CN114561548A - Method for removing and recovering lead in high-lead copper anode slime - Google Patents
Method for removing and recovering lead in high-lead copper anode slime Download PDFInfo
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- CN114561548A CN114561548A CN202210200717.5A CN202210200717A CN114561548A CN 114561548 A CN114561548 A CN 114561548A CN 202210200717 A CN202210200717 A CN 202210200717A CN 114561548 A CN114561548 A CN 114561548A
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- Prior art keywords
- lead
- copper anode
- anode slime
- edta disodium
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 25
- 239000010949 copper Substances 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 20
- LXAHHHIGZXPRKQ-UHFFFAOYSA-N 5-fluoro-2-methylpyridine Chemical compound CC1=CC=C(F)C=N1 LXAHHHIGZXPRKQ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000706 filtrate Substances 0.000 claims abstract description 15
- 238000003825 pressing Methods 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 239000002893 slag Substances 0.000 claims abstract description 12
- 229940056932 lead sulfide Drugs 0.000 claims abstract description 11
- 229910052981 lead sulfide Inorganic materials 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000004073 vulcanization Methods 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 6
- 239000002244 precipitate Substances 0.000 claims abstract description 6
- 230000001376 precipitating effect Effects 0.000 claims abstract description 6
- 229910052979 sodium sulfide Inorganic materials 0.000 claims abstract description 6
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 4
- 239000000956 alloy Substances 0.000 claims abstract description 4
- 229910001316 Ag alloy Inorganic materials 0.000 claims abstract description 3
- PQTCMBYFWMFIGM-UHFFFAOYSA-N gold silver Chemical compound [Ag].[Au] PQTCMBYFWMFIGM-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 3
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 3
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 3
- 230000001698 pyrogenic effect Effects 0.000 claims 1
- 238000004064 recycling Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 abstract 1
- 238000001914 filtration Methods 0.000 description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 5
- 229910052709 silver Inorganic materials 0.000 description 5
- 239000004332 silver Substances 0.000 description 5
- 230000035515 penetration Effects 0.000 description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
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Classifications
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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
-
- 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
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
- C22B13/045—Recovery from waste materials
-
- 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
-
- 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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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides a method for removing and recovering lead in high-lead copper anode slime, which comprises the steps of EDTA disodium deleading-sulfurizing treatment, specifically mixing copper anode slime pressurized slag and EDTA disodium solution according to a solid-to-liquid ratio of 1: 3-4, heating to 80-90 ℃, keeping the temperature for 2-3 hours, and then performing filter pressing, wherein the obtained filter residue is attached to an alloy furnace to produce a gold-silver alloy anode plate; and adding sodium sulfide into the obtained filtrate until no black precipitate exists in the system, completely precipitating lead, heating to 80-90 ℃, reacting for 2-3 hours, condensing and growing solid particles, and performing filter pressing to obtain lead sulfide filter residues. The method can effectively remove lead impurities in the high-lead copper anode slime, the EDTA disodium can be regenerated and recycled by adopting the vulcanization treatment of the liquid after the lead removal, the reagent cost is reduced, and the lead sulfide product with the lead grade of more than 80% is produced, so that the influence of the high lead content in the copper anode slime on the subsequent production is solved, the treatment capacity and the single-furnace discharge capacity of the alloy furnace are improved, and the wet open of lead is realized.
Description
Technical Field
The invention belongs to the technical field of metallurgy, relates to a method for treating copper anode slime, and particularly relates to a method for removing and recovering lead in high-lead copper anode slime.
Background
In the rare and precious metal metallurgical industry, a pressure leaching process is often adopted to remove copper, nickel and tellurium in copper anode slime, but as the components of the copper anode slime are more and more complex, particularly the content of lead is more and more high, the content of lead is increased from the original 20% to about 30%, and the content of lead in pressure slag after pressure leaching even exceeds 37%, great difficulty is caused for the production of a silver anode plate by post-fire smelting, not only is the blowing time increased and a large amount of energy is consumed, but also the consumption of slagging reagents is increased, the production cost is increased, a large amount of lead-containing dust brings negative effects to an environment-friendly dust collecting system, the environment-friendly index fluctuation is caused, and the surrounding environment is influenced.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for removing and recovering lead in high-lead copper anode slime.
