CN1861817A - Tech. of extracting metallic cobait from magnetic-iron ore tailing slag - Google Patents
Tech. of extracting metallic cobait from magnetic-iron ore tailing slag Download PDFInfo
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- CN1861817A CN1861817A CN 200510017588 CN200510017588A CN1861817A CN 1861817 A CN1861817 A CN 1861817A CN 200510017588 CN200510017588 CN 200510017588 CN 200510017588 A CN200510017588 A CN 200510017588A CN 1861817 A CN1861817 A CN 1861817A
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Abstract
This invention discloses a technology to extract the cobalt from the tailing of magnetic iron ore. Its characteristics are as follows: (1) calcining the pretreatment magnetic iron ore at high temperature, (2) prophyrizing the magnetic iron ore which is handed as (1), (3) extracting the ore by sulfuric acid, (4) eliminating the rare-earth, iron, calcium and magnesium by chemical neutralization, (5) eliminating the copper, manganese, zinc and other substance with extraction reagent P204, then we can get cobalt solution by separating nickel and cobalt with extraction P507, (6)back-extracting, (7)depositing the cobalt with ammonium oxalate, (8) calcining the ammonium oxalate to high lever cobalt dioxide. The quality of cobalt dioxide recovered by this way can achieve to the lever of international Y0, the recovery ratio of cobalt can be above 85%.
Description
Affiliated technical field
The invention belongs to the extraction process technology field of cobalt metal, relate generally to a kind of technology of from the magnetite tailings, extracting cobalt metal.
Technical background
The purposes of cobalt is very extensive, is mainly used in to produce various specific alloys.But along with developing rapidly of new high-tech industry, approximately with average annual about 6% speed increase, insufficiency of supply-demand is more and more big for the demand of cobalt metal.Cobalt is more active metal, is difficult to be elemental metals at nature and exists, and becomes the ore deposit to disperse very much.The cobalt ore resource of China is very poor, and in explored cobalt resource, the higher-grade cobalt ore is few, and most and other mineral deposit associations.
According to the raw material difference, the production technique of cobalt differs greatly, but mainly is divided into pyrogenic process and wet processing:
1., thermal process is with cobalt ore or contains the cobalt material through the pyrogenic process pre-treatment, makes cobalt obtain preliminary enrichment, then by wet extraction, remove impurity and prepare pure cobalt liquor, produce cobalt metal through electrolysis again, perhaps utilize pure cobalt liquor to produce cobalt salt or oxide compound.
2., full wet processing is will contain the cobalt material earlier to carry out wet method and leach, and cobalt is entered in the solution, prepares pure cobalt liquor through removing impurity, cobalt metal or direct production cobalt oxide are produced in electrolysis then.
At present, the raw material that China produces cobalt oxide mainly contains two kinds, and the one, cobalt concentrate or mineral intergrowth are as cobalt sulphur concentrate or symbiosis nickel cobalt ore etc.; The 2nd, cobalt-containing alloy or catalyzer waste material are as waste materials such as Wimet, kovar alloy, permanent magnet alloy and cobalt catalyst.Magnetite is rich on Tongbai mountain range, Henan, only in the Tongbo County with regard to two on hairiness collection and jewel precipice proven reserve and the magnetite having implemented to develop, mainly adopt magnetic separation process, the former year handles 300,000 tons of magnetites, the latter is 150,000 tons.Select the mine tailings behind the iron not process basically, directly be deposited in around the mining area, more than 140 ten thousand tons of the existing mine tailings in Mao Ji ore deposit and ore deposit, jewel precipice.Utilizable noble metal element is still arranged in these ore deposit tailings, should be reclaimed.
Through random sampling, assay, main chemical compositions is as follows in above-mentioned two magnetite tailings:
The main chemical compositions (wt.%) of table 1. Tongbai magnetite tailings
| Fe | FeO | Fe 3O 4 | SiO 2 | CaO | MgO | MnO | S | P | Cu | Co | Ni | |
| Before the magnetic separation | 41.7 | 18.5 | 34.8 | 15.0 | 8.6 | 2.7 | 0.37 | 0.95 | 0.01 | 0.09 | ||
| After the magnetic separation | 9.4 | 5.9 | 1.5 | 30.7 | 20.1 | 4.7 | 0.9 | 1.9 | 0.06 | 0.08 | 0.37 | 0.004 |
As seen, the grade that contains cobalt metal in the tailings is higher, and total amount is considerable, therefore has higher industrial recovery value.
