CN111349781A - Method for reducing acid in copper sulfide concentrate by oxygen pressure leaching - Google Patents
Method for reducing acid in copper sulfide concentrate by oxygen pressure leaching Download PDFInfo
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- CN111349781A CN111349781A CN202010291293.9A CN202010291293A CN111349781A CN 111349781 A CN111349781 A CN 111349781A CN 202010291293 A CN202010291293 A CN 202010291293A CN 111349781 A CN111349781 A CN 111349781A
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- oxygen pressure
- pressure leaching
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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
- C22B3/08—Sulfuric acid, other sulfurated 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
- C22B15/0071—Leaching or slurrying with acids or salts thereof containing sulfur
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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
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/12—Electrolytic production, recovery or refining of metals by electrolysis of solutions of copper
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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Abstract
The invention discloses a method for reducing acid in copper sulfide concentrate by oxygen pressure leaching, which comprises the following steps: (1) adding water into copper sulfide concentrate, finely grinding, adding waste electrolyte for size mixing, and returning to an oxygen pressure leaching solution for ore pulp preparation; (2) pumping the prepared ore pulp into an autoclave, introducing oxygen at the same time, carrying out oxygen pressure leaching, returning one part of the obtained leachate to the step (1) for ore pulp preparation, and entering the other part into the subsequent step; (3) the oxygen pressure leaching solution entering the step is neutralized by limestone, and the neutralized supernatant is sent to electrodeposition to produce electrodeposited copper. The invention utilizes the oxygen pressure leaching solution to return to prepare the ore pulp, reduces the initial acid of the oxygen pressure leaching solution and the final acid of the oxygen pressure leaching solution, namely, the initial acid is high in the oxygen pressure leaching process, and the final acid is low in the oxygen pressure leaching process. The invention utilizes the return of the oxygen pressure leaching solution to prepare ore pulp to reduce the acidity of the oxygen pressure leaching solution, can reduce the dosage of the neutralizing agent limestone in the subsequent neutralization process and achieves the purpose of reducing the loss of copper carried away by the neutralization slag.
Description
Technical Field
The invention belongs to the technical field of non-ferrous metal hydrometallurgy, and particularly relates to an oxygen pressure leaching deacidification method for copper sulfide concentrate.
Background
At present, in the world, low-grade copper-containing materials are mostly recovered by a wet copper extraction technology, and copper sulfide concentrate is mostly recovered by a pyrometallurgical copper smelting technology. The pyrometallurgical copper smelting produces a large amount of sulfuric acid, and in some areas rich in copper sulfide concentrate, but the sulfuric acid is difficult to sell, store and transport, the pyrometallurgical copper smelting technology can not be implemented obviously.
Because the oxygen pressure leaching wet method copper extraction has the advantages of high efficiency, environmental protection and no sulfuric acid generation, the defects of pyrometallurgical copper smelting can be overcome, but for the oxygen pressure leaching wet method copper extraction technology, the biggest challenge is how to reduce the acidity in the leaching solution so as to reduce the loss of large amount of neutralization slag and copper brought away in the subsequent neutralization process. Taking copper sulphide concentrates, e.g. chalcopyrite, for example, their molecular formula CuFeS2The iron-containing copper leaching agent contains Fe, and the leaching rate of copper can be improved only by leaching the iron in the process of oxygen pressure leaching of the copper, a large amount of sulfuric acid is consumed in the process, but a large amount of sulfuric acid is released in the process of hydrolysis iron precipitation of the leached iron. The acidity of the leachate is high, a large amount of neutralizing agent such as limestone needs to be added in the subsequent neutralization process, a large amount of neutralized slag is produced, and partial copper can be taken away in the neutralization process and the process of separating the neutralized slag, so that the loss of copper is caused.
Disclosure of Invention
The invention aims to provide a method for reducing acid in copper sulfide concentrate by oxygen pressure leaching, which can effectively reduce the acidity of a leaching solution, thereby reducing the use of a neutralizer and reducing the loss of copper.
The method for reducing acid in the copper sulfide concentrate by oxygen pressure leaching comprises the following steps:
(1) adding water into copper sulfide concentrate, finely grinding, adding waste electrolyte for size mixing, and returning to an oxygen pressure leaching solution for ore pulp preparation;
(2) pumping the prepared ore pulp into an autoclave, introducing oxygen at the same time, carrying out oxygen pressure leaching, returning one part of the obtained leachate to the step (1) for ore pulp preparation, and entering the other part into the subsequent step;
(3) the oxygen pressure leaching solution entering the step is neutralized by limestone, and the neutralized supernatant is sent to electrodeposition to produce electrodeposited copper.
In the step (1), the adding flow rate ratio of the copper sulfide concentrate, the waste electrolyte and the oxygen pressure leaching liquid is (2-4) kg/h, (6-9) L/h, (5-7L)/h, and the liquid-solid ratio needs to be controlled to be 3-5: 1 in the ore pulp preparation process.