The invention relates to a method for removing and recovering lead in high-lead copper anode slime, which comprises the following steps:
(1) removing lead from disodium EDTA: mixing the copper anode mud pressurized slag and an EDTA disodium solution according to a solid-to-liquid ratio of 1: 3-4, heating to 80-90 ℃, keeping the temperature for 2-3 hours, then performing filter pressing, performing cross vulcanization treatment on filtrate, and feeding the obtained filter residue into an alloying furnace to produce a gold-silver alloy anode plate;
(2) and (3) vulcanization treatment: adding sufficient industrial sodium sulfide into the filtrate obtained in the step (1) until a system does not have black precipitate, completely precipitating lead, heating to 80-90 ℃ for reaction for 2-3 hours, condensing and growing solid particles, avoiding penetration filtration and filter pressing, wherein the main component of the filtrate is EDTA disodium, the EDTA disodium can be recycled to the lead removal process, the production cost is reduced, and the main component of the filter residue is lead sulfide and can be sold for external use.
The method adopts EDTA disodium as a deleading reagent to be applied to the field of copper anode slime pretreatment, can effectively remove lead impurities in the high-lead copper anode slime, and produces lead sulfide with lead grade of more than 80% by adopting vulcanization treatment on the liquid after the deleading, thereby not only solving the influence of high lead content in the copper anode slime on subsequent production, improving the treatment capacity and single-furnace discharge amount of an alloy furnace, but also realizing wet treatment of lead and effectively reducing the production cost of a system.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
The same batch of raw material copper anode slime pressurized slag contains 9.25% of silver and 35% of lead.
Example 1
(1) Adding copper anode slime pressurized slag (pressurized decoppering material) and a disodium EDTA solution with the concentration of 150g/L into a reaction tank according to the solid-to-liquid ratio of 1:3, heating to 85 ℃, keeping the temperature for 3 hours, and then performing filter pressing, wherein the slag rate of filter residue is 70%, the grade of gold and silver is improved from 9.25% to 13.5%, and the content of lead is reduced to 15%. The lead content in the filtrate was 80g/L, and the lead removal rate was about 72%.
(2) Adding enough industrial sodium sulfide into the filtrate obtained in the step (1) until no black precipitate exists in the system, completely precipitating lead, heating to 80 ℃ for reaction for 2-3 hours, condensing and growing solid particles, avoiding penetration filtration and filter pressing, wherein the main component of the filtrate is EDTA disodium and can be recycled to the deleading process, the production cost is reduced, and the main component of the filter residue is lead sulfide and can be sold for the outside. The content of lead sulfide recovered after the vulcanization treatment is 82%.
Example 2
(1) Adding copper anode slime pressurized slag (pressurized decoppering material) and 130g/L EDTA disodium solution into a reaction tank according to the solid-to-liquid ratio of 1:4, heating to 90 ℃, keeping the temperature for 2 hours, and then performing filter pressing, wherein the slag filtration rate is 67%, the grade of gold and silver is improved from 9.25% to 14.01%, and the content of lead is reduced to 12%. The lead content in the filtrate was 65g/L, and the lead removal rate was about 77%.
(2) Adding enough industrial sodium sulfide into the filtrate obtained in the step (1) until no black precipitate exists in the system, completely precipitating lead, heating to 90 ℃ for reaction for 2-3 hours, condensing and growing solid particles, avoiding penetration filtration and filter pressing, wherein the main component of the filtrate is EDTA disodium and can be recycled to the lead removal process, the production cost is reduced, and the main component of the filter residue is lead sulfide and can be sold for the outside. The content of lead sulfide recovered after the vulcanization treatment is 85%.
Example 3
(1) Adding copper anode slime pressurized slag (pressurized decoppering material) and EDTA disodium solution with the concentration of 100g/L into a reaction tank according to the solid-to-liquid ratio of 1:4, heating to 80 ℃, keeping the temperature for 2 hours, and then performing filter pressing, wherein the slag filtration rate is 76%, the grade of gold and silver is improved from 9.25% to 12.96%, and the lead content is reduced to 17%. The lead content in the filtrate was 60g/L, and the lead removal rate was about 64%.
(2) Adding enough industrial sodium sulfide into the filtrate obtained in the step (1) until no black precipitate exists in the system, completely precipitating lead, heating to 90 ℃ for reaction for 2-3 hours, condensing and growing solid particles, avoiding penetration filtration and filter pressing, wherein the main component of the filtrate is EDTA disodium and can be recycled to the lead removal process, the production cost is reduced, and the main component of the filter residue is lead sulfide and can be sold for the outside. The content of lead sulfide recovered after the vulcanization treatment is 80%.
