CN101994008B - Zinc-cobalt separation process for producing nickel-cobalt slag by zinc smelting purification - Google Patents
Zinc-cobalt separation process for producing nickel-cobalt slag by zinc smelting purification Download PDFInfo
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- CN101994008B CN101994008B CN2010105437007A CN201010543700A CN101994008B CN 101994008 B CN101994008 B CN 101994008B CN 2010105437007 A CN2010105437007 A CN 2010105437007A CN 201010543700 A CN201010543700 A CN 201010543700A CN 101994008 B CN101994008 B CN 101994008B
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Abstract
The invention relates to a zinc-cobalt separation process for producing nickel-cobalt slag through zinc smelting purification, which separates and enriches cobalt from nickel-cobalt slag leachate by using a cobalt activation inorganic coacervation method to recover the cobalt, removes cadmium from the leachate after cobalt removal by using a conventional zinc powder replacement method to obtain sponge metal cadmium, and feeds the sponge metal cadmium into a zinc smelting copper-cadmium treatment process to recover the metal cadmium. The liquid after cobalt and cadmium removal is returned to the leaching procedure in the main zinc smelting system for recovery, so that metals such as zinc, cobalt, cadmium and the like in the nickel-cobalt slag are comprehensively recovered, the influence of long-term accumulation of the slag on environmental pollution in the zinc industry and the risk of transferring heavy metal pollutants such as cadmium and the like in irregular takeaway are eliminated, the slag is recycled and operated in a closed circuit, no waste water and waste gas is discharged, valuable metals are comprehensively recovered, the requirement of clean production is met, and the industrial problem is solved.
Description
Technical field
The invention belongs to Metal smelting comprehensive reutilization field, relate in particular to a kind of Technology of the comprehensive reutilization to the nickel cobalt slag that produces in the zinc hydrometallurgy cleaning section.
Background technology
Flowsheet of wet zinc smelting is the zinc ore concentrate roasting, and the calcining of generation leaches zinc, and zinc lixiviating solution purification and impurity removal, zinc scavenging solution electrodeposition sink zinc.Zinc lixiviating solution purification and impurity removal operation can produce a kind of slag charge that contains metals such as zinc, cobalt, cadmium, is commonly called as nickel cobalt slag.
Wet method zinc smelting enterprise only carries out simple pickling to the nickel cobalt slag that produces at present, and the technical term selectivity leaches.Because also easily by the acid dissolving, therefore, pickling can only add a spot of acid to metals such as the cobalt in the nickel cobalt slag, cadmium; Metallic zinc in the nickel cobalt slag is leached sub-fraction; Reclaim wherein sub-fraction zinc, the pickling slag is then stored up or is undersold, and sells the part major part and is prepared pension parachute by the zinc salt of small scale; Because small scale; Environmental protection facility is incomplete, when handling nickel cobalt slag, environment is caused severe contamination (cadmium pollution incident in recent years all has substantial connection with this slag transfer processing, like Xiang Tan, Hunan, Shaoguan, Guangdong).There is patent to adopt in the pressure oxidation acidleach method leaching zinc hydrometallurgy purified waste residue valency heavy metal (Chinese patent is arranged; Application number 200810103261.0), this technology is just studied the leaching of valuable metal in the purified waste residue, but does not propose the stripping technique that nickel cobalt slag leaches zinc, cobalt, cadmium in the solution of back; Cadmium adopts zinc dust precipitation to come out from the leach liquor displace easily; Cobalt then is not easy to be come out by zinc dust precipitation, needs to consume a large amount of zinc powders, should technology not see industrial applications simultaneously.
Summary of the invention
The objective of the invention is to avoid the deficiency of prior art to provide a kind of zinc smelting purification to produce nickel cobalt slag zinc cobalt separating technology; The cobalt enrichment is separated and made to this technology to cobalt with cobalt activated inorganic coacervation method from nickel cobalt slag leach liquor; Make cobalt obtain reclaiming; Except that adopting conventional zinc replacement that cadmium is removed, the leach liquor behind the cobalt obtains the sponge grease cadmium; Send into zinc copper smelting cadmium treatment process and reclaim cadmium metal, remove cobalt and reclaim except that the leaching operation that the leach liquor behind the cadmium returns in the zinc smelting host system, metals such as the zinc in the nickel cobalt slag, cobalt, cadmium are comprehensively reclaimed like this.