Summary of the invention
The objective of the invention is based on containing the higher feature of cobalt in the Tongbai Shan Mountain magnetite tailings, a kind of technology of extracting cobalt metal from the magnetite tailings is provided.
The present invention realizes that the technical scheme that above-mentioned purpose takes is as follows: (1) high-temperature roasting pre-treatment magnetite tailings; (2) baked magnetite tailings is pulverized; (3) leach with sulfuric acid; (4) chemical neutralisation is removed rare earth, iron and calcium magnesium; (5) remove impurity such as copper, manganese, zinc with the P204 extraction agent, use P507 extracting and separating nickel and cobalt again, make more purified cobalt-carrying solution; (6) back extraction; (7) add ammonium oxalate and sink cobalt; (8) high-purity cobalt oxide is produced in the cobalt oxalate roasting.
Each processing step division of above scheme is as follows:
(1) roasting: purpose is that the metallic sulfide in the waste residue is converted into oxide compound, and iron is oxidized to Fe
2O
3, be beneficial to next step acidleach cobalt and removal of impurities.Condition experiment shows that suitable maturing temperature is 600～750 ℃, and roasting time should be 2.5～4.5 hours.
(2) abrasive material: the magnetite tailings after the roasting is pulverized, sieved with 200 mesh sieves, sieve (〉=200 order) powder down send dissolution process.(≤200 order) meal returns grinding on the sieve, and to powder sampling analysis cobalt and iron, calcium magnesium etc.
(3) leaching: leaching is a key of putting forward cobalt technology.The concentration of acid, liquid-solid ratio, temperature and time all can produce material impact to the leaching result in this process.The optimal conditions experimental result shows that the best leaching condition of sulfuric acid to leach magnetite tailings is: sulfuric acid concentration is advisable with 30～35%, and liquid-solid ratio gets 2～3: 1, and temperature is 80～100 ℃, leaches to get final product in 1～1.5 hour.
(4) deironing copper, calcium magnesium and rare earth: through behind the leaching process, contain a large amount of iron in the leach liquor, should at first remove.The sodium carbonate solution that adds 10～15% concentration in the gained acid dip solution is regulated pH value to 10～11 of leach liquor, with iron with alkali formula iron double salt (yellow modumite Na
2Fe
6(SO
4)
4(OH)
12) the difficulty soluble salt form remove.Simultaneously, most copper ion and trace rare-earth also are removed with the precipitation forms of Basic Chrome Sulphate in the solution.Filter, filter residue washs 2～3 times with room temperature water, and filtrate is sent subsequent processing.
Also contain a little copper (0.29g/l) and calcium, magnesium in the solution after the deironing, adopt Na
2S
2O
3Copper removal, NaF deliming, magnesium.The copper removal condition is: get the solution after a certain amount of deironing, add Na
2S
2O
3, make Cu and Na
2S
2O
3Mass ratio be about 1: 8～10.Heating makes temperature reach 90～95 ℃, and PH is 2.5～3.0, reaction times 1.0～1.5h.Add NaF then, make the mol ratio of calcium, magnesium reach 1: 1.2～1.5, the reaction times is decided to be 1.5～2.0h.
(5) extraction: it is that extraction agent P204 and P507 further remove impurity such as Cu, Mn, Zn that the present invention utilizes organic phosphine, and Co, Ni ion are separated.
P204, two (2-ethylhexyl) phosphonic acids.Pale yellow oily liquid body, proportion are 0.9694.
P507,2-ethylhexyl phosphonic acid list (2-ethylhexyl) ester, water white transparency thick liquid, proportion 0.9475.
