CN102244309A - 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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- CN102244309A CN102244309A CN2011101476967A CN201110147696A CN102244309A CN 102244309 A CN102244309 A CN 102244309A CN 2011101476967 A CN2011101476967 A CN 2011101476967A CN 201110147696 A CN201110147696 A CN 201110147696A CN 102244309 A CN102244309 A CN 102244309A
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- raffinate
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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 is the method that reclaims lithium the electrokinetic cell from the electric automobile lithium.
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 main lithium-ion-power cell manufacturing enterprise in the whole world has begun to invest layout, concentrate on 2009～went into operation in 2010, China's lithium ion battery output in 2009 is 18.75 hundred million (about 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 (about 57200 tons), when the time comes, the production capacity of the cobalt of lithium-ion-power cell resource will reach 11440 tons, promptly be equivalent to the exploitation of a large-scale nonferrous metal mine.Production practices both domestic and external show: 1 ton of primary non-ferrous 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%.
Because the existing harm of waste and old electrokinetic cell self and its value that is rich in non-ferrous metal have received more and more people's concern, the recovery of the cobalt in the lithium ion battery, nickel, manganese has begun industrialization, but has defectives such as process program energy consumption height, cost height, economic benefit are not remarkable, industrialization value is little for the present employed method 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 the 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 behind the extracting copper is added extractant extraction cobalt.This method needs high-temperature calcination, and the energy consumption height very easily causes secondary pollution.
As the disclosed preparation Li that from waste and old lithium ion battery, reclaims of CN1747224A
xCoCO
2Method, the positive electrode of lithium battery is shredded, bubble is in N-N-methyl-2-2-pyrrolidone N-liquid, cobalt acid lithium powder is isolated in heating.Add nitric acid or hydrochloric acid and leach Co
2+And Li
+Ion adds the heavy Co that makes of ammoniacal liquor
2+Precipitation adds surfactant and LiOH simultaneously and adjusts Li
+Concentration.Obtain suspension.Filter out at last in the suspension sediment and at 600 ℃ ~ 900 ℃ roasting temperature, obtain Li
xCoCO
2Powder.This method needs high-temperature roasting energy consumption height, very easily causes secondary pollution, simultaneously, does not have the removal of impurities process in the technology, and product impurity is many, and quality is difficult to guarantee.
And for example CN101519726 discloses the method that a kind of roasting direct is handled waste and old lithium ion battery and reclaimed valuable metal, particularly at being the recycling of the waste and old lithium ion battery of positive electrode with cobalt acid lithium.At first remove the organic binder bond on the organic diaphragm material and electrode material in the battery at 500～850 ℃ of roasting temperatures, to size mixing through mixing with sodium sulphate (or potassium sulfate), the concentrated sulfuric acid after the battery material fragmentation of roasting, in electric furnace, carry out secondary heat treatment under 350～600 ℃ of temperature, making the metallic transitions such as cobalt, copper and lithium in the waste and old lithium ion battery is sulfate soluble in water, after water or dilution heat of sulfuric acid leach, from leachate, extract cobalt, copper respectively with organic extractant 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 handles hot secondary heat treatment material.This method exists energy consumption big equally, can cause shortcomings such as secondary pollution.
In addition, in the existing recovery technology, only the lithium electricity at single type reclaims, for example cobalt acid lithium, LiMn2O4 etc., to other positive electrode and inapplicable, and the elements such as lithium that reclaim, purity is generally lower, need 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 is the method that reclaims lithium the electrokinetic cell from the electric automobile lithium.
The technical solution used in the present invention is:
A kind of is the method that reclaims lithium the electrokinetic cell from the electric automobile lithium, may further comprise the steps:
With lithium is that electrokinetic cell is pulverized, and obtains powder;
In powder, add strong base solution, the oxide of dissolved aluminum and aluminium, filter 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 the raffinate;
In raffinate, add water-soluble villiaumite,, filter and obtain lithium salt solution calcium in the raffinate and magnesium precipitate.
Strong base solution is at least a in NaOH, the 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 are formed, and in oil phase, the volumn concentration of P204 is 20～30%, and surplus is a sulfonated kerosene.
The invention has the beneficial effects as follows: recovery method of the present invention is applicable to that all types of lithiums are electrokinetic cell, the product of last gained is that purity is not less than 97.5% pure Lithium Carbonate, can directly apply to production, not have high-temperature process in the recycling process, energy consumption is lower.