For realizing above-mentioned purpose, the technical scheme that the present invention takes is: a kind of zinc smelting purification produces nickel cobalt slag zinc cobalt separating technology, and it is characterized in that: step is:
(1) one section leaching: with joining in the leaching vat after the pulp of nickel cobalt slag water, add sulfuric acid then, stir; Reaction solution sulfuric acid initial concentration is controlled at 110～135g/L; Reaction solution quality liquid-solid ratio is 3～4 to 1,70～80 ℃ of Heating temperatures, 1～2 hour reaction times; Filter then, obtain one section leach liquor and one section leached mud;
(2) two sections leachings: with joining in the leaching vat after the pulp of one section leached mud water, add sulfuric acid then, stir; Reaction solution sulfuric acid initial concentration is controlled at 190～200g/L, and reaction solution quality liquid-solid ratio is 3～4 to 1,70～80 ℃ of Heating temperatures; 1～2 hour reaction times; Filter then, obtain two sections leach liquors and two sections leached muds, two sections leach liquors turn back to one section leaching operation of next batch;
(3) the activated inorganic coacervation removes cobalt: one section leach liquor is delivered to except that the cobalt groove, be heated to 70～95 ℃, add cobalt acvator and inorganic flocculation agent then; Cobalt acvator and inorganic flocculation agent add simultaneously in batches, and cobalt acvator add-on adds 40～60 kilograms by nickel cobalt slag per ton, and inorganic flocculation agent add-on adds 30～50 kilograms by nickel cobalt slag per ton; Divide to add for 3～6 times, each 13-20 minute at interval, reacted 2～4 hours; Filter then, obtain except that liquid and high cobalt slag behind the cobalt; Described acvator is made up of following component by weight percentage: ZnO 25～38%, Na
2O
221～45%, Na
2SO
425～42%, acvator adopts the general method uniform mixing to form; Described inorganic flocculation agent is made up of following component by weight percentage: ZnCO
32Zn (OH)
2H
2O 40～70%, and NaOH 30～60%, and inorganic flocculation agent adopts the general method uniform mixing to form.
Described zinc smelting purification produces nickel cobalt slag zinc cobalt separating technology, and comprise that also step (4) displacement removes cadmium: will deliver to except that the cadmium groove except that liquid behind the cobalt, the control initial acidity is pH4.0; 40～50 ℃ of temperature add zinc powder, and the zinc powder add-on is 1.1～1.2 times of theoretical amount of cadmium in the solution; Reacted 0.5～1 hour, and filtered then, obtain the sponge grease cadmium and remove cobalt except that liquid behind the cadmium; The sponge grease cadmium send the cadmium recovery system, removes cobalt and send Zn system except that liquid behind the cadmium.
Principle of the present invention is: be to leach nickel cobalt slag with sulfuric acid, valuable metal is dissolved in the solution, press filtration obtains containing the filtrating of Zn, Co, Cd etc.; Adopt the cobalt ion acvator with the cobalt activation; Add inorganic flocculation agent then cobalt is removed from solution, press filtration obtains high cobalt slag and the filtrating that contains Zn, Cd, with zinc dust precipitation cadmium is precipitated again; Press filtration obtains the sponge grease cadmium and contains zinc filtrating, the zinc-containing solution after purifying is turned back to wet zinc-making system reclaim zinc.
Main chemical equation is following:
Zn+H
2SO
4＝ZnSO
4+H
2↑
Co+H
2SO
4＝CoSO
4+H
2↑
Cd+H
2SO
4＝CdSO
4+H
2↑
Co
3++3OH
-＝Co(OH)
3↓
Cd
2++Zn＝Zn
2++Cd↓
The invention has the beneficial effects as follows: comprehensively reclaimed metals such as zinc in the nickel cobalt slag, cobalt, cadmium, two sections leached mud staples that produce in the process are for plumbous, can be sold to plumbous smeltery as the refining leady raw materials collocation use; Cobalt contents can be used as the raw material of producing cobalt greater than 8% in the high cobalt slag; Cadmium content is delivered to cadmium workshop section and is produced cadmium greater than 40% in the high cadmium slag.Owing to smelt the accessory system of main system as zinc; The waste residue that does not produce waste water and gas and need store up for a long time in the process; Eliminated in the zinc industry this slag is stored up the influence of environmental pollution for a long time and irregularly taken out the risk that shifts heavy metal contaminants such as cadmium; Realized the recycling closed circuit operation of this slag; Reach the cleaner production requirement, solved an industry difficult problem.
