CN102244309B - Method for recovering lithium from lithium power battery of electric automobile - Google Patents
Method for recovering lithium from lithium power battery of electric automobile Download PDFInfo
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- CN102244309B CN102244309B CN2011101476967A CN201110147696A CN102244309B CN 102244309 B CN102244309 B CN 102244309B CN 2011101476967 A CN2011101476967 A CN 2011101476967A CN 201110147696 A CN201110147696 A CN 201110147696A CN 102244309 B CN102244309 B CN 102244309B
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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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- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
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Abstract
The invention discloses a method for recovering lithium from a lithium power battery of an electric automobile, which comprises the following steps of: pulverizing the lithium power battery to obtain powder; adding a strong alkaline solution into the powder, dissolving aluminum and aluminum oxides, and filtering the solution to obtain filter mud; leaching the filter mud with a mixed solution of sulfuric acid solution and hydrogen peroxide solution to obtain a leaching liquid; adding an extraction liquid into the leaching liquid, and performing extraction and separation to take raffinate; regulating the pH of the raffinate to 3.0-8.0 by using an alkaline liquid, and precipitating impurities in the raffinate; and adding water-soluble fluorine salt into the raffinate to precipitating calcium and magnesium in the raffinate, and filtering to obtain a lithium salt solution. The method provided by the invention is applicable to all types of lithium power batteries, the finally obtained product is high-purity lithium carbonate with purity not less than 97.5% and can be directly applied to production, no high-temperature treatment is performed in the recovery treatment process, and the energy consumption is lower.
Description
Technical field
The present invention relates to a kind of method that reclaims lithium, particularly a kind of method that reclaims lithium from lithium power battery of electric automobile.
Background technology
At present, China's electrokinetic cell mainly adopts Ni-MH battery and two kinds of forms of lithium ion battery.The lithium-ion-power cell project is the emphasis of industry new investment, the whole world main lithium-ion-power cell manufacturing enterprise has begun investment distribution, concentrate on 2009～went into operation in 2010, China's lithium ion battery output in 2009 is 18.75 hundred million (approximately 37500 tons), on average contain 20% estimation of cobalt amount by waste and old lithium ion battery, contain the cobalt total amount and be about 7500 tons.Along with the increase of production capacity, estimate that China's lithium ion battery output in 2013 will reach 28.6 hundred million (approximately 57200 tons), when the time comes, the production capacity of the cobalt of lithium-ion-power cell resource will reach 11440 tons, namely be equivalent to the exploitation in a Large scale nonferrous metals mine.Production practices both domestic and external show: 1 ton of secondary metal of every production, and on average need 70 tons of ores of exploitation, and utilize the secondary nonferrous metal, energy conservation 85%～95%, production cost reduces by 50%～70%.
Received more and more people's concern due to the existing harm of waste and old electrokinetic cell self and its value that is rich in non-ferrous metal, the recovery of the cobalt in lithium ion battery, nickel, manganese has begun industrialization, but has the defectives such as the process program energy consumption is high, cost is high, economic benefit is remarkable, industrialization value is little for the present method of using of the recovery of lithium.
A kind of method that reclaims valuable metal from waste lithium cell is disclosed as CN101921917A, with the waste lithium cell mechanical crushing after discharge, 350 ℃～400 ℃ calcinings of high temperature, obtain containing the material of cobalt, copper and aluminium, adding content is 5%～10% sodium hydroxide solution, reacts 2～3 hours, alkali lye is filtered, washing, drying obtains containing the material of cobalt, copper, and the material that contains cobalt, copper is added certain density sulfuric acid and Na
2S
2O
3, stirring and dissolving adds the extractant extracting copper, and the solution after extracting copper is added the extractant Extraction of Cobalt.The method needs high-temperature calcination, and energy consumption is high, very easily causes secondary pollution.