Embodiment
A kind of is the method that reclaims lithium the electrokinetic cell from the electric automobile lithium, may further comprise the steps:
1) be that electrokinetic cell is pulverized with lithium, screening obtains powder;
2) sieve powder is down put into container, places 30～80 ℃ water bath with thermostatic control, in powder, add sodium hydroxide solution or the potassium hydroxide solution that mass percent is 10-30% and flooded 1～5 hour, the oxide of dissolved aluminum and aluminium, filter filter mud;
3) be that the mixed solution of 30～50% hydrogen peroxide solution leaches with filter mud with the sulfuric acid solution of 3～5mol/L and mass concentration, 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 leachate at last;
4) (extract is that oil phase and water are formed, and the volume ratio of water and oil phase is 4～1:1, in the oil phase to add extract in leachate, the volumn concentration of P204 is 20～30%, surplus is a sulfonated kerosene) carry out the extraction of 3～15 stage countercurrents, control 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) under stirring, in the raffinate of removing filter residue, add the solid sodium fluoride and do not generate, remove by filter sediment and obtain lithium solution to there being precipitation;
7) (solid sodium carbonate of adding and the mass ratio of the powder in the step 1) are 0.3～0.35:1) to add solid sodium carbonate under stirring in filtrate, obtain pure Lithium Carbonate solution, condensing crystallizing obtains pure Lithium Carbonate, Li in the pure Lithium Carbonate that obtains after the crystallization
2CO
3Content greater than 97.5%, and meet the requirement of national non-ferrous metal industry standard YS/T 582-2006 to impurity in the battery lithium carbonate.
Below in conjunction with embodiment, further specify the present invention.
Embodiment 1
With waste and old lithium is electrokinetic cell, pulverizes, and sieves with 80 purpose standard screens, and the powder 3kg that gets under the sieve puts into container, places water bath with thermostatic control, and temperature is provided with 50 ° of C, and the adding mass concentration is 15% sodium hydroxide solution 12L, keeps magnetic agitation, floods 4 hours.Reacted the back filtration and used distilled water flushing, obtained filter mud, the adding molar concentration is the sulfuric acid 10L of 3.0mol/L and 30% hydrogen peroxide 2L in the mud toward considering, and keeps 60 ° of C to leach 2 hours, filters and obtains leachate.Preparation extract 20L, in the extract, the volume ratio of water and oil phase is 4:1, and in the oil phase, the volumn concentration of P204 is 25%, and surplus is a sulfonated kerosene, uses extract that leachate is carried out the extraction of 5 stage countercurrents, and control 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.Under stirring, in solution, add the solid sodium fluoride, remove by filter sediment to there not being the precipitation generation.In filtrate, add solid sodium carbonate 1kg, obtain high purity lithium solution.Through condensing crystallizing, obtain pure Lithium Carbonate, Li in the product
2CO
3Content reach 99.6%.
Embodiment 2:
Getting waste and old lithium is electrokinetic cell, pulverizes, and with the screening of 80 purpose standard screens, gets the material powder 100g after sieving, and the 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 distilled water flushing for several times.Filter mud is placed the 500mL beaker, and adding molar concentration is the sulfuric acid solution 350ml of 4.0mol/L, adds 40% hydrogen peroxide 100ml again, leaches 1 hour under 60 ° of C environment, filters and obtains leachate.The extract that uses 1.8L is (in the 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 the extraction of 5 stage countercurrents, control pH is 1, obtain raffinate, to wherein adding ammoniacal liquor, control pH value is 6, under agitation reacts after 1 hour to remove by filter sediment.In filtrate, add the solid sodium fluoride again and do not generate, cross and filter to remove sediment until there being precipitation.In filtrate, add solid sodium carbonate 35g again,, obtain pure Lithium Carbonate, Li in the product through condensing crystallizing
2CO
3Content reach 99.7%.
Embodiment 3:
Getting waste and old lithium is electrokinetic cell, pulverizes, and with the screening of 80 purpose standard screens, gets the material powder 200g after sieving, and the 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 distilled water flushing for several times.Filter mud is placed the 500mL beaker, and adding molar concentration is the sulfuric acid solution 600ml of 5.0mol/L, adds 50% hydrogen peroxide 200ml again, leaches 1 hour under 90 ° of C environment, filters and obtains leachate.The extract that uses 3.6L is (in the 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 the extraction of 3 stage countercurrents, control pH is 3, obtain raffinate, to wherein adding ammoniacal liquor, control pH value is 7, under agitation reacts after 1 hour to remove by filter sediment.In filtrate, add the solid sodium fluoride again and do not generate, cross and filter to remove sediment until there being precipitation.In filtrate, add solid sodium carbonate 60g again,, obtain pure Lithium Carbonate, Li in the product through condensing crystallizing
2CO
3Content reach 99.7%.
