CN114214522A - Wet treatment process for refined copper slag - Google Patents
Wet treatment process for refined copper slag Download PDFInfo
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- CN114214522A CN114214522A CN202111586660.9A CN202111586660A CN114214522A CN 114214522 A CN114214522 A CN 114214522A CN 202111586660 A CN202111586660 A CN 202111586660A CN 114214522 A CN114214522 A CN 114214522A
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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
- 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
- C22B7/04—Working-up slag
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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
- C22B15/0078—Leaching or slurrying with ammoniacal solutions, e.g. ammonium hydroxide
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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
- 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
- C22B7/006—Wet processes
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
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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
- 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 relates to a wet treatment process of refined copper slag, which comprises the following steps: step S1, coarsely crushing, finely crushing and ball-milling refined copper slag, wherein the granularity of the refined copper slag reaches-80 to-200 meshes; step S2, leaching the ground refined copper slag and an ammonia water-ammonium sulfate mixed solution at normal temperature and normal pressure, performing solid-liquid separation after leaching, and obtaining a copper ammonia complex solution and metal leaching slag after the solid-liquid separation; step S3, extracting the copper ammonia complex solution and a copper extractant, concentrating copper in the extracted solution into the extractant, and performing back extraction on the extractant through electro-deposition copper-poor liquid or sulfuric acid to obtain a copper-rich solution; step S4, the copper-rich solution enters an electrodeposition copper system for electrodeposition, and a cathode copper finished product is obtained by precipitation on the cathode; the raffinate after extraction is returned to be leached to be used as a leaching bottom liquid. The process has the advantages of simple principle, low energy consumption, mechanized operation in the whole process, low labor intensity of workers, more than or equal to 95 percent of copper recovery rate in the whole process, and capability of returning leached slag to the fuming furnace to continuously recover other metal elements in the leached slag.
Description
Technical Field
The invention relates to the field of non-ferrous metallurgy, in particular to a wet treatment process for refined copper slag.
Background
The method is characterized in that a copper anode plate in the electrolytic copper production process is smelted by adopting an anode furnace, impurity removal is carried out while the anode plate is smelted, oxygen is blown in to remove other metal impurities such as lead, zinc and the like in the smelting process by adding a slagging agent and a reducing agent, part of copper is oxidized together in the process of oxidizing the impurity metals by blown oxygen, and slag containing high copper and generated in the oxidation-reduction smelting process is refined copper slag. According to different raw materials of the anode furnace, the refined copper slag also has metal components except copper, but the main metal elements mainly comprise copper, lead, zinc, tin, nickel, silicon, calcium and iron, wherein the copper mainly exists in a cuprous oxide form, a small amount of copper oxide and a simple substance copper form, the nickel and the tin exist in an alloy form, and the iron, the silicon and the calcium mainly exist in a ferric silicate form and a calcium silicate form.
The traditional treatment method of refined copper slag comprises environment-friendly furnace smelting, anode furnace refining and electrolytic refining, the refined slag is returned to the environment-friendly furnace to be used as lump material, copper is enriched in the form of copper matte or black copper, and blowing, refining and electrolysis are carried out to obtain the finished product copper. The treatment method mainly adopts pyrometallurgical smelting, and needs a blast system, an oxygen production system, a dust removal system, a waste heat boiler, a desulfurization system and the like, and simultaneously needs to consume a large amount of coke and coal powder as smelting heat and reducing atmosphere. The method is characterized by long processing process flow, large processing capacity, large equipment investment, more matching flows, stable raw material requirement, high furnace starting and stopping cost, long maintenance time and the like.
