CN106222411A - Three sections of extraction copper removals, manganese, ferrum, calcium, methods of magnesium are used from cobalt salt solution - Google Patents
Three sections of extraction copper removals, manganese, ferrum, calcium, methods of magnesium are used from cobalt salt solution Download PDFInfo
- Publication number
- CN106222411A CN106222411A CN201610726211.2A CN201610726211A CN106222411A CN 106222411 A CN106222411 A CN 106222411A CN 201610726211 A CN201610726211 A CN 201610726211A CN 106222411 A CN106222411 A CN 106222411A
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- China
- Prior art keywords
- liquid
- ferrum
- cobalt
- manganese
- extract
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0476—Separation of nickel from cobalt
Abstract
The invention belongs to apparatus technical field, particularly relate to a kind of three sections of extraction copper removals, manganese, ferrum, calcium, methods of magnesium of employing from cobalt salt solution.The invention discloses three sections of extraction copper removals, manganese, ferrum, calcium, methods of magnesium of employing from cobalt salt solution, it is characterized in that, p204 extract removing calcium with solvent extraction, copper, manganese, zinc, ferrum, the hydrochloric acid solution of 0.6N ~ 1.0N, the nitric acid liquid of 0.6N ~ 1.0N is used during one-section abstraction；Washing progression 4 ~ 6 grades, till aqueous phase flow is for keeping 1 ~ 2 grade of aqueous phase of outlet without obvious redness, washing water outlet PH is 3.0 ~ 4.0, and anti-ferrum liquid is 6N HCl.The invention has the beneficial effects as follows: technique is simple, reliable, low equipment investment, separating and removing impurities are effective, production efficiency is high, and environment is not resulted in pollution.
Description
Technical field
The invention belongs to apparatus technical field, particularly relate to a kind of use from cobalt salt solution three sections of extraction copper removals, manganese,
Ferrum, calcium, the method for magnesium.
Background technology
Cobalt concentrate, cobalt enriched substance are through leaching, except ferrum, or agent precipitate method removing calcium and magnesium, adjust pH4.5 ~ 5.0, miscellaneous through p204 extraction,
After p507 separates cobalt and nickel magnesium, the cobalt sulfate solution of back extraction gained or cobalt nitrate solution or cobalt chloride solution, impurity Cu, Mn, Fe,
It is metal impurities that Mg typically can only reach about 0.004g/L, i.e. Co/Me(Me) >=(20000 ~ 25000): 1, and produce LITHIUM BATTERY
Cobalt salt typically requires Co/Me >=25000:1 or higher, for improving the purity of cobalt salt, conventional way one be reduce extraction before
Feed liquid impurity content, as in feed liquid, Fe, Ca, Mg all reach below 0.00*g/L, one is to increase extraction and the washing progression of extraction line,
With finished fluid purity after raising extract and separate, although both measures all can be effectively improved product quality, reach LITHIUM BATTERY cobalt
The prescription that salt produces, but one is that production cost is high, and equipment investment is big, and one is that metal yield is low.And use three sections of extractions point
Cobalt salt is purified with other magazines, although add one section of deeply purified extn line from cobalt, will after separating cobalt and nickel magnesium due to p507
The concentration of cobalt is improved to 70 ~ 160g/L by 12 ~ 18g of feed liquid, thus deep purifying extraction miscellaneous line the most main extraction line is one
The extraction line that physical dimension is the least, not only low equipment investment, production efficiency is high, and constant product quality is good in economic efficiency, and right
The impurity content of extraction feed liquid is also put relatively wide, after oxidized for leachate neutralizing hydrolysis need to be removed ferrum by general, adjusts pH4.5
~ 5.0 can enter abstraction impurity removal and extract and separate high-purity cobalt salt product.