In the step (2), the oxygen pressure leaching temperature is 140-160 ℃, the leaching pressure is 1.2-1.5 Mpa, and the leaching time is 2.0-3.0 h; the oxygen pressure leaching solution returned to the step (1) accounts for 40-60% of the total oxygen pressure leaching solution; final acid H of the oxygen pressure leaching solution2SO4Less than 30 g/L.
And (3) neutralizing until the pH value is 2.5-3.5.
The method has the beneficial effects that (1) the oxygen pressure leaching solution is returned to prepare the ore pulp, so that the initial acid in the oxygen pressure leaching process is reduced, and the final acid (H) of the oxygen pressure leaching solution can be reduced2SO4Less than 30g/L), namely, the initial acid is high in the oxygen pressure leaching process, and the final acid is low when the initial acid is low. (2) The invention utilizes the return of the oxygen pressure leaching solution to prepare ore pulp to reduce the acidity of the oxygen pressure leaching solution, can reduce the dosage of the neutralizing agent limestone in the subsequent neutralization process and achieves the purpose of reducing the loss of copper carried away by the neutralization slag. (3) In the invention, although the system increases the return quantity of the oxygen pressure leaching solution, namely the circulation quantity, namely the solution yield is low, the circulation quantity of the waste electrolyte is correspondingly reduced, and the direct copper yield is unchanged.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The process flow of the invention is shown in figure 1 and specifically comprises the following steps: copper sulfide concentrate (main component CuFeS)2) Adding water for fine grinding, adding waste electrolyte for size mixing, returning oxygen pressure leaching liquid, wherein the returning amount is 40% -50% of the output volume, controlling the liquid-solid ratio to be 3-5: 1 to prepare ore pulp, pumping the prepared ore pulp into an autoclave, introducing oxygen, controlling the oxygen pressure leaching temperature to be 140-160 ℃, the pressure to be 1.2-1.5 Mpa, and the reaction time to be 2.0-3.0 h. And (3) cooling and depressurizing the ore pulp after the reaction, carrying out liquid-solid separation, producing an oxygen pressure leaching solution, sending the oxygen pressure leaching solution to a subsequent neutralization process, neutralizing the obtained solution to a pH value of 2.5-3.5 by using limestone, and sending the neutralized supernatant to electrodeposition to produce electrodeposited copper.
Example 1
Copper sulfide concentrate (main component CuFeS)2) Adding water at a rate of 3kg/H, grinding, adding waste electrolyte (H in waste electrolyte)2SO4Concentration of 160g/L)9L/h pulp mixing, simultaneously returning 6L/h oxygen pressure leaching solution, controlling the liquid-solid ratio to be 5:1 to prepare ore pulp, pumping the prepared ore pulp into a 30L autoclave, simultaneously introducing oxygen, controlling the leaching temperature to be 145 ℃, the pressure to be 1.2Mpa, the reaction time to be 2.0h, cooling and depressurizing the ore pulp after reaction, separating liquid from solid, producing 9L/h oxygen pressure leaching solution, and 30g/LH of final acid2SO4(the total generated oxygen pressure leaching solution is 15L/h, wherein 6L/h leaching solution (40%) returns to the size mixing step, the rest 9L/h enters the subsequent step), the neutralization process is carried out, limestone is adopted for neutralization till the pH value is 3.2, the neutralization slag carries out copper loss of 1.37%, and the supernatant is neutralized and sent to electrodeposition for producing electrodeposited copper.
Example 2
Copper sulfide concentrate (main component CuFeS)2) Adding water at a rate of 3kg/H, grinding, adding waste electrolyte (H in waste electrolyte)2SO4Concentration of 160g/L)6L/h pulp mixing, returning 6L/h oxygen pressure leaching solution, controlling liquid-solid ratio to be 4:1, preparing ore pulp, pumping the prepared ore pulp into a 30L autoclave, introducing oxygen, controlling leaching temperature to be 155 ℃, pressure to be 1.5Mpa, reaction time to be 2.5h, cooling and depressurizing the ore pulp after reaction, performing liquid-solid separation, producing 6L/h oxygen pressure leaching solution, and obtaining 26g/LH of final acid2SO4(the total generated oxygen pressure leaching solution is 12L/h, wherein 6L/h leaching solution (50%) returns to the size mixing step, the rest 6L/h enters the subsequent step), the neutralization process is carried out, limestone is adopted for neutralization till the pH value is 2.8, the neutralization slag carries out copper loss of 1.16%, and the supernatant is neutralized and sent to electrodeposition for producing electrodeposited copper.
Comparative example 1
According to the method in the example 1, the leaching solution is not circulated, the adding speed of the copper sulfide concentrate is 3kg/h, the adding speed of the waste electrolyte is 15L/h, the liquid-solid ratio is controlled to be 5:1, and the pulp is prepared, and other process conditions are consistent with the example 1.