Claims (3)
1. A method for removing and recovering lead in high-lead copper anode slime comprises the following steps:
(1) removing lead from disodium EDTA: mixing the copper anode mud pressurized slag and an EDTA disodium solution according to a solid-to-liquid ratio of 1: 3-4, heating to 80-90 ℃, keeping the temperature for 2-3 hours, and then performing filter pressing, wherein the obtained filter slag is treated by an alloy furnace pyrogenic process to produce a gold-silver alloy anode plate;
(2) and (3) vulcanization treatment: and (2) adding sodium sulfide into the filtrate obtained in the step (1) until no black precipitate exists in the system, completely precipitating lead, heating to 80-90 ℃, reacting for 2-3 hours, condensing and growing solid particles, and performing filter pressing to obtain lead sulfide filter residue.
2. The method for removing and recovering lead in the high-lead copper anode slime according to claim 1, which is characterized by comprising the following steps of: in the step (1), the concentration of the EDTA disodium solution is 100-150 g/L.
3. The method for removing and recovering lead in the high-lead copper anode slime according to claim 1, which is characterized by comprising the following steps of: and (3) in the step (2), recycling the EDTA disodium filtrate subjected to filter pressing to the deleading procedure in the step (1).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210200717.5A CN114561548A (en) | 2022-03-02 | 2022-03-02 | Method for removing and recovering lead in high-lead copper anode slime |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210200717.5A CN114561548A (en) | 2022-03-02 | 2022-03-02 | Method for removing and recovering lead in high-lead copper anode slime |
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| Publication Number | Publication Date |
|---|---|
| CN114561548A true CN114561548A (en) | 2022-05-31 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210200717.5A Pending CN114561548A (en) | 2022-03-02 | 2022-03-02 | Method for removing and recovering lead in high-lead copper anode slime |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4704260A (en) * | 1983-12-20 | 1987-11-03 | Union Oil Company Of California | Lead removal method |
| JPH04263874A (en) * | 1991-02-18 | 1992-09-18 | Jgc Corp | Method for cleaning soil contaminated with heavy metal |
| CN101451198A (en) * | 2007-11-29 | 2009-06-10 | 黄石理工学院 | Method for recovering zinc and lead from waste electrolysis anode sludge |
| CN104561577A (en) * | 2014-12-07 | 2015-04-29 | 金川集团股份有限公司 | Method for removing lead from lead-containing precious metal materials |
| CN107142378A (en) * | 2017-05-31 | 2017-09-08 | 攀枝花火凤凰再生资源回收利用有限责任公司 | The extracting method of lead in a kind of sintering flue dust |
-
2022
- 2022-03-02 CN CN202210200717.5A patent/CN114561548A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4704260A (en) * | 1983-12-20 | 1987-11-03 | Union Oil Company Of California | Lead removal method |
| JPH04263874A (en) * | 1991-02-18 | 1992-09-18 | Jgc Corp | Method for cleaning soil contaminated with heavy metal |
| CN101451198A (en) * | 2007-11-29 | 2009-06-10 | 黄石理工学院 | Method for recovering zinc and lead from waste electrolysis anode sludge |
| CN104561577A (en) * | 2014-12-07 | 2015-04-29 | 金川集团股份有限公司 | Method for removing lead from lead-containing precious metal materials |
| CN107142378A (en) * | 2017-05-31 | 2017-09-08 | 攀枝花火凤凰再生资源回收利用有限责任公司 | The extracting method of lead in a kind of sintering flue dust |
Non-Patent Citations (1)
| Title |
|---|
| 张传宝等: "难处理铅锌矿酸浸渣回收硫酸铅的工艺研究", 应用化工, no. 07, pages 1188 - 1192 * |
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| TA01 | Transfer of patent application right |
Effective date of registration: 20240508 Address after: 737199 No. 2 Jianshe Road, Jinchuan District, Jinchang City, Gansu Province (east of Beijing Road, west of Heya Road, south of Guiyang Road) Applicant after: Jinchuan Group Copper Gui Co.,Ltd. Country or region after: China Address before: No.98, Jinchuan Road, Jinchuan District, Jinchang City, Gansu Province 737100 Applicant before: JINCHUAN GROUP Co.,Ltd. Country or region before: China |
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