For example, chinese patent publication No. CN110157913A discloses a method for comprehensively treating copper slag, which comprises the following steps:
A. ore grinding, proportioning and activating: after removing impurities from the copper slag, adding a leaching agent, an additive and water, wet-grinding to 200-400 meshes, and adjusting the liquid-solid ratio to obtain slurry; the wet grinding is that the raw materials are coarsely crushed by an overflow rod mill and then ground by an overflow ball mill to a proper particle size, a leaching agent is selected from electrolyte, copper-removed liquid, waste acid, contaminated acid or industrial sulfuric acid, an additive is a chlorine-containing substance or an oxidizing substance or a mixture of the chlorine-containing substance and the oxidizing substance, the chlorine-containing substance is one or more of hydrochloric acid, chlorine and chlorine salt, the oxidizing substance is sodium chlorate or hydrogen peroxide, and the additive can be added at any stage of ball milling or leaching;
B. leaching: pumping the slurry into a pressure kettle, and stirring and pressurizing for leaching under the conditions of proper temperature and oxygen partial pressure to obtain leached slurry;
C. concentrating and crystallizing copper sulfate and performing sulfuration replacement: the leached slurry is subjected to liquid-solid separation to obtain leachate and leached residues, the leachate is purified and then directly returned to an electrolysis system or is subjected to evaporation crystallization and filtration to obtain copper sulfate and crystallization mother liquor, the leached residues are sent to an antimony-bismuth recovery process, the crystallization mother liquor is subjected to sulfidization replacement to obtain copper sulfide residues and replacement mother liquor, and the copper sulfide residues are sent to a smelting and batching process;
D. reduction and purification of the replacement mother liquor: sending the replacement mother liquor to a reduction process to obtain arsenic trioxide and reduction mother liquor, sending the reduction mother liquor to a purification process to produce antimony-bismuth slag, and sending the antimony-bismuth slag to an antimony-bismuth recovery process; the purified liquid returns to a copper smelting electrolysis system or directly returns to the step A for slurrying.
The process adopts high-pressure acid leaching under oxygen pressure, concentrated crystallization converts copper into copper sulfate, then electrolytic copper is fed in for electrolysis, and other metals subjected to acid leaching are further separated, so that the whole process flow is long, and the metal separation is complex.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a wet treatment process for refined copper slag.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a wet treatment process of refined copper slag comprises the following steps:
step S1, coarsely crushing, finely crushing and ball-milling refined copper slag, wherein the granularity of the refined copper slag reaches-80 to-200 meshes;
step S2, leaching the ground refined copper slag and the mixed solution of ammonia water and ammonium sulfate at normal temperature and normal pressure, performing solid-liquid separation after leaching, and obtaining a copper ammonia complex solution and leached slag containing nickel, lead, iron and tin polymetallic after the solid-liquid separation;
step S3, extracting the copper ammonia complex solution and a copper extractant, concentrating copper in the extracted solution into the extractant, and performing back extraction on the extractant through electro-deposition copper-poor liquid or sulfuric acid to obtain a copper-rich solution;
step S4, the copper-rich solution enters an electrodeposition copper system for electrodeposition, and a cathode copper finished product is obtained by precipitation on the cathode; the raffinate after extraction is returned to be leached to be used as a leaching bottom liquid.
Further, the leaching process parameters in the step S2 are as follows: the concentration of ammonia water and ammonium sulfate is respectively controlled to be 6-8mol/L, the concentration of ammonia in the ammonium sulfate is 2-4mol/L, the leaching time is 6-8 hours, the reaction temperature is 30-40 ℃, the solid-to-solid ratio of leaching liquid is 8-10:1, and the pH value of the leaching end point is 7.5-8.5.
Further, in the step S3, the copper extractant is prepared by blending ZJ980 copper extractant with sulfonated space kerosene at a volume ratio of 1: 4.
Further, in step S3, the oil-water ratio during extraction is controlled to be: 2-4:1, adopting countercurrent combined reflux mixed extraction, wherein the stage number of an extraction section is 4, the flow of an extraction material liquid is adjusted by judging the color of a raffinate and combining assay data, the extracted organic is washed by tap water, the washing also adopts a countercurrent combined reflux mixed washing process, the washing stage number is 4, and the washing oil-water ratio is as follows: and the washed organic matter is back extracted by using electrodeposition barren liquor or 200g/l sulfuric acid to obtain 55-60g/l copper sulfate solution, and the oil-water ratio of the back extraction is as follows: 4-10:1.
Further, in the step S3, the copper-poor solution contains acid 170-185g/l, copper 30-35g/l, electrogenerated distance 100mm, and current density 80-120A/m2The circulation flow of the electric effusion is 25-50L/min; guar gum is added as an inhibitor in the electrodeposition process, and the dosage is 150-300 g/tCu.
Further, in the step S2, the copper leaching rate of the refined copper slag is greater than 96%, and the content ratio of copper to other metal ions in the leached liquid is greater than 500: 1.
Further, the ammonia water-ammonium sulfate mixed solution is used as a leaching agent for refining copper slag.
Further, the leached copper-containing leachate is subjected to copper extraction by using a hydroximic copper extractant capable of inhibiting ammonia extraction.
Further, the refined copper slag contains 30-50% of copper, 4-8% of lead, 4-8% of tin and 6-10% of nickel.
