CN102732729B - Method for removing nickel and copper from high nickel copper anode mud - Google Patents
Method for removing nickel and copper from high nickel copper anode mud Download PDFInfo
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- CN102732729B CN102732729B CN201210214571.6A CN201210214571A CN102732729B CN 102732729 B CN102732729 B CN 102732729B CN 201210214571 A CN201210214571 A CN 201210214571A CN 102732729 B CN102732729 B CN 102732729B
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- copper
- nickel
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- selenium
- anode mud
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 239000010949 copper Substances 0.000 title claims abstract description 58
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 57
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 30
- YOCUPQPZWBBYIX-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Cu] YOCUPQPZWBBYIX-UHFFFAOYSA-N 0.000 title claims abstract description 27
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 23
- 239000011669 selenium Substances 0.000 claims abstract description 23
- 238000002386 leaching Methods 0.000 claims abstract description 16
- 230000003647 oxidation Effects 0.000 claims abstract description 9
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 9
- 239000010970 precious metal Substances 0.000 claims description 30
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 13
- 239000000706 filtrate Substances 0.000 claims description 12
- 235000011149 sulphuric acid Nutrition 0.000 claims description 8
- 239000001117 sulphuric acid Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 239000000284 extract Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 230000001698 pyrogenic effect Effects 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000010907 mechanical stirring Methods 0.000 claims description 3
- 238000000605 extraction Methods 0.000 abstract description 2
- 229910000510 noble metal Inorganic materials 0.000 abstract 3
- 238000009853 pyrometallurgy Methods 0.000 abstract 1
- 239000000956 alloy Substances 0.000 description 7
- 229910045601 alloy Inorganic materials 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- KRRRBSZQCHDZMP-UHFFFAOYSA-N selanylidenesilver Chemical compound [Ag]=[Se] KRRRBSZQCHDZMP-UHFFFAOYSA-N 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 238000005987 sulfurization reaction Methods 0.000 description 2
- MTJGVAJYTOXFJH-UHFFFAOYSA-N 3-aminonaphthalene-1,5-disulfonic acid Chemical compound C1=CC=C(S(O)(=O)=O)C2=CC(N)=CC(S(O)(=O)=O)=C21 MTJGVAJYTOXFJH-UHFFFAOYSA-N 0.000 description 1
- 241000784732 Lycaena phlaeas Species 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011499 joint compound Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
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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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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a method for removing nickel and copper from high nickel copper anode mud. According to the method, a pressurizing leaching method is adopted to firstly remove nickel from high nickel copper anode mud, then an oxidation leaching method is adopted to remove copper, the nickel and the cooper are recovered from the leached solutions, and noble metals and selenium are extracted from the leached residues. According to the present invention, the nickel content and the nickel content in the leached residues are less than 1%, and the noble metals and the selenium are enriched, such that convenient conditions are provided for extractions of noble metals and selenium through subsequent wet processing or pyrometallurgy processing, wherein the high nickel copper anode mud is subjected to nickel removing and cooper removing to obtain the leached residues.
Description
Technical field
A method that removes nickel and copper in high content of nickel copper anode mud, relates to pressure leaching nickel and copper, extracts the technological process of precious metal.
Background technology
In order to extract the rare precious metals such as gold and silver selenium from copper anode mud, need first the base metals such as separated nickel wherein, copper, be the needs of comprehensive utilization like this, the extraction for rare precious metals such as gold and silver selenium creates conditions again.At present, the method that industrial production is taked has sulfurization roasting and pressure oxidation to leach.Sulfurization roasting is serious because of its equipment corrosion, and operating environment is poor to be eliminated gradually, and pressure leaching both economical, efficiently environmental protection has become a kind of developing direction.But the method for pressure leaching and condition are not suitable for the processing of high ambrose alloy copper anode mud.On the one hand, the oxide compound of copper and mickel has different solubleness in sulphuric acid soln, and the oxide compound of copper is well in vitriolization, and the dissolving that the oxide compound of nickel can only trace.The solubleness of copper and mickel in sulfuric acid on the other hand, according to melting (roasting) temperature and solution temperature and concentration and determine, when maturing temperature is higher than 600 ℃, solution temperature is less than 50 ℃, and sulfuric acid concentration is while being less than 10%, and the amount that NiO is dissolved in solution is less than 3%, improve maturing temperature and reduce solution temperature, will make the solubleness of NiO in sulphuric acid soln greatly reduce, when maturing temperature is higher than 1000 ℃, the nickel amount in solution of entering is no better than zero.When maturing temperature is during higher than 600 ℃, the oxide compound of nickel and copper will generate sosoloid (3NiO.Cu), and the copper that is combined to sosoloid with nickel all becomes insoluble.
