CN101186972A - Leaching treatment technique for cobalt-containing rare alloy - Google Patents
Leaching treatment technique for cobalt-containing rare alloy Download PDFInfo
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- CN101186972A CN101186972A CNA2007101925512A CN200710192551A CN101186972A CN 101186972 A CN101186972 A CN 101186972A CN A2007101925512 A CNA2007101925512 A CN A2007101925512A CN 200710192551 A CN200710192551 A CN 200710192551A CN 101186972 A CN101186972 A CN 101186972A
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- 239000000956 alloy Substances 0.000 title claims abstract description 46
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 45
- 238000002386 leaching Methods 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000010941 cobalt Substances 0.000 title claims abstract description 34
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 34
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000010949 copper Substances 0.000 claims abstract description 33
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052802 copper Inorganic materials 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims description 15
- 229910000831 Steel Inorganic materials 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 239000010959 steel Substances 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 7
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 7
- 239000011707 mineral Substances 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 239000002002 slurry Substances 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 230000002411 adverse Effects 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 239000002893 slag Substances 0.000 claims description 5
- 235000011149 sulphuric acid Nutrition 0.000 claims description 5
- 239000001117 sulphuric acid Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 239000000284 extract Substances 0.000 claims description 4
- 238000007654 immersion Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 abstract description 26
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 10
- 239000002184 metal Substances 0.000 abstract description 7
- 229910052751 metal Inorganic materials 0.000 abstract description 7
- 229910052742 iron Inorganic materials 0.000 abstract description 4
- 238000002844 melting Methods 0.000 abstract description 4
- 230000008018 melting Effects 0.000 abstract description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 abstract description 3
- 238000003723 Smelting Methods 0.000 abstract description 2
- 235000013312 flour Nutrition 0.000 abstract 4
- 238000003801 milling Methods 0.000 abstract 4
- 238000005507 spraying Methods 0.000 abstract 2
- 230000003247 decreasing effect Effects 0.000 abstract 1
- 238000010304 firing Methods 0.000 abstract 1
- 238000010409 ironing Methods 0.000 abstract 1
- 150000007522 mineralic acids Chemical class 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 13
- 239000000243 solution Substances 0.000 description 12
- 229910000905 alloy phase Inorganic materials 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 238000000605 extraction Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 229910019001 CoSi Inorganic materials 0.000 description 2
- 229910017061 Fe Co Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- RIVZIMVWRDTIOQ-UHFFFAOYSA-N cobalt iron Chemical compound [Fe].[Co].[Co].[Co] RIVZIMVWRDTIOQ-UHFFFAOYSA-N 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical class [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 1
- -1 Co 2Si Inorganic materials 0.000 description 1
- 229910020711 Co—Si Inorganic materials 0.000 description 1
- 229910017758 Cu-Si Inorganic materials 0.000 description 1
- 229910017827 Cu—Fe Inorganic materials 0.000 description 1
- 229910017931 Cu—Si Inorganic materials 0.000 description 1
- 229910017082 Fe-Si Inorganic materials 0.000 description 1
- 229910017133 Fe—Si Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 229940069428 antacid Drugs 0.000 description 1
- 239000003159 antacid agent Substances 0.000 description 1
- 230000001458 anti-acid effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000002447 crystallographic data Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 238000009689 gas atomisation Methods 0.000 description 1
- 239000003978 infusion fluid Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004540 process dynamic Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001698 pyrogenic effect Effects 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 238000009692 water atomization 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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Abstract
The invention discloses a leaching treatment process of cobalt rare alloy, belonging to the technical field of wet-firing methods combined smelting of non-ferrous metal. After being melted, the cobalt rare alloy is impacted by high-pressure water, then atomized and cooled down, turning into the shape of flour, and is leached out by employing inorganic acid. Compared with the milling and leaching process of the existing rare alloy, the invention simplifies the technical process, changes flour milling of two-stage mechanical crushing into flour-manufacture of melting and spraying, and three-stage countercurrent or multi-mersion into the leaching of two-stage countercurrent. Compared with devices with same investment, the production efficiency is largely increased, the flour milling amount with the use of flour milling process of melting and spraying is increased by more than two times, and the leaching time is shortened by one third. The leaching ratio of cobalt and copper is more than 99% and is increased by more than three percentage points. The leaching ratio of iron is less than 60% and is decreased by one third, thereby reducing one third of the subsequent de-ironing costs.