The preparation Li that reclaims from waste and old lithium ion battery as disclosed in CN1747224A
xCoCO
2Method, the positive electrode of lithium battery is shredded, bubble is in METHYLPYRROLIDONE liquid, cobalt acid lithium powder is isolated in heating.Add nitric acid or Leaching in Hydrochloric Acid Co
2+And Li
+Ion adds the heavy Co that makes of ammoniacal liquor
2+Precipitation adds simultaneously surfactant and LiOH and adjusts Li
+Concentration.Obtain suspension.Filter out at last in suspension sediment and at the roasting temperature of 600 ℃ ~ 900 ℃, obtain Li
xCoCO
2Powder.The method needs the high-temperature roasting energy consumption high, very easily causes secondary pollution, simultaneously, there is no the removal of impurities process in technique, and product impurity is many, and quality is difficult to guarantee.
And for example CN101519726 discloses a kind of method that roasting direct is processed waste and old lithium ion battery and reclaimed valuable metal, particularly for the recycling take cobalt acid lithium as the waste and old lithium ion battery of positive electrode.At first the organic binder bond on organic diaphragm material and electrode material in 500～850 ℃ of roasting temperatures are removed battery, to size mixing through mixing with sodium sulphate (or potassium sulfate), the concentrated sulfuric acid after the battery material fragmentation of roasting, carry out secondary heat treatment at 350～600 ℃ of temperature in electric furnace, making the Metal Phase Transitions such as cobalt, copper and lithium in waste and old lithium ion battery is sulfate soluble in water, after water or dilution heat of sulfuric acid leach, extract respectively cobalt, copper with organic extractant from leachate again, and obtain copper and cobalt product.After precipitating lithium metal with sodium carbonate from the leachate that has removed cobalt and copper, leachate returns again processes hot secondary heat treatment material.The method exists energy consumption large equally, can cause the shortcomings such as secondary pollution.
In addition, in existing recovery technology, only the lithium electricity for single type reclaims, such as cobalt acid lithium, LiMn2O4 etc., to other positive electrode and inapplicable, and the elements such as lithium that reclaim, purity is generally lower, need to carry out complicated subsequent treatment and just can use by secondary, this has also increased the cost that uses virtually.
Summary of the invention
The object of the present invention is to provide a kind of method that reclaims lithium from lithium power battery of electric automobile.
The technical solution used in the present invention is:
A kind of method that reclaims lithium from lithium power battery of electric automobile comprises the following steps:
Be that electrokinetic cell is pulverized with lithium, obtain powder;
Add strong base solution in powder, the oxide of dissolved aluminum and aluminium filters to get filter mud;
The mixed solution of filter mud with sulfuric acid solution and hydrogen peroxide solution leached, obtain leachate;
Add extract at leachate, extract and separate is got raffinate;
The pH that regulates raffinate with alkali lye is 3.0～8.0, with the contamination precipitation in raffinate;
Add water-soluble villiaumite in raffinate, with the calcium in raffinate and magnesium precipitate, filter and obtain lithium salt solution.
Strong base solution is at least a in NaOH, potassium hydroxide.
The concentration of described sulfuric acid solution is 3～5mol/L.
The mass concentration of described hydrogen peroxide solution is 30～50%.
The temperature that leaches is 60～90 ℃.
Extract is that water and oil phase form, and in oil phase, the volumn concentration of P204 is 20～30%, and surplus is sulfonated kerosene.
The invention has the beneficial effects as follows: it is electrokinetic cell that recovery method of the present invention is applicable to all types of lithiums, the product of last gained is that purity is not less than 97.5% pure Lithium Carbonate, can directly apply to production, in the recycling process, without high-temperature process, energy consumption is lower.
