CN104726717A - Method for recovering cobalt from inverse antimony purified cobalt residue - Google Patents
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Abstract
The invention relates to a method for recovering cobalt from inverse antimony purified cobalt residue. The inverse antimony purified cobalt residue of zinc hydrometallurgy is taken as a raw material, and the cobalt concentrate is prepared by use of the processes of leaching, iron removal and cobalt settlement. The reducing atmosphere of leaching the cobalt residue in sulfuric acid is controlled so that metals such as copper and germanium cannot be leached and only zinc, cadmium, cobalt and little iron can be leached; in this way, a relatively high pH value can be controlled during iron removal, the purpose of thorough iron removal can be achieved and the iron can be prevented from being oxidized and hydrolyzed into the cobalt concentrate during cobalt settlement; air serves as an iron removal oxidizing agent, while hydrogen peroxide serves as a cobalt settlement oxidizing agent, and no impurity is imported; and the method is advantageous for increasing the grade of the cobalt concentrate.
Description
Technical field
The present invention relates to a kind of method of inverse antimony purified cobalt slag Call Provision, belong to technical field of wet metallurgy.
Background technology
Known inverse antimony purified cobalt slag treatment process is mainly divided into following a few class: 1) simple weak acid wash: cobalt slag is after low temperature weak-acid leaching, and solution returns electric zinc host system, and slag muck retains cobalt to be recycled.The condition such as temperature, acidity, reaction times required by this technique is harsher, is completely difficult to be guaranteed by manual operation, so extensive tissue performs not strict in producing.2) leaching-extraction process: first the method will, against antimony purified cobalt slag sulfuric acid leaching cobalt, zinc, cadmium, adopt P204 extraction except impurity such as de-iron, zinc, cadmiums, then with P507 or N235 Extraction of Cobalt, through back extraction Call Provision or cobalt salt again.2) the heavy cobalt of sulfuric acid leaching-oxidation: the method first will against antimony purified cobalt slag sulfuric acid leaching cobalt, zinc, cadmium, copper, deironing after filtering, replace copper removal, cadmium more afterwards, cobalt oxidation is become high-valence state and hydrolytic precipitation by last oxidizer (chlorine, potassium permanganate, Sodium Persulfate, ammonium persulphate etc.), obtains cobalt concentrate.The pH value of the method deironing controls usually 4.0 ~ 4.5, and iron removing is not thorough, being together precipitated in hydrolysis cobalt slag, affecting cobalt concentrate grade when being oxidized heavy cobalt.In addition, oxygenant easily brings impurity element into, causes disadvantageous effect to valuable metal recovery in liquid after cobalt concentrate grade or heavy cobalt.
The condition adopted in the patent documentation method for wet separation of valuable metal " in the clean liquid cobalt slags of wet zinc-making system ": (1) cobalt slag meutral innersion: add sulfuric acid and water in the clean liquid cobalt slags of Xiang Hanxin, cobalt, sulfuric acid starting point concentration 100 ~ 120g/l, controlling liquid-solid ratio is 4 ~ 5: 1, extraction temperature is 80 ~ 85 DEG C, extraction time 4 ~ 5h, reaction end solution pH value is 5.0 ~ 5.2, obtains middle immersion fluid and middle leaching cobalt slag after reaction through press filtration; Middle leaching cobalt slag enters acidic leaching operation; (2) cobalt slag acidic leaching: soak cobalt slag in passing through and add acidic leaching groove, add sulfuric acid and water, sulfuric acid starting point concentration 120 ~ 150g/l, liquid-solid ratio is 5 ~ 6: 1, extraction temperature is 80 ~ 85 DEG C, extraction time 4 ~ 5h, terminal acidity 50 ~ 80g/l, obtain the plumbous body refuse of acidleach and acid leaching solution through press filtration after reaction; (3) immersion fluid deironing in: immersion fluid in cobalt slag meutral innersion is added iron removal trough, under agitation heat up and add hydrogen peroxide, 1 times of theoretical amount when the add-on of hydrogen peroxide is iron and oxidant reaction in middle immersion fluid, temperature of reaction controls between 55 ~ 60 DEG C, reaction times 1 ~ 2h, in reaction process, pH value remains between 4 ~ 4.5, obtains immersion fluid in after deironing through press filtration; (4) in, immersion fluid under agitation adds potassium permanganate in immersion fluid in cobalt is after deironing, potassium permanganate add-on is 2 times of the cobalt chemical reaction theoretical amount in oxidizing middle immersion fluid, temperature of reaction controls between 80 ~ 85 DEG C, reaction times 2 ~ 4h, in reaction process, pH value remains between 4 ~ 4.5, be purified liquid and filter-press residues through press filtration, gained filter-press residues is cobalt concentrate.The method deironing pH value controls between 4 ~ 4.5, and deironing is not thorough, will affect cobalt concentrate grade.Heavy cobalt oxidation agent potassium permanganate is reduced postprecipitation hydrolysis cobalt slag, also can affect the grade of cobalt slag.