Description
Technical field
The present invention is a kind of leaching treatment technique of cobalt-containing rare alloy, belongs to the pyrogenic process of non-ferrous metal---wet method combined technical field of smelting.
Background technology
The said rare alloy of the present invention is a kind of alloy that mainly contains cobalt, copper, iron and element silicon.Various constituent content scopes in this kind alloy are roughly (%): Co5-60; Cu10-60; Fe20-60; Si5-15, it is a kind of oxidized ore by Africa, after the high temperature reduction melting, forming granularity with shrend is the irregular particle of 1-30 millimeter.Warp is (%): Co34.39 to composition; Cu13.08; Fe28.50; The material phase analysis of Si7.54, there are three kinds of basic thing phases in this kind alloy: two kinds of alloys are not arranged again in the alloy phase of alloyed metal (AM) copper, alloying.
This alloy X-ray diffraction spectrogram is seen Fig. 1.As seen from Figure 1, diffract spectral line is few, simple, and the strongest diffracted ray of 1.9876 dusts is key characters of ferrous alloy diffraction pattern, because the Si-Fe-Co alloy diffraction data of no standard can be for contrasting spectral line and Cu-Fe alloy (Fe
4Cu
3), Co-Si alloy (CoSi, Co
2Si, CoSi
2, Co
2Si
3) and Cu-Si alloy (Cu
5Si, Cu
4Si) etc. all be not quite similar, only and Fe
3Si is approaching, so can only be designated the Fe-Si alloy.In addition, also there is a certain amount of metallic copper phase in the raw material.Confirm that through microscopical analysis this part copper mostly is the finely-divided metal copper in the alloy phase into of being wrapped.
The feature of each thing phase is seen Fig. 2 and Fig. 3 in the powder.A is the alloy phase aggregate enlarged view of white among Fig. 2, and still there are two kinds of alloy phases and finely-divided metal copper in this aggregate inside, and Cu represents metallic copper.
Further by microscopical analysis, as seen from Figure 3, alloy phase A mostly is metallic copper and wraps up.
In sum, this alloy raw material is actually the quite complicated multicomponent alloy of a kind of composition, and this alloy that mainly contains Si-Fe-Co itself is exactly antacid probably.
Because cobalt is big land very rare China, and its range of application is very extensive, therefore, this kind alloy becomes a kind of important source material of refining cobalt.This kind alloy does not have direct applied value, has only wherein cobalt and copper refinement are separated, and could embody its using value.
At present, the domestic technology that has two kinds with this kind alloy separation and Extraction cobalt and copper.
A kind of is that this kind alloy directly is soaked in the certain density mineral acid, and soak solution is extracted in tens of hours (72 hours or longer) back, and the mineral acid that reinjects soaks after tens of hours and extracts soak solution, so repeatedly carries out repeatedly, is no longer only leached until cobalt and copper.Repeatedly the soak solution of Chou Quing send follow-up extraction to extract cobalt and copper.Though this technology is simple, have following shortcoming in production practice: (1) production efficiency is low, and the production cycle is long, often needs to finish in more than ten day a leaching process; (2) soak solution acidity is too high, makes the extraction of subsequent process increase difficulty and production cost; (3) cobalt and copper leaching rate are not high, and the leaching yield of a leaching process is less than 90%, and leached mud needs to handle to reclaim again.(4) to take the production capital amount big for the leaching process raw material, because raw material accounts for 75% of total cost of production.
Another kind is this kind alloy to be broken with multistage machinery be milled to finely powdered, reinject back one section leach liquor and mineral acid leaches in steel basin, after a few hours, isolate leach liquor, reinject second section leach liquor and mineral acid of leached mud leaches in steel basin, after a few hours, isolate leach liquor, leached mud reinjects and mixes mineral acid and leach in steel basin, after a few hours, isolate leach liquor, so leach through three sections adverse currents, leached mud can reach discarded requirement, leaching yield reaches 96%, three section leach liquor and send follow-up extraction to extract cobalt and copper.Compare with preceding kind of technology, leaching process production efficiency improves greatly; Leach liquor acidity is controlled; Leaching yield improves greatly, and leached mud can be discarded; The production capital turnover is accelerated.But also there are two shortcomings: the one, the broken mill of machinery process efficiency is low.Because this kind alloy ingredient variation range is big, has very big toughness and ductility, crushing mechanism is difficult to its broken finely powdered that is milled to.The 2nd, leaching process is still longer.