Description of drawings
Fig. 1 is a schema of the present invention
Embodiment
Below principle of the present invention and characteristic are described, institute gives an actual example and only is used to explain the present invention, is not to be used to limit scope of the present invention.
Embodiment 1: see Fig. 1, a kind of zinc smelting purification produces nickel cobalt slag zinc cobalt separating technology, and step is:
(1) one section leaching: with joining in the leaching vat after the pulp of nickel cobalt slag water, leaching vat are provided with the natural exhaust pipe, add sulfuric acid then; Reaction solution sulfuric acid initial concentration is controlled at 120～130g/L, and reaction solution quality liquid-solid ratio is 3/1, stirs; 70～75 ℃ of Heating temperatures; 110 minutes reaction times, filter then, obtain one section leach liquor and one section leached mud;
(2) two sections leachings: with joining in the leaching vat after the pulp of one section leached mud water, leaching vat are provided with the natural exhaust pipe, add sulfuric acid then; Reaction solution sulfuric acid initial concentration is controlled at 195～200g/L, and reaction solution quality liquid-solid ratio is 3/1, stirs; 70～75 ℃ of Heating temperatures in 110 minutes reaction times, are filtered then; Obtain two sections leach liquors and two sections leached muds, two sections leach liquors turn back to one section leaching operation of next batch;
(3) the activated inorganic coacervation removes cobalt: one section leach liquor is delivered to except that the cobalt groove, be heated to 75～85 ℃, add cobalt acvator and inorganic flocculation agent then; Cobalt acvator and inorganic flocculation agent add simultaneously in batches, and nickel cobalt slag per ton adds 50 kilograms in acvator, and nickel cobalt slag per ton adds 40 kilograms of inorganic flocculation agents; Add for 4 times, each 18 minutes at interval, reacted 3.5 hours; Filter then, obtain except that liquid and high cobalt slag behind the cobalt.
Described acvator, form by following component by weight percentage:
ZnO 25％
Na
2O
2 45％
Na
2SO
4 30％
Acvator adopts the general method uniform mixing to form.
Described inorganic flocculation agent, form by following component by weight percentage:
ZnCO
3·2Zn(OH)
2·H
2O 45％
NaOH 55％
Inorganic flocculation agent adopts the general method uniform mixing to form.
Embodiment 2: see Fig. 1, a kind of zinc smelting purification produces nickel cobalt slag zinc cobalt separating technology, and step is:
(1) one section leaching: with joining in the leaching vat after the pulp of nickel cobalt slag water, leaching vat are provided with the natural exhaust pipe, add sulfuric acid then; Reaction solution sulfuric acid initial concentration is controlled at 130～135g/L, and reaction solution quality liquid-solid ratio is 4/1, stirs; 75～80 ℃ of Heating temperatures; 90 minutes reaction times, filter then, obtain one section leach liquor and one section leached mud;
(2) two sections leachings: with joining in the leaching vat after the pulp of one section leached mud water, leaching vat are provided with the natural exhaust pipe, add sulfuric acid then; Reaction solution sulfuric acid initial concentration is controlled at 195～200g/L, and reaction solution quality liquid-solid ratio is 4/1, stirs; 70～80 ℃ of Heating temperatures in 90 minutes reaction times, are filtered then; Obtain two sections leach liquors and two sections leached muds, two sections leach liquors turn back to one section leaching operation of next batch;
(3) the activated inorganic coacervation removes cobalt: one section leachate is delivered to except that the cobalt groove; Be heated to 80～90 ℃; Add cobalt activator and inorganic flocculation agent then, cobalt activator and inorganic flocculation agent add simultaneously in batches, and nickel cobalt slag per ton adds 55 kilograms in activator; Nickel cobalt slag per ton adds 45 kilograms of inorganic flocculation agents; Add for 5 times, each 15 minutes at interval, reacted 3 hours; Filter then, obtain except that liquid and high cobalt slag behind the cobalt;
(4) displacement removes cadmium: will deliver to except that the cadmium groove except that liquid behind the cobalt, the control initial acidity is pH4.0,40～50 ℃ of temperature; Add zinc powder, the zinc powder add-on is 1.1 times of theoretical amount of cadmium in the solution, reacts 1 hour; Filter then, obtain the sponge grease cadmium and remove cobalt except that liquid behind the cadmium, removing cobalt is zinc sulfate except that liquid major ingredient behind the cadmium; The sponge grease cadmium send the cadmium recovery system, removes cobalt and send Zn system except that liquid behind the cadmium.