The condition adopted patent documentation " from zinc abstraction containing the method for cobalt waste slag and recycling cobalt ": step 1 ball milling: take zinc abstraction and contain cobalt waste residue and add water and carry out wet ball-milling, water: slag weight ratio is 4.5:1 ~ 5.5:1; After ball milling, particle diameter-200 object is greater than 60%, is sent into by ore pulp and leaches steel basin and start stirring; Step 2 leaches: in leaching steel basin, slowly add heavy percentage concentration is 93% vitriol oil, and add-on is that zinc abstraction contains 73 ~ 78% of cobalt waste residue weight; Give the liquid heat leached in steel basin, temperature of reaction 65 ~ 75 DEG C, 1.0 ~ 1.5 hours vitriol oil joining days simultaneously, after the vitriol oil adds, continue stirring reaction to PH 4.5 ~ 5.0; Ore pulp must be leached; Step 3 press filtration lead skim: leaching ore pulp step 2 obtained enters pressure filter press filtration; Obtain lead skim and leach filtrate; Step 4 removing of iron and manganese: leaching filtrate step 3 obtained enters removing of iron and manganese steel basin, and analyze the iron manganese content leaching filtrate; Start to stir and heat and leach filtrate to 70 ~ 80 DEG C; The potassium permanganate taking mass content be greater than 98% according to 1.25 ~ 1.27 times of ferrimanganic weight in removing of iron and manganese steel basin, adds water and is made into the potassium permanganate solution that weight percent concentration is 0.5 ~ 1.5%; The sodium hydroxide taking mass content be greater than 95% according to 1.5 ~ 1.56 times of ferrimanganic weight in removing of iron and manganese steel basin, adds water and is made into the sodium hydroxide solution that weight percent concentration is 5 ~ 10%; Within the time of 30 ~ 40 minutes, slowly add potassium permanganate solution in removing of iron and manganese steel basin, and slowly add sodium hydroxide solution simultaneously, in control flume, solution pH value is between 4.5 ~ 5.0, keeps temperature 70 ~ 80 DEG C; Add rear continuation reaction 25 ~ 30 minutes, obtain removing of iron and manganese liquid; Step 5 press filtration ferrimanganic slag: removing of iron and manganese liquid step 4 obtained enters pressure filter press filtration; Obtain ferrimanganic slag and removing of iron and manganese filtrate; Step 6 sinks cobalt: removing of iron and manganese filtrate step 5 obtained enters heavy cobalt steel basin, and analyzes the cobalt contents of removing of iron and manganese filtrate; Start and stir and heat removing of iron and manganese filtrate to 70 ~ 80 DEG C; The ammonium persulphate that mass content is 98% is taken according to 5 ~ 6 times of weight of cobalt in heavy cobalt steel basin; Take according to 2.2 ~ 2.7 times of weight of cobalt in heavy cobalt steel basin the sodium hydroxide that mass content is 95%, add water and be made into the sodium hydroxide solution that weight percent concentration is 5 ~ 10%; Within the time of 1 ~ 2 hour, slowly add ammonium persulphate in heavy cobalt steel basin, and slowly add sodium hydroxide solution simultaneously, in control flume, solution pH value is between 4.0 ~ 4.5, keeps temperature 70 ~ 80 DEG C; Add rear continuation reaction 3 hours, cobalt contents in sampling analysis reaction liquid, if cobalt contents is greater than 10mg/l in reaction soln, continues reaction and be less than 10mg/l to reaction soln containing cobalt; Must sink cobalt liquid; Step 7 press filtration cobalt slag: the heavy cobalt liquid that step 6 is obtained; Enter pressure filter press filtration; Cobalt contents 30 ~ 42% cobalt slag and heavy cobalt filtrate.The method potassium permanganate removing of iron and manganese, because potassium permanganate is inherently containing MnO4, is entered slag at next step this MnO4 by high price cobalt precipitate reduction, affects the quality of cobalt product.Heavy cobalt oxidation agent ammonium persulphate and neutralizing agent sodium hydroxide can introduce ammonium, sodium ion, and after giving heavy cobalt, in solution, the recovery of valuable metal produces adverse influence.