High content of nickel copper anode mud is the intermediate material producing in electrolytic refining course of copper, is the raw material that extracts precious metal, wherein contains a large amount of nickel, copper.Because copper anode plate has passed through high melt, the oxide compound of generating nickel, ambrose alloy sosoloid are inevitably, so the treatment process of high content of nickel copper anode mud and common copper anode mud makes a big difference.Test shows, common pressure oxidation leaching method, and in its leached mud, nickel and copper content are all higher, are unfavorable for subsequent extracted precious metal and selenium, and the comprehensive utilization of ambrose alloy is had a certain impact.
Summary of the invention
The object of the invention is in order to extract the rare precious metal in high content of nickel copper anode mud, and make ambrose alloy be convenient to recycle simultaneously, and set up a kind of both effectively, the treatment process that removes nickel and copper of economy and environmental protection.
The object of the invention is to be achieved through the following technical solutions:
A method that removes nickel and copper in high content of nickel copper anode mud, preferentially removes the nickel in described high content of nickel copper anode mud in pressure leaching mode, then with Oxidation Leaching method, removes copper; From leach liquor, reclaim nickel and copper, from leached mud, extract precious metal and selenium; Its detailed process is:
A. described high content of nickel copper anode mud is placed in an autoclave with mechanical stirring and heating unit, by liquid-solid mass ratio 4-6; 1 adds sulphuric acid soln, and this sulphuric acid soln concentration 90～240g/L, at 160～200 ℃, under agitation condition, reacts 1～5h;
B. liquid-solid separation: after the reaction in described a, the nickel in described high content of nickel copper anode mud more than 99% and a small amount of copper enter solution, and most copper and all precious metals, selenium stay in leached mud, realizes the separated of nickel and copper, precious metal and selenium; Obtain filtrate 1 and leached mud 1; Nickel in described filtrate 1 and a small amount of copper are reclaimed;
C, described leached mud 1 copper anode mud treatment process routinely, in dilution heat of sulfuric acid, carries out Oxidation Leaching;
D, after the reaction in described c, copper in described high content of nickel copper anode mud more than 99% enters solution, overwhelming majority precious metal and selenium stay in leached mud, this leached mud is the raw material that precious metal is extracted in follow-up wet method or pyrogenic attack, thus, realize the separated of copper and precious metal and selenium, obtain filtrate 2 and leached mud 2; Copper in described filtrate 2 is reclaimed.
The mud of high content of nickel copper anode described in the present invention removes in the leached mud after nickel and copper, and nickeliferous and copper is all less than 1%, and precious metal and selenium obtain enrichment, for precious metal and the selenium condition of providing convenience is extracted in follow-up wet method or pyrogenic attack.
Accompanying drawing explanation
Fig. 1 is schema of the present invention.
Embodiment
With reference to Fig. 1, a kind of method that removes nickel and copper in high content of nickel copper anode mud,, in pressure leaching mode, preferentially remove the nickel in described high content of nickel copper anode mud, then with Oxidation Leaching method, remove copper; From leach liquor, reclaim nickel and copper, from leached mud, extract precious metal and selenium; Its detailed process is:
A. described high content of nickel copper anode mud is placed in an autoclave with mechanical stirring and heating unit, by liquid-solid mass ratio 4:1,5:1 or 6:1, add sulphuric acid soln, this sulphuric acid soln concentration 90,100,150,200 or 240g/L, at 160,170,180,190 or 200 ℃, under agitation condition, react 1,2,3,4 or 5h;
B. liquid-solid separation: after the reaction in described a, the nickel in described high content of nickel copper anode mud more than 99% and a small amount of copper enter solution, and most copper and all precious metals, selenium stay in leached mud, realizes the separated of nickel and copper, precious metal and selenium; Obtain filtrate 1 and leached mud 1; Nickel in described filtrate 1 and a small amount of copper are reclaimed;
C, described leached mud 1 copper anode mud treatment process routinely, in dilution heat of sulfuric acid, carries out Oxidation Leaching;
D, after the reaction in described c, copper in described high content of nickel copper anode mud more than 99% enters solution, overwhelming majority precious metal and selenium stay in leached mud, this leached mud is the raw material that precious metal is extracted in follow-up wet method or pyrogenic attack, thus, realize the separated of copper and precious metal and selenium, obtain filtrate 2 and leached mud 2; Copper in described filtrate 2 is reclaimed, and wherein a small amount of selenium takes the method for displacement to be reclaimed.In described leached mud 2, nickeliferous and copper is all less than 1%, and precious metal and selenium obtain enrichment; Concrete production data is as follows:
The chemical composition of described high content of nickel copper anode mud is as table 1.