The present invention utilizes sulfonated kerosene as P204 and P507 thinner.The sulfonated kerosene method for making: domestic kerosene mixes stirring twice with the cold vitriol oil (volume ratio 5: 1), and each stir about 10 minutes is fully removed unsaturated olefin and nitrogenous basic cpd in the kerosene, uses 5% Na again
2CO
3Solution (kerosene and Na
2CO
3Liquor capacity was than about 5: 1), stir, clean about 10 minutes, to remove sulfuric acid residual in the kerosene and oxygen acid compound, wash with water at last to neutrality and get final product.Its chemical ingredients is C
13-15H
28-32Alkane compound, chemical property is more stable, belongs to inert solvent.Kerosene sulfonated purpose is wherein to be unfavorable for the impurity such as unsaturated olefin that extract in order to remove.
Adopt NaOH that P204 is carried out pre-neutralization.The sulfonated kerosene solution of P204 and NaOH reaction is a saponification process, becomes soap with high alkali liquid (every liter of solution contains 500 and restrains NaOH) pre-neutralization, reach certain saponification degree after, make saponification degree reach 60～70% and get final product, be directly used in extraction.The mix proportions of P204 and sulfonated kerosene is 1: 3 (volume ratio), and the acidity of organic phase is advisable with 0.3～0.5, and the volume ratio of extraction agent and feed liquid is 3: 2～2.5.
After the P204 extraction finishes, again with P507 extraction and separation of Cobalt and Nickel.The mix proportions of P507 and sulfonated kerosene (volume ratio) is decided to be 1: 3, and its acidity is set at 0.60～0.75mol/l, and saponification degree reaches 60～70%, and the volume ratio of extraction agent and feed liquid is 3: 2.
(6) back extraction: the effect of back extraction is separation of cobalt and P507, and strip liquor uses the hydrochloric acid of 2.5～3.0mol/l to get final product, and isolated P507 returns and reuses.
(7) heavy cobalt: the concentration that contains cobalt chloride in the feed liquid after extraction and the back extraction is Co 〉=60～70g/l, Co/Ni 〉=and more than 3000.Adding concentration is the ammonium oxalate solution of 110～120g/l, and control reaction temperature is 60～65 ℃, and in 40～50 minutes reaction times, question response finishes, stop to stir, the sedimentation clarification, the pH value of clear liquid is in 1.0～1.5 scopes, filter, containing cobalt in the filtrate should return and use below 0.5g/l.
(8) roasting: will filter gained filter cake oven dry and remove moisture, and place 600～700 ℃ roasting temperature 3.0～3.5 hours then, making the cobalt oxalate decomposition and inversion is cobalt oxide.Be chilled to room temperature, pack, promptly get product.
The quality of the product cobalt oxide that aforesaid method reclaims reaches GB Y0 level, and the total yield of cobalt reaches more than 85%.
Description of drawings
Accompanying drawing is a process flow sheet of the present invention.
Embodiment:
Embodiment 1
The magnetite tailings is carried out high-temperature roasting at 600 ℃ handle about 2.5 hours of roasting time.Solid slag after the roasting is levigate to granularity be more than 200 orders, with the sulfuric acid to leach powder of 30% concentration, making liquid-solid ratio is 2: 1, temperature is 80 ℃, the time is 1 hour.Add the pH value to 10 of the sodium carbonate regulating solution of 10% concentration in the gained solution, iron is removed with the difficulty soluble salt form.Reaction is filtered after finishing, and filter residue washes with water 2 times.Get the solution after a certain amount of deironing, add Na
2S
2O
3, make Cu and Na
2S
2O
3Mass ratio be about 1: 8, the heating, make temperature reach 90, PH is 2.5, reaction times 1.0h.Ca, Mg total content adding NaF according to wherein make the mol ratio of the two reach 1: 1.2, react about 1.5h.With organic phosphine is that extraction agent P204 further removes impurity such as Cu, Mn, Zn and Co, Ni ion are separated with P507.The mix proportions of P204 and sulfonated kerosene is 1: 4 (volume ratio), and the acidity of organic phase gets 0.3, and the volume ratio of extraction agent and feed liquid is 3: 2, and it is 60% proper that saponification degree is controlled at.After the extraction of P204 extraction agent finishes, change down the operation of one P507 extraction and separation of Cobalt and Nickel over to.The mix proportions of P507 and sulfonated kerosene (volume ratio) is decided to be 1: 3, and its acidity is decided to be 0.60mol/l, and the saponification degree of control P507 is 60%.Use the above-mentioned gained of hydrochloric acid back extraction of 2.5mol/l to contain cobalt liquid.The ammonium oxalate solution that adds 110g/l concentration in the strip liquor reacts completely down to reacting to make in 40 minutes at 60 ℃, stops to stir, and the sedimentation clarification is filtered then.Filter cake oven dry is removed moisture, place 600 ℃ roasting temperature 3 hours then, making the cobalt oxalate decomposition and inversion is cobalt oxide, is chilled to room temperature, packs, and promptly gets product.