Above-mentioned known technology there is impurity iron or manganese removes halfway problem, because iron or manganese are easily precipitated into hydrolysis cobalt slag when being oxidized heavy cobalt, thus affects cobalt concentrate grade.Heavy cobalt oxidation agent can introduce impurity, causes adverse influence to the recovery of valuable metal in liquid after cobalt concentrate grade and heavy cobalt.
Summary of the invention
The present invention is intended to solve known inverse antimony purified cobalt slag treatment technology iron, manganese removing is not thorough, and impurity brought into by oxygenant, reduces the technical barrier of cobalt concentrate grade.Invention one in a wet process zinc metallurgy is raw material against antimony purified cobalt slag, adopts leaching, deironing, heavy cobalt technique to prepare cobalt concentrate.Control the reduction atmosphere of sulfuric acid leaching cobalt slag, the metal such as copper, germanium is not allowed to leach, zinc, cadmium, cobalt and a small amount of iron is only allowed to leach, just can control higher pH value during such deironing, reach thorough deironing object, avoid that iron is oxidized in the lump when heavy cobalt to be hydrolyzed into cobalt concentrate, except ferroxidant air, heavy cobalt oxidation agent hydrogen peroxide, does not introduce impurity, and the method is conducive to improving cobalt concentrate grade.
The method of a kind of inverse antimony purified cobalt slag Call Provision of the present invention, is characterized in that: zinc metallurgy is raw material against antimony purified cobalt slag in a wet process, and adopt leaching, deironing, heavy cobalt technique to obtain cobalt concentrate, its concrete steps are carried out as follows,
(1) leach: with mass ratio range, according to inverse antimony purified cobalt slag: the ratio of water=1:2.0 ~ 2.5, to join against antimony purified cobalt slag (dry weight) produces in water, composition mixed liquor, stir, be warmed up to 86 ~ 90 DEG C, the sulphuric acid soln of 30 ~ 50wt% is slowly evenly added to mixed liquor, stop adding sulphuric acid soln when mixed liquor pH value is reduced to 2.5, when pH value is elevated to 4.0, slowly all sulphuric acid soln is even again adds sulphuric acid soln, circulation like this, until pH value no longer rises, add a small amount of cobalt slag and pH value is risen to 4.0, filter mixed liquor and obtain leach liquor and leached mud respectively,
(2) deironing: pass into air to step (1) gained leach liquor and carry out iron removal by oxidation, temperature controls at 86 ~ 90 DEG C, add neutralizing agent adjust ph in 4.0 ~ 4.5 scopes, deironing time 3 ~ 4h, with neutralizing agent, pH value is adjusted to 5.2 ~ 5.4 during terminal, filters and obtain liquid and iron dross removing after deironing respectively;
(3) heavy cobalt: add theoretical amount 2 ~ 3 times of hydrogen peroxide in the solution after step (2) gained deironing, temperature controls at 70 ~ 90 DEG C, time 250 ~ 300min, and with neutralizing agent adjust ph 5.2 ~ 5.4, filtration obtains liquid and cobalt concentrate after heavy cobalt respectively.
Described leaching step (1) gained leached mud gives other to smelt flow process, for reclaiming other valuable metals.