Embodiment
A kind of method that reclaims lithium from lithium power battery of electric automobile comprises the following steps:
1) be that electrokinetic cell is pulverized with lithium, screening obtains powder;
2) the lower powder of sieve is put into container, is placed in the water bath with thermostatic control of 30～80 ℃, and adding mass percent in powder is that sodium hydroxide solution or the potassium hydroxide solution of 10-30% flooded 1～5 hour, and the oxide of dissolved aluminum and aluminium filters to get filter mud;
3) be that the mixed solution of 30～50% hydrogen peroxide solution leaches with the sulfuric acid solution of 3～5mol/L and mass concentration with filter mud, the ratio that institute adds liquid volume and filter mud solid masses is 4～6L:1kg, extraction temperature is 60～90 ℃, and extraction time is 1～4 hour, obtains at last leachate;
4) (extract is that oil phase and water form, and the volume ratio of water and oil phase is 4～1:1, in oil phase to add extract in leachate, the volumn concentration of P204 is 20～30%, surplus is sulfonated kerosene) carry out 3～15 stage countercurrent extractions, controlling pH is 1～4, gets raffinate;
5) pH with alkali lye adjusting raffinate is 3.0～8.0, and stirring reaction 1～2 hour is removed filter residue;
6) add the solid sodium fluoride to generating without precipitation in the raffinate of removing filter residue under stirring, remove by filter sediment and obtain lithium solution;
7) (solid sodium carbonate that adds and the mass ratio of the powder in step 1) are 0.3～0.35:1) to add solid sodium carbonate in the filtrate under stirring, obtain pure Lithium Carbonate solution, condensing crystallizing obtains pure Lithium Carbonate, Li in the pure Lithium Carbonate that obtains after crystallization
2CO
3Content greater than 97.5%, and meet national non-ferrous metal industry standard YS/T 582-2006 to the requirement of impurity in the battery lithium carbonate.
Below in conjunction with embodiment, further illustrate the present invention.
Embodiment 1
Be electrokinetic cell with waste and old lithium, pulverize, and with 80 purpose standard screens screenings, the powder 3kg that gets under sieve puts into container, is placed in water bath with thermostatic control, temperature arranges 50 ° of C, and adding mass concentration is 15% sodium hydroxide solution 12L, and the maintenance magnetic agitation was flooded 4 hours.Reacted rear filtration and used distilled water flushing, having obtained filter mud, to add molar concentration in mud be the sulfuric acid 10L of 3.0mol/L and 30% hydrogen peroxide 2L toward considering, and keeps 60 ° of C to leach 2 hours, and filtration obtains leachate.Preparation extract 20L, in extract, the volume ratio of water and oil phase is 4:1, and in oil phase, the volumn concentration of P204 is 25%, and surplus is sulfonated kerosene, uses extract to carry out 5 stage countercurrent extractions to leachate, and controlling the pH value is 4, obtains raffinate.Add NaOH in raffinate, regulating the pH value is 5.0, and stirring reaction removed by filter filter residue after 1 hour.Add the solid sodium fluoride to generating without precipitation in solution under stirring, remove by filter sediment.Add solid sodium carbonate 1kg in filtrate, obtain high purity lithium solution.Through condensing crystallizing, obtain pure Lithium Carbonate, Li in product
2CO
3Content reach 99.6%.
Embodiment 2:
Getting waste and old lithium is electrokinetic cell, pulverizes, and with 80 purpose standard screens screenings, gets the material powder 100g after sieving, and adding mass concentration is 20% sodium hydroxide solution 150ml, stirs 1 hour under the condition of 80 ° of C, filters and obtains filter mud, with the distilled water flushing several.Filter mud is placed in the 500mL beaker, and adding molar concentration is the sulfuric acid solution 350ml of 4.0mol/L, then adds 40% hydrogen peroxide 100ml, leaches 1 hour under 60 ° of C environment, filters and obtains leachate.Use the extract of 1.8L (in extract, the volume ratio of water and oil phase is 2:1, the volumn concentration that consists of of oil phase is that 25% P204 and volumn concentration are 75% sulfonated kerosene) leachate is carried out 5 stage countercurrents extractions, controlling pH is 1, obtain raffinate, add wherein ammoniacal liquor, controlling the pH value is 6, under agitation reacts after 1 hour to remove by filter sediment.Add the solid sodium fluoride until generate without precipitation again in filtrate, cross and filter to remove sediment.Add solid sodium carbonate 35g again in filtrate, through condensing crystallizing, obtain pure Lithium Carbonate, Li in product
2CO
3Content reach 99.7%.