Embodiment 2
The magnetite tailings is carried out high-temperature roasting at 700 ℃ handle roasting time 3.5 hours.Solid after the roasting is levigate to granularity be more than 200 orders, with the sulfuric acid to leach powder of 33% concentration, making liquid-solid ratio is 2.5: 1, temperature is 90 ℃, the time is 1.2 hours.The pH value to 12 of the concentration sodium carbonate regulating solution of adding 12% can be removed iron in the gained solution with the difficulty soluble salt form.Reaction is filtered after finishing, and filter residue washes with water 3 times.Get the solution after a certain amount of deironing, add Na
2S
2O
3, make Cu and Na
2S
2O
3Mass ratio be about 1: 9, the heating, make temperature reach 93 ℃, PH is 2.8, reaction times 1.2h.The total content of foundation Ca, Mg wherein adds NaF, makes the mol ratio of the two reach 1: 1.4, reacts about 1.8h.With organic phosphine is that extraction agent P204 further removes impurity such as Cu, Mn, Zn and Co, Ni ion are separated with P507.The mix proportions of P204 and sulfonated kerosene is 1: 4 (volume ratio), and the acidity of organic phase gets 0.4, and the volume ratio of extraction agent and feed liquid is 3: 2.5, and it is 65% proper that saponification degree is controlled at.After the extraction of P204 extraction agent finishes, change down the operation of one P507 extraction and separation of Cobalt and Nickel over to.The mix proportions of P507 and sulfonated kerosene (volume ratio) is decided to be 1: 3, and its acidity is decided to be 0.70mol/l, and the saponification degree of control P507 is 65% to get final product.Use the above-mentioned gained of hydrochloric acid back extraction of 2.8mol/l to contain cobalt liquid.The ammonium oxalate solution that adds 115g/l concentration reacts completely down to reacting to make in 45 minutes at 62 ℃, stops to stir, and the sedimentation clarification is filtered then.The filter cake oven dry is removed moisture, placed 650 ℃ of roasting temperatures then 3.2 hours, making the cobalt oxalate decomposition and inversion is cobalt oxide, is chilled to room temperature, packs, and promptly gets product.
Embodiment 3
The magnetite tailings is carried out high-temperature roasting at 750 ℃ handle roasting time 4.5 hours.Solid after the roasting is levigate to granularity be more than 200 orders, with the sulfuric acid to leach powder of 35% concentration, making liquid-solid ratio is 3: 1, temperature is 100 ℃, the time is 1.5 hours.Add the pH value to 15 of the sodium carbonate regulating solution of 15% concentration in the gained solution, iron can be removed with the difficulty soluble salt form.Reaction is filtered after finishing, and filter residue washes with water 3 times.Get the solution after a certain amount of deironing, add Na
2S
2O
3, make Cu and Na
2S
2O
3Mass ratio be about 1: 10, the heating, make temperature reach 95 ℃, PH is 3.0, reaction times 1.5h.The total content of foundation Ca, Mg wherein adds NaF, makes the mol ratio of the two reach 1: 1.5, reacts about 2.0h.With organic phosphine is that extraction agent P204 further removes impurity such as Cu, Mn, Zn and Co, Ni ion are separated with P507.The mix proportions of P204 and sulfonated kerosene is 1: 4 (volume ratio), and the acidity of organic phase gets 0.5, and the volume ratio of extraction agent and feed liquid is 3: 2.5, and it is 70% proper that saponification degree is controlled at.After the extraction of P204 extraction agent finishes, change down the operation of one P507 extraction and separation of Cobalt and Nickel over to.The mix proportions of P507 and sulfonated kerosene (volume ratio) is decided to be 25: 75, and its acidity is decided to be 0.75mol/l, and the saponification degree of control P507 is 70% to get final product.Use the above-mentioned gained of hydrochloric acid back extraction of 3.0mol/l to contain cobalt liquid.The ammonium oxalate solution that adds 120g/l concentration reacts completely down to reacting to make in 50 minutes at 65 ℃, stops to stir, and the sedimentation clarification is filtered then.The filter cake oven dry is removed moisture, placed 700 ℃ of roasting temperatures then 3.5 hours, making the cobalt oxalate decomposition and inversion is cobalt oxide, is chilled to room temperature, packs, and promptly gets product.