Described acvator, form by following component by weight percentage:
ZnO 35％
Na
2O
2 40％
Na
2SO
4 25％
Acvator adopts the general method uniform mixing to form.
Described inorganic flocculation agent, form by following component by weight percentage:
ZnCO
3·2Zn(OH)
2·H
2O 55％
NaOH 45％
Inorganic flocculation agent adopts the general method uniform mixing to form.
Embodiment 3: see Fig. 1, step is with embodiment 2, and be that described acvator is made up of following component by weight percentage: ZnO 33%, Na
2O
232%, Na
2SO
435%.
Described inorganic flocculation agent is made up of following component by weight percentage: ZnCO
32Zn (OH)
2H
2O60%, NaOH 40%.
Embodiment 4: step is with embodiment 2, and be that described acvator is made up of following component by weight percentage: ZnO 30%, Na
2O
235%, Na
2SO
435%.
Described inorganic flocculation agent is made up of following component by weight percentage: ZnCO
32Zn (OH)
2H
2O65%, NaOH 35%.
Embodiment 5: step is with embodiment 2, and be that described acvator is made up of following component by weight percentage: ZnO 38%, Na
2O
222%, Na
2SO
440%.
Described inorganic flocculation agent is made up of following component by weight percentage: ZnCO
32Zn (OH)
2H
2O70%, NaOH 30%.
Embodiment 6: step is with embodiment 2, and be that described acvator is made up of following component by weight percentage: ZnO 37%, Na
2O
221%, Na
2SO
442%.
Described inorganic flocculation agent is made up of following component by weight percentage: ZnCO
32Zn (OH)
2H
2O40%, NaOH 60%.
Embodiment 7: new precious emblem group zinc smelting system is built in Gansu, and this factory's nickel cobalt slag ingredient is: Zn 52%, and Co 0.43%, and Cd 2.58%, and Ni 0.05%, produces 2100t nickel cobalt slag every year approximately.After the step process according to embodiment 2, the cobalt that removes that obtains contains zinc 130～150g/L, Co≤10mg/L except that liquid behind the cadmium; Cd≤10mg/L; This solution returns zinc and smelts the mixing flow container that leaches the workshop in the host system, and high cobalt slag contains cobalt 8～10%, and the sponge grease cadmium contains cadmium 40%.
Zinc recovery 92% in the nickel cobalt slag.The 1000 tons of electric zinc that have been enterprise's fecund reclaimed and contained 9 tons of cobalt amounts of metal comprehensive recovery every year of nickel cobalt slag, reclaimed 51 tons of cadmium metals, annually were more than 600 ten thousand yuan of enterprise's increase profits.
The above is merely preferred embodiment of the present invention, in order to restriction the present invention, all any modifications of within spirit of the present invention and principle, being done, is not equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (2)
1. a zinc smelting purification produces nickel cobalt slag zinc cobalt separating technology, and it is characterized in that: step is:
(1) one section leaching: with joining in the leaching vat after the pulp of nickel cobalt slag water, add sulfuric acid then, stir; Reaction solution sulfuric acid initial concentration is controlled at 110～135g/L; Reaction solution quality liquid-solid ratio is 3～4 to 1,70～80 ℃ of Heating temperatures, 1～2 hour reaction times; Filter then, obtain one section leach liquor and one section leached mud;
(2) two sections leachings: with joining in the leaching vat after the pulp of one section leached mud water, add sulfuric acid then, stir; Reaction solution sulfuric acid initial concentration is controlled at 190～200g/L, and reaction solution quality liquid-solid ratio is 3～4 to 1,70～80 ℃ of Heating temperatures; 1～2 hour reaction times; Filter then, obtain two sections leach liquors and two sections leached muds, two sections leach liquors turn back to one section leaching operation of next batch;
(3) the activated inorganic coacervation removes cobalt: one section leach liquor is delivered to except that the cobalt groove, be heated to 70～95 ℃, add cobalt acvator and inorganic flocculation agent then; Cobalt acvator and inorganic flocculation agent add simultaneously in batches, and cobalt acvator add-on adds 40～60 kilograms by nickel cobalt slag per ton, and inorganic flocculation agent add-on adds 30～50 kilograms by nickel cobalt slag per ton; Divide to add for 3～6 times, each 13-20 minute at interval, reacted 2～4 hours; Filter then, obtain except that liquid and high cobalt slag behind the cobalt; Wherein acvator is made up of following component by weight percentage: ZnO 25～38%, Na
2O
221～45%, Na
2SO
425～42%; Inorganic flocculation agent is made up of following component by weight percentage: ZnCO
32Zn (OH)
2H
2O 40～70%, and NaOH 30～60%.