Chinese invention patent 200610032051.8 has proposed " a kind of method that leaches the copper ferro-cobalt from copper ferrocobalt alloy ", and this technology will be mixed the powdered alloy of high pressure gas or water atomization and to be heat-treated fragmentation with solubility promoter.Increased operation.
Summary of the invention
Problem to be solved by this invention is: propose a kind of leaching treatment technique of cobalt-containing rare alloy, to overcome the deficiency of existing technology, shorten technological process, enhance productivity, improve the leaching yield of cobalt and copper.
In order to address the above problem, basic design of the present invention is: for guaranteeing different thermodynamic condition in leaching process dynamic conditions and the different element leaching process, at first solve the powder process problem of this rare alloy, kinetics requires the specific surface area of the solid matter of participation solid-liquid reaction to want big, be that granularity is little, usually to could guarantee speed of response faster by the above screen analysis granularity of 100 orders.Solve the powder process problem, change the mode of the broken powder-grinding of multistage machinery, because tool toughness is had the material of ductility again, this mode is of no avail.Known by the metallurgical analysis of this rare alloy and the character and the leaching thermodynamics of principal element: cobalt, iron, copper metal are selectively to be dissolved in certain organic acid, and the priority of dissolving order also can be directed at solute and be reduced to metal again because of the different redox potential of element.Therefore, the present invention uses mixed organic acid, and the redox potential of solution in the control process makes the dissolved of valuable metal cobalt and copper maximum possible.
Realize that technical scheme of the present invention is:
A kind of leaching treatment technique of cobalt-containing rare alloy with after the cobalt-containing rare alloy fusing, becomes finely powdered with high pressure water impact atomizing and cooling earlier, leaches with mineral acid again; It is characterized in that: the concrete processing step that is adopted is:
A, with electric furnace with after the cobalt-containing rare alloy fusing, send into an atomizing container, become the finely powdered slip with high pressure water impact and cooling;
B, the fine powder slip is sent in first steel basin that dilute sulphuric acid is housed, be heated to 50-95 ℃ of temperature after, add concentrated nitric acid;
C, the slurry that the b step reaction is ended carry out solid-liquid separation, and isolated immersion liquid is sent, and extract cobalt and copper;
D, the b step soaked slag send in second steel basin that dilute sulphuric acid, rare nitric acid are housed, be heated to 50-95 ℃ of temperature after, add concentrated nitric acid again;
E, the slurry that the d step reaction is ended carry out solid-liquid separation, and isolated immersion liquid adverse current is sent back in first steel basin of b step;
F, the slag that soaks of e step is sent into water washing and reclaimed.
The present invention and existing rare alloy powder process and extract technology have relatively been simplified technological process, and two sections Mechanical Crushing powder-grindings are changed into the fusing spray pulverization, three sections adverse currents or repeatedly soak and change into two sections adverse currents and leach; Improved production efficiency greatly, the powder manufacturing apparatus of identical investment more than the many twices of fusing spray pulverization technology powder process amount, has shortened extraction time 1/3; The leaching yield of cobalt and copper＞99% improves more than three percentage points; The leaching yield of iron＜60% reduces by 1/3, thereby reduces follow-up deironing cost 1/3.
Flouring technology of the present invention can also substitute the water quenching technology of this rare alloy, about 500 yuan/ton of the production cost of saving powder process melting process.
Description of drawings
Most preferred embodiment of the present utility model can provide in conjunction with the following drawings:
Fig. 1 is an alloy raw material X-ray diffraction spectrogram;
Fig. 2 is the microphotograph (* 520) of alloy material;
Fig. 3 amplifies for Fig. 2 A;
Fig. 4 is a process flow sheet of the present invention
Embodiment
The combined process flow process, with concrete embodiment the present invention is done detailed description:
Process flow sheet is described to be a kind of technology that rare alloy is produced the solution of purification cobalt and copper of separating.
The first step is produced the fine powder slip of rare alloy according to following technology: earlier this rare alloy particle is put into furnace melting, fish for the slag of bath surface, melt temperature risen to be higher than 100 ℃ of fusing points, the starting high-pressure hydraulic pump, the about 40Mpa of deployed hydraulic pressure injects the bottom pour ladle that spray chamber top has certain pore size with melt, and moment obtains the fine powder slip, the fine powder slip by 100 order water sieves, is become the qualified fine powder slip for leaching cobalt and copper.