Described iron removal (2) neutralizing agent used is one of calcium oxide, calcium hydroxide or the two mixture by any ratio.
The harmless treatment of described deironing gained iron dross removing pyrogenic process.
The preferred sodium hydroxide of described heavy cobalt neutralizing agent used.
Described heavy cobalt step (3) gained sinks liquid after cobalt and gives other to smelt flow process, for reclaiming other valuable metals.
Described heavy cobalt step (3) gained cobalt concentrate is as the raw material carrying cobalt.
Tool of the present invention has the following advantages and effect:
(1) the reduction atmosphere of sulfuric acid leaching cobalt slag is controlled, do not allow the metal such as copper, germanium leach, only allow zinc, cadmium, cobalt and a small amount of iron leach, during such deironing, just can control higher pH value, reach thorough deironing object, avoid that iron is together oxidized when heavy cobalt to be hydrolyzed into cobalt concentrate.
(2) except ferroxidant air, heavy cobalt oxidation agent hydrogen peroxide, does not introduce impurity, is conducive to improving cobalt concentrate grade.
Embodiment
The present invention is implemented by following steps
(1) leach: according to the ratio of weight ratio 1:2.0 ~ 2.5, to join against antimony purified cobalt slag (dry weight) produces in water, composition mixed liquor, stir, be warmed up to 86 ~ 90 DEG C, the sulphuric acid soln of 30 ~ 50wt% is slowly evenly added to mixed liquor, stop adding sulphuric acid soln when mixed liquor pH value is reduced to 2.5, again slowly evenly sulphuric acid soln is added when pH value is elevated to 4.0, circulation like this, until pH value no longer rises, add a small amount of cobalt slag and pH value is risen to 4.0, filter mixed liquor and obtain leach liquor and leached mud respectively;
(2) deironing: pass into atmospheric oxidation deironing to step (1) gained leach liquor, control temperature 86 ~ 90 DEG C, adds neutralizing agent adjust ph 4.0 ~ 4.5, deironing time 3 ~ 4h, with neutralizing agent, pH value is adjusted to 5.2 ~ 5.4 during terminal, filters and obtain liquid and iron dross removing after deironing respectively.
(3) heavy cobalt: add theoretical amount 2 ~ 3 times of hydrogen peroxide in liquid after step (2) gained deironing, control temperature 70 ~ 90 DEG C, time 250 ~ 300min, and with neutralizing agent adjust ph 5.2 ~ 5.4, filtration obtains liquid and cobalt concentrate after heavy cobalt respectively.
Described step (1) gained leached mud gives other to smelt flow process, for reclaiming other valuable metals;
Described step (2) neutralizing agent used is calcium oxide or calcium hydroxide or the two mixture by any ratio;
The harmless treatment of described step (2) gained iron dross removing pyrogenic process;
Described step (3) hydrogen peroxide used is the aqueous solution containing hydrogen peroxide 20 ~ 60%, i.e. hydrogen peroxide;
Described step (3) neutralizing agent used is sodium hydroxide;
Described step (3) gained sinks liquid after cobalt and gives other to smelt flow process, for reclaiming other valuable metals;
Described step (3) gained cobalt concentrate is as the raw material carrying cobalt.
embodiment 1
(1) leach: inverse antimony purified cobalt slag is (containing cobalt 0.2wt%, zinc 20wt%, plumbous 15wt%, cadmium 7wt%, copper 5wt%, iron 1wt%, silver 300g/t, germanium 600g/t) dry weight 1t, join together with the production water of 2t in mechanical agitating tank, stir, be warmed up to 88 DEG C, the sulphuric acid soln of 40wt% is evenly slowly added to mixed liquor, stop adding sulphuric acid soln when mixed liquor pH value is reduced to 2.5, again slowly evenly sulphuric acid soln is added when pH value is elevated to 4.0, circulation like this, until pH value no longer rises, add a small amount of cobalt slag and pH value is risen to 4.0, filter mixed liquor and obtain leach liquor and leached mud respectively, the leaded 31.25wt% of gained leached mud, cupric 9.6wt%, germanic 0.11wt%, argentiferous 625g/t, this leached mud send lead bullion melting to reclaim plumbous, silver, copper, then send fuming furnace to reclaim zinc and germanium, gained leach liquor is containing cobalt 0.89g/l, containing zinc 73g/l, cadmium 31g/l, iron content 1.4g/l.