Summary of the invention
It is an object of the invention to solve techniques discussed above problem, it is provided that a kind of technique is simple, reliable, equipment investment
Save, separating and removing impurities is effective, production efficiency is high, and environment does not results in three sections of extractions of employing from cobalt salt solution of pollution
The method following the example of copper removal, manganese, ferrum, calcium, magnesium, its technical scheme is as follows:
Three sections of extraction copper removals, manganese, ferrum, calcium, methods of magnesium are used, it is characterised in that adopt during one-section abstraction from cobalt salt solution
With p204 extract removing calcium with solvent extraction, copper, manganese, zinc, ferrum, during two-stage extraction, use p507 extract extract and separate cobalt and nickel magnesium, three
The further degree of depth deliming of p204 extract and ferrum, copper, manganese is used during section extraction；Organic facies during three sections of extractions is mass percent
For: the p204 extract of 15% ~ 25% adds mass percent and is: the solvent naphtha of 75% ~ 85%, and feed liquid is the anti-cobalt of p507 extract
Liquid, pH value is 2.5 ~ 3.5, and organic facies first carries out homogeneous saponification with the NaOH that mass percent is 32%, is then converted to cobalt soap soap
Changing, during cobalt soap saponification, controlling PH is 6, CoSO4 concentration 15 ~ 20g/L, soda soap 1 ~ 2 grade, and cobalt soap 4 ~ 6 grades extracts level 9 ~ 12 grades, washes
The section of washing regards the different washing liquid of different choice processing feed liquid system, and cobaltous sulfate liquid, cobaltous chloride liquid, cobalt nitrate liquid select 0.6N respectively
The sulphuric acid liquid of ~ 1.0N, the hydrochloric acid solution of 0.6N ~ 1.0N, the nitric acid liquid of 0.6N ~ 1.0N；Washing progression 4 ~ 6 grades, aqueous phase flow is for protecting
Hold 1 ~ 2 grade of aqueous phase of outlet without obvious redness till, washing water outlet PH is 3.0 ~ 4.0, and anti-ferrum liquid is 6N HCl.
What the present invention provided uses three sections of extraction copper removals, manganese, ferrum, calcium, methods of magnesium from cobalt salt solution, and P204 extracts
Liquid deep purifying is particularly suitable for sulfuric acid system and nitric acid system, not only can by the calcium in cobaltous sulfate liquid or cobalt nitrate liquid by 0.1 ~
0.3g/L is down to below 0.001g/L, it is possible to ferrum, copper, manganese are down to≤0.001g/L, to cobalt chloride solution, degree of depth deliming effect
Though more slightly worse than cobaltous sulfate liquid deep purifying, but calcium remains to reach about 0.005g/L, typically exists due to cobalt chloride solution Cl-concentration again
160 ~ 180g/L, Cu2+CuCl4 can be formed with Cl-2-The relation of complex anion, copper removal effect is poor, but still has 20-30% to Fe
Clearance.
Three sections of purification by liquid extraction cobalt salt solutions, the 3rd section of p204 extract deep purifying deliming and extraction equilibrium pH value relation ratio
Closer: as pH ＜ 2.5, the extraction yield of calcium raises with pH value and raises, and after pH ＞ 3.5, the extraction yield of calcium then raises with pH
And reduce, and copper, manganese, zinc particularly zinc is when pH reduces, and still has a higher extraction yield, and all along with pH value rising and
Raise.
The invention has the beneficial effects as follows: technique is simple, reliable, low equipment investment, separating and removing impurities are effective, produce effect
Rate is high, and environment is not resulted in pollution.
Detailed description of the invention
Embodiment be specifically described below:
From cobalt salt solution, use three sections of extraction copper removals, manganese, ferrum, calcium, methods of magnesium, during one-section abstraction, use p204 extract
Removing calcium with solvent extraction, copper, manganese, zinc, ferrum, use p507 extract extract and separate cobalt and nickel magnesium, use during three sections of extractions during two-stage extraction
The further degree of depth deliming of p204 extract and ferrum, copper, manganese；Organic facies during three sections of extractions is that mass percent is: 15% ~ 25%
P204 extract adds mass percent: the solvent naphtha of 75% ~ 85%, and feed liquid is the anti-cobalt liquid of p507 extract, and pH value is 2.5 ~
3.5, organic facies first carries out homogeneous saponification with the NaOH that mass percent is 32%, is then converted to cobalt soap saponification, during cobalt soap saponification,
Controlling PH is 6, CoSO4 concentration 15 ~ 20g/L, soda soap 1 ~ 2 grade, and cobalt soap 4 ~ 6 grades extracts level 9 ~ 12 grades, and washing section regards and processes feed liquid
The washing liquid that the different choice of system is different, cobaltous sulfate liquid, cobaltous chloride liquid, cobalt nitrate liquid select respectively 0.6N ~ 1.0N sulphuric acid liquid,
The hydrochloric acid solution of 0.6N ~ 1.0N, the nitric acid liquid of 0.6N ~ 1.0N；Washing progression 4 ~ 6 grades, aqueous phase flow is for keeping 1 ~ 2 grade of aqueous phase of outlet
Till obvious redness, washing water outlet PH is 3.0 ~ 4.0, and anti-ferrum liquid is 6N HCl.