Embodiment 3:
Getting waste and old lithium is electrokinetic cell, pulverizes, and with 80 purpose standard screens screenings, gets the material powder 200g after sieving, and adding mass concentration is 10% sodium hydroxide solution 600ml, stirs 5 hours under the condition of 30 ° of C, filters and obtains filter mud, with the distilled water flushing several.Filter mud is placed in the 500mL beaker, and adding molar concentration is the sulfuric acid solution 600ml of 5.0mol/L, then adds 50% hydrogen peroxide 200ml, leaches 1 hour under 90 ° of C environment, filters and obtains leachate.Use the extract of 3.6L (in extract, the volume ratio of water and oil phase is 1:1, the volumn concentration that consists of of oil phase is that 20% P204 and volumn concentration are 80% sulfonated kerosene) leachate is carried out 3 stage countercurrents extractions, controlling pH is 3, obtain raffinate, add wherein ammoniacal liquor, controlling the pH value is 7, under agitation reacts after 1 hour to remove by filter sediment.Add the solid sodium fluoride until generate without precipitation again in filtrate, cross and filter to remove sediment.Add solid sodium carbonate 60g again in filtrate, through condensing crystallizing, obtain pure Lithium Carbonate, Li in product
2CO
3Content reach 99.7%.
Embodiment 4:
Getting waste and old lithium is electrokinetic cell, pulverizes, and with 80 purpose standard screens screenings, gets the material powder 500g after sieving, and adding mass concentration is 30% sodium hydroxide solution 750ml, stirs 2 hours under the condition of 80 ° of C, filters and obtains filter mud, with the distilled water flushing several.Filter mud is placed in the 500mL beaker, and adding molar concentration is the sulfuric acid solution 1500ml of 5.0mol/L, then adds 50% hydrogen peroxide 500ml, leaches 1 hour under 70 ° of C environment, filters and obtains leachate.Use the extract of 9L (in extract, the volume ratio of water and oil phase is 4:1, the volumn concentration that consists of of oil phase is that 30% P204 and volumn concentration are 70% sulfonated kerosene) leachate is carried out 15 stage countercurrents extractions, controlling pH is 3, obtain raffinate, add wherein ammoniacal liquor, controlling the pH value is 8, under agitation reacts after 2 hours to remove by filter sediment.Add the solid sodium fluoride until generate without precipitation again in filtrate, cross and filter to remove sediment.Add solid sodium carbonate 150g again in filtrate, through condensing crystallizing, obtain pure Lithium Carbonate, Li in product
2CO
3Content reach 99.7%.
Claims (1)
1. method that reclaims lithium from lithium power battery of electric automobile comprises the following steps:
1) be that electrokinetic cell is pulverized with lithium, screening obtains powder;
2) the lower powder of sieve is put into container, is placed in the water bath with thermostatic control of 30～80 ℃, and adding mass percent in powder is that sodium hydroxide solution or the potassium hydroxide solution of 10-30% flooded 1～5 hour, and the oxide of dissolved aluminum and aluminium filters to get filter mud;
3) be that the mixed solution of 30～50% hydrogen peroxide solution leaches with the sulfuric acid solution of 3～5mol/L and mass concentration with filter mud, the ratio that institute adds liquid volume and filter mud solid masses is 4～6L:1kg, extraction temperature is 60～90 ℃, and extraction time is 1～4 hour, obtains at last leachate;
4) add extract to carry out 3～15 stage countercurrent extractions in leachate, controlling pH is 1～4, gets raffinate; Extract is that oil phase and water form, and the volume ratio of water and oil phase is 4～1:1, and in oil phase, the volumn concentration of P204 is 20～30%, and surplus is sulfonated kerosene;
5) pH with alkali lye adjusting raffinate is 3.0～8.0, and stirring reaction 1～2 hour is removed filter residue;
6) add the solid sodium fluoride to generating without precipitation in the raffinate of removing filter residue under stirring, remove by filter sediment and obtain lithium solution;
7) add solid sodium carbonate to obtain pure Lithium Carbonate solution in filtrate under stirring, condensing crystallizing obtains pure Lithium Carbonate; The solid sodium carbonate that adds and the mass ratio of the powder in step 1) are 0.3～0.35:1.