(2) deironing: pass into atmospheric oxidation deironing to step (1) gained leach liquor, control temperature 87 DEG C, adds calcium hydroxide adjust ph 4.3, deironing time 3.2h, with calcium hydroxide, pH value is adjusted to 5.2 ~ 5.4 during terminal, filters and obtain liquid and iron dross removing after deironing respectively.Gained iron dross removing, carries out harmless treatment with fuming furnace; After deironing, liquid is containing cobalt 0.87g/l.
(3) heavy cobalt: add hydrogen peroxide in step (2) gained deironing liquid, add-on is according to reaction equation: 2Co
2++ H
20
2+ 4OH
-→ 2 Co (OH)
33.0 times of ↓ procedural theory amount, control temperature 75 DEG C, time 300min, and by sodium hydroxide adjust ph 5.2 ~ 5.4, filters and obtains liquid and cobalt concentrate after heavy cobalt respectively; Gained sinks liquid after cobalt and gives other operations to reclaim cadmium, zinc and nickel; Gained cobalt concentrate contains cobalt 18.1wt%, as the raw material carrying cobalt.The rate of recovery 95.8% of whole process cobalt.
embodiment 2
(1) leach: inverse antimony purified cobalt slag is (containing cobalt 1wt%, zinc 15wt%, plumbous 10wt%, cadmium 5wt%, iron 1.5wt%) dry weight 1t, join together with the production water of 2.5t in mechanical agitating tank, stir, be warmed up to 90 DEG C, the sulphuric acid soln of 35% is evenly slowly added to mixed liquor, stop adding sulphuric acid soln when mixed liquor pH value is reduced to 2.5, again slowly evenly sulphuric acid soln is added when pH value is elevated to 4.0, circulation like this, until pH value no longer rises, add a small amount of cobalt slag and pH value is risen to 4.0, filter mixed liquor and obtain leach liquor and leached mud respectively, the leaded 22.2wt% of gained leached mud, zinc 6.7wt%, it is plumbous that this leached mud send lead bullion melting to reclaim, then send fuming furnace to reclaim zinc, gained leach liquor is containing cobalt 4.45g/l, containing zinc 55g/l, cadmium 22g/l, iron content 2.0g/l.
(2) deironing: pass into atmospheric oxidation deironing to step (1) gained leach liquor, control temperature 89 DEG C, adds calcium oxide adjust ph 4.5, deironing time 3.5h, with calcium oxide, pH value is adjusted to 5.2 ~ 5.4 during terminal, filters and obtain liquid and iron dross removing after deironing respectively.Gained iron dross removing, carries out harmless treatment with fuming furnace; After deironing, liquid is containing cobalt 4.40g/l.
(3) heavy cobalt: add hydrogen peroxide in step (2) gained deironing liquid, add-on is according to reaction equation: 2Co
2++ H
20
2+ 4OH
-→ 2 Co (OH)
32.5 times of calculating of ↓ procedural theory amount, control temperature 85 DEG C, time 250min, and by sodium hydroxide adjust ph 5.2 ~ 5.4, filters and obtains liquid and cobalt concentrate after heavy cobalt respectively; Gained sinks liquid after cobalt and gives other operations to reclaim cadmium, zinc and nickel; Gained cobalt concentrate contains cobalt 23.4wt%, as the raw material carrying cobalt.The rate of recovery 96.9% of whole process cobalt.