Claims (1)
1. from cobalt salt solution, use three sections of extraction copper removals, manganese, ferrum, calcium, methods of magnesium, it is characterised in that during one-section abstraction
Use p204 extract removing calcium with solvent extraction, copper, manganese, zinc, ferrum, during two-stage extraction, use p507 extract extract and separate cobalt and nickel magnesium,
The further degree of depth deliming of p204 extract and ferrum, copper, manganese is used during three sections of extractions；Organic facies during three sections of extractions is percent mass
Ratio is: the p204 extract of 15% ~ 25% adds mass percent and is: the solvent naphtha of 75% ~ 85%, and feed liquid is the anti-cobalt of p507 extract
Liquid, pH value is 2.5 ~ 3.5, and organic facies first carries out homogeneous saponification with the NaOH that mass percent is 32%, is then converted to cobalt soap soap
Changing, during cobalt soap saponification, controlling PH is 6, CoSO4 concentration 15 ~ 20g/L, soda soap 1 ~ 2 grade, and cobalt soap 4 ~ 6 grades extracts level 9 ~ 12 grades, washes
The section of washing regards the different washing liquid of different choice processing feed liquid system, and cobaltous sulfate liquid, cobaltous chloride liquid, cobalt nitrate liquid select 0.6N respectively
The sulphuric acid liquid of ~ 1.0N, the hydrochloric acid solution of 0.6N ~ 1.0N, the nitric acid liquid of 0.6N ~ 1.0N；Washing progression 4 ~ 6 grades, aqueous phase flow is for protecting
Hold 1 ~ 2 grade of aqueous phase of outlet without obvious redness till, washing water outlet PH is 3.0 ~ 4.0, and anti-ferrum liquid is 6N HCl.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610726211.2A CN106222411A (en) | 2016-08-26 | 2016-08-26 | Three sections of extraction copper removals, manganese, ferrum, calcium, methods of magnesium are used from cobalt salt solution |
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| CN201610726211.2A CN106222411A (en) | 2016-08-26 | 2016-08-26 | Three sections of extraction copper removals, manganese, ferrum, calcium, methods of magnesium are used from cobalt salt solution |
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| CN106222411A true CN106222411A (en) | 2016-12-14 |
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| CN201610726211.2A Pending CN106222411A (en) | 2016-08-26 | 2016-08-26 | Three sections of extraction copper removals, manganese, ferrum, calcium, methods of magnesium are used from cobalt salt solution |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108342572A (en) * | 2018-03-20 | 2018-07-31 | 衢州华友钴新材料有限公司 | Using the technique of two-stage extraction method removal of impurities from copper-cobalt mine leachate |
| CN108677009A (en) * | 2018-05-21 | 2018-10-19 | 兰州金川新材料科技股份有限公司 | A kind of depth abstraction impurity removal method of cobalt chloride solution |
| CN108946826A (en) * | 2018-07-31 | 2018-12-07 | 金川集团股份有限公司 | A method of handling copper in nickeliferous cobalt sulfate solution, manganese impurity |
| CN109518005A (en) * | 2018-10-29 | 2019-03-26 | 安徽寒锐新材料有限公司 | A kind of production method of battery grade cobalt sulfate crystal |
| CN110257628A (en) * | 2019-07-24 | 2019-09-20 | 江苏理工学院 | A kind of method of iron in extraction cobalt sulfate solution |
| CN110669932A (en) * | 2019-09-25 | 2020-01-10 | 中南大学 | Method for comprehensively utilizing copper electrolyte purification resources |
| CN112481501A (en) * | 2020-11-12 | 2021-03-12 | 阳谷祥光铜业有限公司 | Method for preparing nickel powder by using decoppering final solution |
| CN113044889A (en) * | 2021-03-11 | 2021-06-29 | 浙江中金格派锂电产业股份有限公司 | Co-production process of cobalt sulfate and cobalt chloride |