The invention has the beneficial effects that: the invention adopts the ammonia method for leaching, so that copper and other metals are well and directly separated during leaching, the process principle is simple, the energy consumption is low, the whole process is mechanically operated, the labor intensity of workers is low, the recovery rate of copper in the whole process is more than or equal to 95 percent, and the leached slag can return to the fuming furnace to continuously recover other metal elements in the leached slag.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
As shown in FIG. 1, a wet treatment process for refined copper slag comprises the following steps:
step S1, coarsely crushing, finely crushing and ball-milling refined copper slag, wherein the granularity of the refined copper slag reaches-80 to-200 meshes;
step S2, leaching the ground refined copper slag and the mixed solution of ammonia water and ammonium sulfate at normal temperature and normal pressure, performing solid-liquid separation after leaching, and obtaining a copper ammonia complex solution and leached slag containing nickel, lead, iron and tin polymetallic after the solid-liquid separation;
step S3, extracting the copper ammonia complex solution and a copper extractant, concentrating copper in the extracted solution into the extractant, and performing back extraction on the extractant through electro-deposition copper-poor liquid or sulfuric acid to obtain a copper-rich solution;
step S4, the copper-rich solution enters an electrodeposition copper system for electrodeposition, and a cathode copper finished product is obtained by precipitation on the cathode; the raffinate after extraction is returned to be leached to be used as a leaching bottom liquid.
The leaching process parameters in step S2 are as follows: the concentration of ammonia water and ammonium sulfate is respectively controlled to be 6-8mol/L, the concentration of ammonia in the ammonium sulfate is 2-4mol/L, the leaching time is 6-8 hours, the reaction temperature is 30-40 ℃, the solid-to-solid ratio of leaching liquid is 8-10:1, and the pH value of the leaching end point is 7.5-8.5.
In step S3, the copper extractant is prepared by mixing ZJ980 copper extractant with sulfonated space kerosene according to the volume ratio of 1: 4.
The oil-water ratio in the extraction is controlled as follows: 2-4:1, adopting countercurrent combined reflux mixed extraction, wherein the stage number of an extraction section is 4, the flow of an extraction material liquid is adjusted by judging the color of a raffinate and combining assay data, the extracted organic is washed by tap water, the washing also adopts a countercurrent combined reflux mixed washing process, the washing stage number is 4, and the washing oil-water ratio is as follows: and the washed organic matter is back extracted by using electrodeposition barren liquor or 200g/l sulfuric acid to obtain 55-60g/l copper sulfate solution, and the oil-water ratio of the back extraction is as follows: 4-10:1.
In step S3, the copper-poor solution contains acid of 170-185g/l, copper of 30-35g/l, electropolar distance of 100mm, and current density of 80-120A/m2The circulation flow of the electric effusion is 25-50L/min; guar gum is added as an inhibitor in the electrodeposition process, and the dosage is 150-300 g/tCu.
In step S2, the copper leaching rate of the refined copper slag is more than 96%, and the content ratio of copper to other metal ions in the leached liquid is more than 500: 1.
In the embodiment, the ammonia water-ammonium sulfate mixed liquor is used as a leaching agent for refining copper slag, and a copper-containing leaching solution after leaching is subjected to copper extraction by adopting a hydroximic copper extracting agent capable of inhibiting ammonia extraction; the refined copper slag contains 30-50% of copper, 4-8% of lead, 4-8% of tin and 6-10% of nickel.
The invention will now be illustrated with reference to specific examples, in which:
a typical refined copper slag chemical composition, unit: is based on
Element(s) | Cu | Ni | Pb | Fe | Sn | Zn | CaO | SiO2 |
Content (wt.) | 44.57 | 2.55 | 4.9 | 4.58 | 2.08 | 2.88 | 0.48 | 10.34 |
The processing technology is as follows:
1. coarsely crushing, finely crushing and ball-milling refined copper slag, and enabling the granularity of the refined copper slag to reach-80 to-200 meshes; 2. preparing a leaching agent, wherein the concentrations of ammonia water and ammonium sulfate are respectively controlled to be 8mol/L and 3 mol/L;
3. the leaching time is 8 hours, the solid-to-liquid ratio of the leaching solution is 10:1, and the pH value at the end of leaching is 8.0; the copper content of the leached liquid is 35g/l, and the copper leaching rate is more than 96 percent;
4. the oil-water ratio in the extraction is controlled as follows: 4:1, washing oil-water ratio: 15:1, oil-water ratio of back extraction: 4:1, wherein the copper content of the raffinate is 0.2g/l, and the copper content of the copper-rich liquid is 55 g/l;
5. and (3) an electrodeposition refining process: the current density is 100A/m2The circulating flow of the electric effusion is 35L/min; the dosage of the additive guar gum is 200 g/tCu.