Table 1 high content of nickel copper anode mud chemical composition, %
Above-mentioned four batches of test raw materials are respectively after acidleach nickel removal, oxygen soak decopper(ing) leaching, and leached mud, leach liquor chemical composition are respectively as Table 2,3.Obtained nickelic low copper and the low nickel solution of high-copper, in leached mud, ambrose alloy content is all less than 1%, slag rate 21%, and precious metal stays in slag, has realized the separation of ambrose alloy and the enrichment of precious metal, for extracting precious metal and recovery ambrose alloy etc., has created condition.
Table 2 leached mud chemical composition
Table 3 leach liquor chemical composition
Claims (1)
1. a method that removes nickel and copper in high content of nickel copper anode mud, is characterized in that: in pressure leaching mode, preferentially remove the nickel in described high content of nickel copper anode mud, then with Oxidation Leaching method, remove copper; From leach liquor, reclaim nickel and copper, from leached mud, extract precious metal and selenium; Its detailed process is:
A. described high content of nickel copper anode mud is placed in an autoclave with mechanical stirring and heating unit, by liquid-solid mass ratio 4-6; 1 adds sulphuric acid soln, and this sulphuric acid soln concentration 90～240g/L, at 160～200 ℃, under agitation condition, reacts 1～5h;
B. liquid-solid separation: after the reaction in described a, the nickel in described high content of nickel copper anode mud more than 99% and a small amount of copper enter solution, and most copper and all precious metals, selenium stay in leached mud, realizes the separated of nickel and copper, precious metal and selenium; Obtain filtrate 1 and leached mud 1; Nickel in described filtrate 1 and a small amount of copper are reclaimed;
C, described leached mud 1 copper anode mud treatment process routinely, in dilution heat of sulfuric acid, carries out Oxidation Leaching;
D, after the reaction in described c, copper in described high content of nickel copper anode mud more than 99% enters solution, overwhelming majority precious metal and selenium stay in leached mud, this leached mud is the raw material that precious metal is extracted in follow-up wet method or pyrogenic attack, thus, realize the separated of copper and precious metal and selenium, obtain filtrate 2 and leached mud 2; Copper in described filtrate 2 is reclaimed.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210214571.6A CN102732729B (en) | 2012-06-27 | 2012-06-27 | Method for removing nickel and copper from high nickel copper anode mud |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210214571.6A CN102732729B (en) | 2012-06-27 | 2012-06-27 | Method for removing nickel and copper from high nickel copper anode mud |
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| CN102732729A CN102732729A (en) | 2012-10-17 |
| CN102732729B true CN102732729B (en) | 2014-01-15 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102965501B (en) * | 2012-12-21 | 2014-10-15 | 江西铜业股份有限公司 | Method for processing copper anode slime in total wet manner |
| CN104263958B (en) * | 2014-08-30 | 2016-04-20 | 广东省工业技术研究院(广州有色金属研究院) | A kind of method being separated Cu, Ni and Co and platinum family element from platinum family concentrate |
| CN104495761B (en) * | 2014-12-07 | 2016-06-29 | 金川集团股份有限公司 | A kind of method preparing telluride copper from high content of nickel copper anode mud |
| CN109055762B (en) * | 2018-09-29 | 2020-06-30 | 阳谷祥光铜业有限公司 | Copper removal treatment method for copper-selenium-containing waste |
| CN112095016B (en) * | 2020-08-27 | 2022-06-10 | 矿冶科技集团有限公司 | Method for reducing nickel content of high nickel matte leaching residues through hot pressing treatment |
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| CN1301338C (en) * | 2005-09-20 | 2007-02-21 | 云南冶金集团总公司 | Novel copper recovery method by copper anode mud pressurization and pickling |
| CN1821060A (en) * | 2006-03-14 | 2006-08-23 | 云南冶金集团总公司 | Method for leaching tellurium from copper anode mud using pressurized acid leaching process |
| CN101209853B (en) * | 2007-12-25 | 2010-07-21 | 金川集团有限公司 | Method for preparing cupric sulfate from spongy copper and copper-containing acid pickle |
| CN101434385B (en) * | 2008-12-08 | 2010-12-22 | 阳谷祥光铜业有限公司 | Process for extracting tellurium from copper anode mud |
| CN101838088B (en) * | 2010-01-28 | 2012-04-18 | 中国恩菲工程技术有限公司 | Anode mud treatment method of preparing metallic nickel by copper sulphide |
| CN101775498B (en) * | 2010-02-08 | 2011-07-13 | 中南大学 | Pretreatment method of copper anode mud |
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Effective date of registration: 20240301 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) Patentee after: Jinchuan Group Copper Gui Co.,Ltd. Country or region after: China Address before: 737103 No. 98, Jinchuan Road, Jinchang, Gansu Patentee before: Jinchuan Group Co.,Ltd. Country or region before: China |