2. zinc smelting purification as claimed in claim 1 produces nickel cobalt slag zinc cobalt separating technology, and it is characterized in that also comprising that step (4) displacement removes cadmium: will deliver to except that the cadmium groove except that liquid behind the cobalt, the control initial acidity is pH4.0; 40～50 ℃ of temperature add zinc powder, and the zinc powder add-on is 1.1～1.2 times of theoretical amount of cadmium in the solution; Reacted 0.5～1 hour, and filtered then, obtain the sponge grease cadmium and remove cobalt except that liquid behind the cadmium; The sponge grease cadmium send the cadmium recovery system, removes cobalt and send Zn system except that liquid behind the cadmium.
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| CN2010105437007A CN101994008B (en) | 2010-11-11 | 2010-11-11 | Zinc-cobalt separation process for producing nickel-cobalt slag by zinc smelting purification |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102776374B (en) * | 2011-05-09 | 2014-02-26 | 深圳市格林美高新技术股份有限公司 | Treatment method of nickel-cadmium slag |
| CN102517455A (en) * | 2011-12-29 | 2012-06-27 | 株洲冶炼集团股份有限公司 | Method for recovering cadmium from copper cadmium residues |
| CN102649998B (en) * | 2012-05-28 | 2013-08-28 | 陕西水木油田技术服务有限公司 | Method for separating and enriching copper, cadmium and zinc in copper and cadmium sediment |
| CN104152705B (en) * | 2014-08-08 | 2016-08-17 | 西北矿冶研究院 | Process for producing cathode zinc by utilizing casting zinc dross tailings |
| CN106148714A (en) * | 2015-03-31 | 2016-11-23 | 三明学院 | A kind of Solid-Phase Extraction reclaims the method for cobalt in zinc hydrometallurgy mine tailings |
| CN105950875A (en) * | 2016-05-09 | 2016-09-21 | 钟庆文 | Processing method for purified cobalt residues of zinc and manganese hydrometallurgy |
| CN113005303A (en) * | 2021-03-26 | 2021-06-22 | 陕西锌业有限公司 | Method for extracting cobalt from cadmium-poor high-cobalt liquid |
| CN114058874A (en) * | 2021-11-24 | 2022-02-18 | 白银有色集团股份有限公司 | Method for reducing zinc content of lead slag |
| CN114480856B (en) * | 2021-12-15 | 2024-01-19 | 云南驰宏锌锗股份有限公司 | Method for recycling high-cadmium smoke and dust cadmium |
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| CN101550485A (en) * | 2008-04-02 | 2009-10-07 | 中国科学院过程工程研究所 | Oxidative pressure acid leaching method for processing purified waste residue in zinc hydrometallurgy process |
| CN101838736A (en) * | 2010-06-01 | 2010-09-22 | 河南豫光锌业有限公司 | Wet separation method for valuable metals in purified liquid cobalt slags of wet zinc smelting system |
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| JP2002121626A (en) * | 2000-10-18 | 2002-04-26 | National Institute Of Advanced Industrial & Technology | Method for recovering valuable metal from plating sludge |
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| CN101550485A (en) * | 2008-04-02 | 2009-10-07 | 中国科学院过程工程研究所 | Oxidative pressure acid leaching method for processing purified waste residue in zinc hydrometallurgy process |
| CN101838736A (en) * | 2010-06-01 | 2010-09-22 | 河南豫光锌业有限公司 | Wet separation method for valuable metals in purified liquid cobalt slags of wet zinc smelting system |
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