Claims (8)
- A kind of technology of extracting cobalt metal from the magnetite tailings is characterized in that: (1) high-temperature roasting pre-treatment magnetite tailings; (2) baked magnetite tailings is pulverized; (3) leach with sulfuric acid; (4) chemical neutralisation is removed rare earth, iron and calcium magnesium; (5) remove impurity such as copper, manganese, zinc with the P204 extraction agent, use P507 extracting and separating nickel and cobalt again, make cobalt-carrying solution; (6) back extraction; (7) add ammonium oxalate and sink cobalt; (8) high-purity cobalt oxide is produced in the cobalt oxalate roasting.
- 2, the method for extracting cobalt metal from the magnetite tailings according to claim 1, it is characterized in that: to pretreated magnetite tailings material maturing temperature is 600～750 ℃, roasting time 2.5～4.5 hours.
- 3, the technology of extracting cobalt metal from the magnetite tailings according to claim 1 and 2 is characterized in that: baked magnetite ground slag is broken to granularity more than 200 orders.
- 4, the technology of from the magnetite tailings, extracting cobalt metal according to claim 1, it is characterized in that: the leaching condition of sulfuric acid to leach magnetite tailings is: sulfuric acid concentration is 30～35%, liquid-solid ratio 2～3: 1, temperature is 80～100 ℃, leaches 1～1.5 hour.
- 5, the technology of from the magnetite tailings, extracting cobalt metal according to claim 1, it is characterized in that: the sodium carbonate solution that adds 10～15% concentration in the gained acid dip solution is regulated pH value to 10～11 of leach liquor, removes de-iron, most copper ion and trace rare-earth; Filtered filtration residue washes secondary with water, and to the solution heating, temperature is 90～95 ℃, and PH is 2.5～3.0, adds 20% Na 2S 2O 3Solution makes Cu and Na 2S 2O 3Mass ratio be about 1: 8～10, reaction times 1.0～1.5h adds NaF again, makes that the mol ratio of calcium, magnesium is 1: 1.2～1.5, the reaction times is decided to be 1.5～2.0h.
- 6, the technology of from the magnetite tailings, extracting cobalt metal according to claim 1, it is characterized in that: with organic phosphine is that extraction agent P204 further removes impurity such as Cu, Mn, Zn and Co, Ni ion are separated with P507, the mix proportions of P204 and P507 and sulfonated kerosene was respectively 20: 80 and 25: 75 (volume ratio), and the acidity of organic phase is got 0.3～0.5mol/l and 0.6～0.75mol/l respectively.The volume ratio of P204 and P507 and feed liquid is 3: 2～2.5, and saponification degree is controlled at 60～70%.
- 7, the technology of extracting cobalt metal from the magnetite tailings according to claim 1 is characterized in that: P204 and P507 collection cobalt liquid are carried out back extraction with the hydrochloric acid of 2.5～3.0mol/l.
- 8, the technology of from the magnetite tailings, extracting cobalt metal according to claim 1, it is characterized in that: the ammonium oxalate solution that adds concentration in the feed liquid after extraction and back extraction and be 110～120g/l concentration sinks cobalt, temperature of reaction is 60～65 ℃, reaction times is 40～50 minutes, the sedimentation clarification, the pH value of clear liquor is 1.0～1.5.
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| CN107475511A (en) * | 2017-07-14 | 2017-12-15 | 上海大学 | It is a kind of by low nickel matte calcification baking acidleach high efficiency extraction nickel, copper, cobalt method |
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