The invention adopts the ammonia method for leaching, so that copper and other metals are well and directly separated during leaching, the process principle is simple, the energy consumption is low, the whole process is mechanically operated, the labor intensity of workers is low, the recovery rate of copper in the whole process is more than or equal to 95 percent, and the leached slag can return to the fuming furnace to continuously recover other metal elements in the leached slag.
The foregoing shows and describes the general principles of the present invention, its general features, and advantages. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents.
Claims (9)
1. The wet treatment process of the refined copper slag is characterized by comprising the following steps of:
step S1, coarsely crushing, finely crushing and ball-milling refined copper slag, wherein the granularity of the refined copper slag reaches-80 to-200 meshes;
step S2, leaching the ground refined copper slag and the mixed solution of ammonia water and ammonium sulfate at normal temperature and normal pressure, performing solid-liquid separation after leaching, and obtaining a copper ammonia complex solution and leached slag containing nickel, lead, iron and tin polymetallic after the solid-liquid separation;
step S3, extracting the copper ammonia complex solution and a copper extractant, concentrating copper in the extracted solution into the extractant, and performing back extraction on the extractant through electro-deposition copper-poor liquid or sulfuric acid to obtain a copper-rich solution;
step S4, the copper-rich solution enters an electrodeposition copper system for electrodeposition, and a cathode copper finished product is obtained by precipitation on the cathode; the raffinate after extraction is returned to be leached to be used as a leaching bottom liquid.
2. The refining copper slag wet processing process of claim 1, wherein the leaching process parameters in the step S2 are as follows: the concentration of ammonia water and ammonium sulfate is respectively controlled to be 6-8mol/L, the concentration of ammonia in the ammonium sulfate is 2-4mol/L, the leaching time is 6-8 hours, the reaction temperature is 30-40 ℃, the solid-to-solid ratio of leaching liquid is 8-10:1, and the pH value of the leaching end point is 7.5-8.5.
3. The refining copper slag wet processing technology as claimed in claim 1 or 2, wherein in the step S3, the copper extractant is prepared by adopting ZJ980 copper extractant and sulfonated space kerosene according to the volume ratio of 1: 4.
4. The wet processing process of refining copper slag according to claim 3, wherein in step S3, the oil-water ratio during extraction is controlled as follows: 2-4:1, adopting countercurrent combined reflux mixed extraction, wherein the stage number of an extraction section is 4, the flow of an extraction material liquid is adjusted by judging the color of a raffinate and combining assay data, the extracted organic is washed by tap water, the washing also adopts a countercurrent combined reflux mixed washing process, the washing stage number is 4, and the washing oil-water ratio is as follows: and the washed organic matter is back extracted by using electrodeposition barren liquor or 200g/l sulfuric acid to obtain 55-60g/l copper sulfate solution, and the oil-water ratio of the back extraction is as follows: 4-10:1.
5. The wet processing process of refining copper slag as claimed in claim 3, wherein in step S3, the copper-poor solution contains acid 170-185g/l, copper 30-35g/l, electrogenerated distance is 100mm, and current density is 80-120A/m2The circulation flow of the electric effusion is 25-50L/min; guar gum is added as an inhibitor in the electrodeposition process, and the dosage is 150-300 g/tCu.
6. The refining copper slag wet processing technology as claimed in claim 1, wherein in the step S2, the copper leaching rate of the refining copper slag is more than 96%, and the content ratio of copper to other metal ions in the leached liquid is more than 500: 1.
7. The wet processing technology of refined copper slag according to claim 1, wherein the ammonia-ammonium sulfate mixed liquor is used as a leaching agent of refined copper slag.
8. A refining copper slag wet processing technology according to claim 1, characterized in that the leached copper-containing leachate is subjected to copper extraction by using a hydroximic copper extractant which can inhibit ammonia extraction.
9. The wet processing technology of refined copper slag according to claim 1, characterized in that the refined copper slag contains 30-50% of copper, 4-8% of lead, 4-8% of tin and 6-10% of nickel.
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Publication number | Priority date | Publication date | Assignee | Title |
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CN114892004A (en) * | 2022-04-19 | 2022-08-12 | 浙江特力再生资源股份有限公司 | Comprehensive recycling process of copper-containing silicon slag |
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