is 3-10: 1 in ml/g, and the addition amount of the catalyst is 0.05-0.2 times of the mass of the high-nickel copper matte.
5. The method for selectively leaching nickel from high-nickel copper matte at normal pressure according to claim 1, 2 or 3, wherein the leachate obtained in step (2) is used for removing iron, the dosage of hydrogen peroxide is 2 times of the theoretical amount required for reacting with iron, the dosage of potassium sulfate is 1.2 times of the theoretical amount required for reacting with iron, the iron removal temperature is 90-95 ℃, and the iron removal time is 2-4 hours.
6. The method for selectively leaching nickel from high-nickel copper matte under normal pressure according to claim 4, wherein the leachate obtained in the step (2) is subjected to iron removal, the dosage of hydrogen peroxide is 2 times of the theoretical quantity required for reaction with iron, the dosage of potassium sulfate is 1.2 times of the theoretical quantity required for reaction with iron, the iron removal temperature is 90-95 ℃, and the iron removal time is 2-4 hours.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US4100043A (en) * | 1976-09-17 | 1978-07-11 | Amax Inc. | Atmospheric leach ion-exchange process for treating iron-containing nickel-copper matte |
| CA1173655A (en) * | 1981-10-30 | 1984-09-04 | Derek G.E. Kerfoot | Acid leach process for treating magnetic and non- magnetic nickel-copper mattes |
| GB9121528D0 (en) * | 1991-10-10 | 1991-11-27 | Sherritt Gordon Ltd | Process for upgrading copper sulphide residues containing nickel and arsenic |
| US5344479A (en) * | 1992-03-13 | 1994-09-06 | Sherritt Gordon Limited | Upgrading copper sulphide residues containing nickel and arsenic |
| FI97154C (en) * | 1994-11-15 | 1996-10-25 | Outokumpu Eng Contract | Method for dissolving nickel copper rock |
| US5993514A (en) * | 1997-10-24 | 1999-11-30 | Dynatec Corporation | Process for upgrading copper sulphide residues containing nickel and iron |
| CN101195857B (en) * | 2007-12-20 | 2010-07-21 | 金川集团有限公司 | Solvent extraction method for acquiring alloy with magnetic separation copper nickel matte |
| CN101509072B (en) * | 2009-02-18 | 2012-02-29 | 中南大学 | Method for extracting valuable metals from laterite nickel mine with hydrochloric acid full-closed circulation method |
| CN107012324B (en) * | 2017-04-10 | 2018-09-28 | 中南大学 | A kind of method and its system recycling main accompanying element from cu-ni sulphide ore |
| AU2018252056B2 (en) * | 2017-04-10 | 2020-07-23 | Central South University | Method for comprehensively recycling copper-nickel sulfide ore and system thereof |
| CN107058730B (en) * | 2017-04-10 | 2018-10-16 | 中南大学 | A kind of method and its system to cu-ni sulphide ore comprehensive utilization |
| CN107338357B (en) * | 2017-07-07 | 2019-01-22 | 金川集团股份有限公司 | A kind of nitric acid Selectively leaching method of the high iron alloy powder of low nickel |
| CN110342590A (en) * | 2019-08-19 | 2019-10-18 | 中南大学 | A kind of method that normal pressure decomposition converter mattes prepare nickel sulfate |
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