| CN113174485A (en) * | 2021-04-29 | 2021-07-27 | 金川集团镍盐有限公司 | Method for deeply removing calcium and manganese in cobalt sulfate solution |
| CN114657394A (en) * | 2022-02-18 | 2022-06-24 | 浙江立鑫新材料科技有限公司 | Method for removing impurities and purifying cobalt salt solution |
| CN115058597A (en) * | 2022-06-30 | 2022-09-16 | 盛隆资源再生（无锡）有限公司 | Method for recycling electroplating sludge containing calcium, iron, cobalt and nickel |
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| CN101463427A (en) * | 2008-11-27 | 2009-06-24 | 佛山市邦普镍钴技术有限公司 | Method for recycling valuable metal from cobalt white alloy |
| CN101629240A (en) * | 2009-07-30 | 2010-01-20 | 浙江华友钴业股份有限公司 | Method for preparing high-purity cobalt solution by purifying cadmium contained in cobalt solution by solvent extraction method |
| CN102061390A (en) * | 2010-12-03 | 2011-05-18 | 安化金源新材料有限责任公司 | Method for directly producing high-purity electronic level cobaltous sulfate by using cobalt-containing waste |
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- 2016-08-26 CN CN201610726211.2A patent/CN106222411A/en active Pending
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| CN101463427A (en) * | 2008-11-27 | 2009-06-24 | 佛山市邦普镍钴技术有限公司 | Method for recycling valuable metal from cobalt white alloy |
| CN101629240A (en) * | 2009-07-30 | 2010-01-20 | 浙江华友钴业股份有限公司 | Method for preparing high-purity cobalt solution by purifying cadmium contained in cobalt solution by solvent extraction method |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108342572A (en) * | 2018-03-20 | 2018-07-31 | 衢州华友钴新材料有限公司 | Using the technique of two-stage extraction method removal of impurities from copper-cobalt mine leachate |
| CN108677009A (en) * | 2018-05-21 | 2018-10-19 | 兰州金川新材料科技股份有限公司 | A kind of depth abstraction impurity removal method of cobalt chloride solution |
| CN108946826A (en) * | 2018-07-31 | 2018-12-07 | 金川集团股份有限公司 | A method of handling copper in nickeliferous cobalt sulfate solution, manganese impurity |
| CN109518005A (en) * | 2018-10-29 | 2019-03-26 | 安徽寒锐新材料有限公司 | A kind of production method of battery grade cobalt sulfate crystal |
| CN109518005B (en) * | 2018-10-29 | 2021-03-23 | 安徽寒锐新材料有限公司 | Production method of battery-grade cobalt sulfate crystal |
| CN110257628A (en) * | 2019-07-24 | 2019-09-20 | 江苏理工学院 | A kind of method of iron in extraction cobalt sulfate solution |
| CN110669932B (en) * | 2019-09-25 | 2021-04-20 | 中南大学 | Method for comprehensively utilizing copper electrolyte purification resources |
| CN110669932A (en) * | 2019-09-25 | 2020-01-10 | 中南大学 | Method for comprehensively utilizing copper electrolyte purification resources |
| CN112481501A (en) * | 2020-11-12 | 2021-03-12 | 阳谷祥光铜业有限公司 | Method for preparing nickel powder by using decoppering final solution |
| CN112481501B (en) * | 2020-11-12 | 2022-09-27 | 阳谷祥光铜业有限公司 | Method for preparing nickel powder by using decoppering final solution |
| CN113044889A (en) * | 2021-03-11 | 2021-06-29 | 浙江中金格派锂电产业股份有限公司 | Co-production process of cobalt sulfate and cobalt chloride |
| CN113174485A (en) * | 2021-04-29 | 2021-07-27 | 金川集团镍盐有限公司 | Method for deeply removing calcium and manganese in cobalt sulfate solution |
| CN114657394A (en) * | 2022-02-18 | 2022-06-24 | 浙江立鑫新材料科技有限公司 | Method for removing impurities and purifying cobalt salt solution |
| CN115058597A (en) * | 2022-06-30 | 2022-09-16 | 盛隆资源再生（无锡）有限公司 | Method for recycling electroplating sludge containing calcium, iron, cobalt and nickel |
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Application publication date: 20161214 |