Comparative example 2
According to the method in the example 2, the leaching solution is not circulated, the adding speed of the copper sulfide concentrate is 3kg/h, the adding speed of the waste electrolyte is 12L/h, the liquid-solid ratio is controlled to be 4:1, the ore pulp is prepared, and other process conditions are consistent with the example 2.
Table 1 results of comparative examples
| Comparative example 1 | Comparative example 2 | |
| Final acid (H) of leachate2SO4) | 81g/L | 70g/L |
| The neutralized slag carries away copper loss | 4.80％ | 3.71％ |
According to the embodiment 1 and the comparative example 1, and the embodiment 2 and the comparative example 2, it can be obtained that the final acid of the oxygen pressure leaching solution can be obviously reduced by circulating part of the oxygen pressure leaching solution, so that the use amount of lime can be reduced, and the loss of copper can be reduced.
Claims (6)
1. A method for reducing acid in copper sulfide concentrate by oxygen pressure leaching comprises the following steps:
(1) adding water into copper sulfide concentrate, finely grinding, adding waste electrolyte for size mixing, and returning to an oxygen pressure leaching solution for ore pulp preparation;
(2) pumping the prepared ore pulp into an autoclave, introducing oxygen at the same time, carrying out oxygen pressure leaching, returning one part of the obtained leachate to the step (1) for ore pulp preparation, and entering the other part into the subsequent step;
(3) the oxygen pressure leaching solution entering the step is neutralized by limestone, and the neutralized supernatant is sent to electrodeposition to produce electrodeposited copper.
2. The method for reducing acid in the copper sulfide concentrate by oxygen pressure leaching according to claim 1, wherein in the step (1), the feeding flow rate ratio of the copper sulfide concentrate to the waste electrolyte to the oxygen pressure leaching solution is (2-4) kg/h, (6-9) L/h, (5-7) L/h, and the liquid-solid ratio needs to be controlled to be 3-5: 1 in the pulp preparation process.
3. The method for reducing acid in the copper sulfide concentrate by oxygen pressure leaching according to claim 1, wherein in the step (2), the temperature of the oxygen pressure leaching is 140-160 ℃, the leaching pressure is 1.2-1.5 MPa, and the leaching time is 2.0-3.0 h.
4. The method for reducing acid in the oxygen pressure leaching of the copper sulfide concentrate according to claim 1, wherein in the step (2), the oxygen pressure leaching solution returned to the step (1) accounts for 40-60% of the total oxygen pressure leaching solution.
5. The method of oxygen pressure leaching deacidification of copper sulfide concentrate according to claim 1, wherein in said step (2), said oxygen pressure leaching solution H is selected from the group consisting of2SO4Concentration ofShould not be greater than 30 g/L.
6. The method for reducing acid in the oxygen pressure leaching of the copper sulfide concentrate according to claim 1, wherein in the step (3), the copper sulfide concentrate is neutralized to have a pH of 2.5-3.5.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101481755A (en) * | 2009-02-17 | 2009-07-15 | 昆明理工大学 | Method for leaching vanadium from vanadium-containing coal mine |
| CN101643857A (en) * | 2009-08-25 | 2010-02-10 | 西部矿业股份有限公司 | Comprehensive recovery method of complex polymetal sulphide ore containing copper, lead and zinc |
| CN101876005A (en) * | 2009-11-19 | 2010-11-03 | 中南大学 | Method for extracting aurum from difficult-to-handle sulphide ore aurum concentrate by two-segment pressurization leaching method |
| CN103184335A (en) * | 2011-12-31 | 2013-07-03 | 北京有色金属研究总院 | Low-grade multi-metal sulfide mineral selective bioleaching technology |
| CN104947145A (en) * | 2015-06-10 | 2015-09-30 | 云南驰宏锌锗股份有限公司 | Method of balancing acid in high-lead copper sulphate oxygen pressure leaching-electrodepositing process |
-
2020
- 2020-04-14 CN CN202010291293.9A patent/CN111349781B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101481755A (en) * | 2009-02-17 | 2009-07-15 | 昆明理工大学 | Method for leaching vanadium from vanadium-containing coal mine |
| CN101643857A (en) * | 2009-08-25 | 2010-02-10 | 西部矿业股份有限公司 | Comprehensive recovery method of complex polymetal sulphide ore containing copper, lead and zinc |
| CN101876005A (en) * | 2009-11-19 | 2010-11-03 | 中南大学 | Method for extracting aurum from difficult-to-handle sulphide ore aurum concentrate by two-segment pressurization leaching method |
| CN103184335A (en) * | 2011-12-31 | 2013-07-03 | 北京有色金属研究总院 | Low-grade multi-metal sulfide mineral selective bioleaching technology |
| CN104947145A (en) * | 2015-06-10 | 2015-09-30 | 云南驰宏锌锗股份有限公司 | Method of balancing acid in high-lead copper sulphate oxygen pressure leaching-electrodepositing process |
Non-Patent Citations (1)
| Title |
|---|
| 赵天从主编: "《重金属冶金学 上册》", 31 December 1981, 冶金工业出版社 * |
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