Claims (7)
1. a method for inverse antimony purified cobalt slag Call Provision, is characterized in that: zinc metallurgy is raw material against antimony purified cobalt slag in a wet process, and adopt leaching, deironing, heavy cobalt technique to obtain cobalt concentrate, its concrete steps are carried out as follows,
(1) leach: with mass ratio range, according to inverse antimony purified cobalt slag: the ratio of water=1:2.0 ~ 2.5, to join against antimony purified cobalt slag (dry weight) produces in water, composition mixed liquor, stir, be warmed up to 86 ~ 90 DEG C, the sulphuric acid soln of 30 ~ 50wt% is slowly evenly added to mixed liquor, stop adding sulphuric acid soln when mixed liquor pH value is reduced to 2.5, when pH value is elevated to 4.0, slowly all sulphuric acid soln is even again adds sulphuric acid soln, circulation like this, until pH value no longer rises, add a small amount of cobalt slag and pH value is risen to 4.0, filter mixed liquor and obtain leach liquor and leached mud respectively,
(2) deironing: pass into air to step (1) gained leach liquor and carry out iron removal by oxidation, temperature controls at 86 ~ 90 DEG C, add neutralizing agent adjust ph in 4.0 ~ 4.5 scopes, deironing time 3 ~ 4h, with neutralizing agent, pH value is adjusted to 5.2 ~ 5.4 during terminal, filters and obtain liquid and iron dross removing after deironing respectively;
(3) heavy cobalt: add theoretical amount 2 ~ 3 times of hydrogen peroxide in the solution after step (2) gained deironing, temperature controls at 70 ~ 90 DEG C, time 250 ~ 300min, and with neutralizing agent adjust ph 5.2 ~ 5.4, filtration obtains liquid and cobalt concentrate after heavy cobalt respectively.
2. according to the method for a kind of inverse antimony purified cobalt slag Call Provision described in claim 1, it is characterized in that: described leaching step (1) gained leached mud gives other to smelt flow process, for reclaiming other valuable metals.
3., according to the method for a kind of inverse antimony purified cobalt slag Call Provision described in claim 1, it is characterized in that: described iron removal (2) neutralizing agent used is one of calcium oxide, calcium hydroxide or the two mixture by any ratio.
4., according to the method for a kind of inverse antimony purified cobalt slag Call Provision described in claim 1, it is characterized in that: the harmless treatment of described deironing gained iron dross removing pyrogenic process.
5. the method for a kind of inverse antimony purified cobalt slag Call Provision according to claim 1 or 3, is characterized in that: the preferred sodium hydroxide of described heavy cobalt neutralizing agent used.
6. according to the method for a kind of inverse antimony purified cobalt slag Call Provision described in claim 1, it is characterized in that: described heavy cobalt step (3) gained sinks liquid after cobalt and gives other to smelt flow process, for reclaiming other valuable metals.
7., according to the method for a kind of inverse antimony purified cobalt slag Call Provision described in claim 1, it is characterized in that: described heavy cobalt step (3) gained cobalt concentrate is as the raw material carrying cobalt.
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CN114438323A (en) * | 2022-01-25 | 2022-05-06 | 呼伦贝尔驰宏矿业有限公司 | Environment-friendly harmless treatment method for iron slag, cobalt slag, lead slag and sulfur tailings |
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CN107619945A (en) * | 2017-09-12 | 2018-01-23 | 贵州省冶金科学研究室 | A kind of method that high cobalt Zinc residue removes cobalt |
CN108203764A (en) * | 2018-01-09 | 2018-06-26 | 云南驰宏资源综合利用有限公司 | A kind of method of microwave calcination zinc hydrometallurgy purified cobalt nickel slag production cobalt concentrate |
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CN111809066A (en) * | 2020-06-28 | 2020-10-23 | 紫金矿业集团股份有限公司 | Method for efficiently recovering cobalt from low-grade cobalt ore |
CN111809066B (en) * | 2020-06-28 | 2021-06-15 | 紫金矿业集团股份有限公司 | Method for efficiently recovering cobalt from low-grade cobalt ore |
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CN114438323A (en) * | 2022-01-25 | 2022-05-06 | 呼伦贝尔驰宏矿业有限公司 | Environment-friendly harmless treatment method for iron slag, cobalt slag, lead slag and sulfur tailings |
CN114438323B (en) * | 2022-01-25 | 2023-09-12 | 呼伦贝尔驰宏矿业有限公司 | Environment-friendly harmless treatment method for iron slag, cobalt slag, lead slag and sulfur tailings |
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