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| CN2011101476967A CN102244309B (en) | 2011-06-03 | 2011-06-03 | Method for recovering lithium from lithium power battery of electric automobile |
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| CN104124487B (en) * | 2014-07-25 | 2017-02-15 | 宁波卡尔新材料科技有限公司 | Method for recovering and extracting four metal elements including cobalt, copper, aluminum and lithium in waste lithium ion battery by using liquid phase reaction |
| CN104241724B (en) * | 2014-09-02 | 2017-04-05 | 湖南邦普循环科技有限公司 | A kind of method for preparing battery-level lithium carbonate from lithium ion battery regenerant |
| US11101507B2 (en) * | 2014-10-31 | 2021-08-24 | Albemarle Germany Gmbh | Process for recovering lithium from lithium-sulfur accumulators |
| CN104745823B (en) * | 2015-03-12 | 2017-03-22 | 湖南邦普循环科技有限公司 | Method for recycling lithium from waste lithium ion battery |
| CN105742744B (en) * | 2016-03-03 | 2017-10-31 | 中南大学 | A kind of method that lithium is extracted in the waste liquid containing lithium produced from waste and old lithium ion battery removal process |
| CN105932351A (en) * | 2016-05-16 | 2016-09-07 | 上海赛特康新能源科技股份有限公司 | Resource recycling method for waste lithium batteries |
| CN106229577A (en) * | 2016-08-23 | 2016-12-14 | 金川集团股份有限公司 | The method that the mixing of a kind of waste nickel hydrogen battery both positive and negative polarity material is leached |
| CN106229482A (en) * | 2016-08-23 | 2016-12-14 | 兰州金川新材料科技股份有限公司 | A kind of method preparing ternary precursor for raw material with nickel cobalt mixed solution |
| CN106558739B (en) * | 2016-11-28 | 2019-01-15 | 安徽得盈再生资源回收有限公司 | Separating technology is recycled based on lithium ion battery environment-friendly high-efficiency in waste mobile phone |
| CN106684486A (en) * | 2016-12-28 | 2017-05-17 | 天津先众新能源科技股份有限公司 | Method for extracting lithium from waste lithium iron phosphate |
| CN107083484A (en) * | 2017-04-20 | 2017-08-22 | 常州市鼎日环保科技有限公司 | A kind of method that metal is reclaimed from waste lithium cell |
| CN107910612B (en) * | 2017-12-06 | 2020-04-14 | 贵州红星电子材料有限公司 | Method for recovering cobalt and nickel from waste lithium batteries |
| CN110323511B (en) * | 2019-07-10 | 2021-10-26 | 长园泽晖新能源材料研究院(珠海)有限公司 | Chemical method for treating waste lithium battery system and waste lithium battery treatment method |
| CN114772565A (en) * | 2022-04-28 | 2022-07-22 | 西南科技大学 | Method for recovering lithium dihydrogen phosphate from leachate of phosphoric acid system of waste lithium iron phosphate battery |
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| CN1055563C (en) * | 1995-01-06 | 2000-08-16 | 中南工业大学 | Method for prepn. of magnetic materials |
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