Second step was produced the solution that contains cobalt and copper according to following technology: the above-mentioned fine powder slip that makes is added in one section normal pressure leaching vat, inject two sections infusion solutions and dilute sulphuric acid in one section leaching vat in advance, solution acidity is 2N in the groove, is heated to temperature more than 60 ℃, and starting is stirred.Add the fine powder slip and continue to be warming up to 85-90 ℃, add concentrated nitric acid with desired flow simultaneously, the about 400mv of redox potential of control solution in the process.After 6 hours, one section leaching process finished when the PH of solution was 1-2, and the leaching yield of cobalt and copper is about 85% respectively.With slurries filtration, filtrate is sent and is extracted cobalt and copper then, and filter residue adds in two sections normal pressure leaching vat, and solution acidity is 4N in the groove, and other processing parameters are identical with one section leaching, leach terminal point solution acidity＜2N.With slurries filtration, filtrate send one section to make leach liquor then, and filter residue send water washing to regain cobalt and the copper that has leached.The liquid-solid ratio of two sections leachings (weight) determines that according to the composition of this rare alloy general range is 4-10: 1.Two sections comprehensive leaching yield＞99% of the present invention.
Claims (1)
1. the leaching treatment technique of a cobalt-containing rare alloy with after the cobalt-containing rare alloy fusing, becomes finely powdered with high pressure water impact atomizing and cooling earlier, leaches with mineral acid again; It is characterized in that: the concrete processing step that is adopted is:
A, with electric furnace with after the cobalt-containing rare alloy fusing, send into an atomizing container, become the finely powdered slip with high pressure water impact and cooling;
B, the fine powder slip is sent in first steel basin that dilute sulphuric acid is housed, be heated to 50-95 ℃ of temperature after, add concentrated nitric acid;
C, the slurry that the b step reaction is ended carry out solid-liquid separation, and isolated immersion liquid is sent, and extract cobalt and copper;
D, the b step soaked slag send in second steel basin that dilute sulphuric acid, rare nitric acid are housed, be heated to 50-95 ℃ of temperature after, add concentrated nitric acid again;
E, the slurry that the d step reaction is ended carry out solid-liquid separation, and isolated immersion liquid adverse current is sent back in first steel basin of b step;
F, the slag that soaks of e step is sent into water washing and reclaimed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007101925512A CN100545276C (en) | 2007-12-10 | 2007-12-10 | A kind of leaching treatment technique of cobalt-containing rare alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007101925512A CN100545276C (en) | 2007-12-10 | 2007-12-10 | A kind of leaching treatment technique of cobalt-containing rare alloy |
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| Publication Number | Publication Date |
|---|---|
| CN101186972A true CN101186972A (en) | 2008-05-28 |
| CN100545276C CN100545276C (en) | 2009-09-30 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101524761B (en) * | 2009-04-17 | 2010-10-13 | 戴煜 | Method for preparing raw cobalt mineral powder |
| CN104152670A (en) * | 2014-08-29 | 2014-11-19 | 云南天浩稀贵金属股份有限公司 | Pretreatment technology for indium and germanium extraction |
| CN107760865A (en) * | 2016-08-17 | 2018-03-06 | 中国科学院过程工程研究所 | A kind of method of the dipped journey leachate gallium lithium ion enrichment of coal ash alkali |
-
2007
- 2007-12-10 CN CNB2007101925512A patent/CN100545276C/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101524761B (en) * | 2009-04-17 | 2010-10-13 | 戴煜 | Method for preparing raw cobalt mineral powder |
| CN104152670A (en) * | 2014-08-29 | 2014-11-19 | 云南天浩稀贵金属股份有限公司 | Pretreatment technology for indium and germanium extraction |
| CN104152670B (en) * | 2014-08-29 | 2016-05-25 | 云南天浩稀贵金属股份有限公司 | The pre-treating technology that a kind of indium germanium refines |
| CN107760865A (en) * | 2016-08-17 | 2018-03-06 | 中国科学院过程工程研究所 | A kind of method of the dipped journey leachate gallium lithium ion enrichment of coal ash alkali |
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| Publication number | Publication date |
|---|---|
| CN100545276C (en) | 2009-09-30 |
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Effective date of registration: 20200117 Address after: 423000 in the nonferrous metals industrial park, bailutang Town, Suxian District, Chenzhou City, Hunan Province Patentee after: Chenzhou Jincheng Environmental Protection Technology Co., Ltd. Address before: 423000 non ferrous metal industry zone, Hunan, Chenzhou Patentee before: Chenzhou Jinshan Metallurgy Chemical Co., Ltd. |
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