Embodiment 4:
Getting waste and old lithium is electrokinetic cell, pulverizes, and with the screening of 80 purpose standard screens, gets the material powder 500g after sieving, and the 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 distilled water flushing for several times.Filter mud is placed the 500mL beaker, and adding molar concentration is the sulfuric acid solution 1500ml of 5.0mol/L, adds 50% hydrogen peroxide 500ml again, leaches 1 hour under 70 ° of C environment, filters and obtains leachate.The extract that uses 9L is (in the 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 the extraction of 15 stage countercurrents, control pH is 3, obtain raffinate, to wherein adding ammoniacal liquor, control pH value is 8, under agitation reacts after 2 hours to remove by filter sediment.In filtrate, add the solid sodium fluoride again and do not generate, cross and filter to remove sediment until there being precipitation.In filtrate, add solid sodium carbonate 150g again,, obtain pure Lithium Carbonate, Li in the product through condensing crystallizing
2CO
3Content reach 99.7%.
Claims (6)
1. one kind is the method that reclaims lithium the electrokinetic cell from the electric automobile lithium, may further comprise the steps:
With lithium is that electrokinetic cell is pulverized, and obtains powder;
In powder, add strong base solution, the oxide of dissolved aluminum and aluminium, filter 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 the raffinate;
In raffinate, add water-soluble villiaumite,, filter and obtain lithium salt solution calcium in the raffinate and magnesium precipitate.
2. according to claim 1 a kind of be the method that reclaims lithium the electrokinetic cell from the electric automobile lithium, it is characterized in that: strong base solution is at least a in NaOH, the potassium hydroxide.
3. according to claim 1 a kind of be the method that reclaims lithium the electrokinetic cell from the electric automobile lithium, it is characterized in that: the concentration of described sulfuric acid solution is 3～5mol/L.
4. according to claim 1 a kind of be the method that reclaims lithium the electrokinetic cell from the electric automobile lithium, it is characterized in that: the mass concentration of described hydrogen peroxide solution is 30～50%.
5. according to claim 1 a kind of be the method that reclaims lithium the electrokinetic cell from the electric automobile lithium, it is characterized in that: the temperature of leaching is 60～90 ℃.
6. according to claim 1 a kind of be the method that reclaims lithium the electrokinetic cell from the electric automobile lithium, it is characterized in that: extract is that water and oil phase are formed, and in oil phase, the volumn concentration of P204 is 20～30%, and surplus is a sulfonated kerosene.
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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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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104124487A (en) * | 2014-07-25 | 2014-10-29 | 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 |
| CN104241724A (en) * | 2014-09-02 | 2014-12-24 | 湖南邦普循环科技有限公司 | Method for preparing battery-grade lithium carbonate from recycled lithium ion battery material |
| CN104745823A (en) * | 2015-03-12 | 2015-07-01 | 湖南邦普循环科技有限公司 | Method for recycling lithium from waste lithium ion battery |
| CN105742744A (en) * | 2016-03-03 | 2016-07-06 | 中南大学 | Method for extracting lithium from lithium-containing liquid waste generated in waste lithium-ion battery recycling 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 |
| CN106558739A (en) * | 2016-11-28 | 2017-04-05 | 安徽得盈再生资源回收有限公司 | Separating technology is reclaimed 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 |
| CN107910612A (en) * | 2017-12-06 | 2018-04-13 | 贵州红星电子材料有限公司 | A kind of method of the Call Provision nickel from waste lithium cell |
| CN110323511A (en) * | 2019-07-10 | 2019-10-11 | 泽晖新能源材料研究院(珠海)有限公司 | Chemical method disposes waste lithium cell system and waste lithium battery treatment |
| US11101507B2 (en) * | 2014-10-31 | 2021-08-24 | Albemarle Germany Gmbh | Process for recovering lithium from lithium-sulfur accumulators |
| 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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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104124487A (en) * | 2014-07-25 | 2014-10-29 | 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 |
| CN104241724A (en) * | 2014-09-02 | 2014-12-24 | 湖南邦普循环科技有限公司 | Method for preparing battery-grade lithium carbonate from recycled lithium ion battery material |
| US11101507B2 (en) * | 2014-10-31 | 2021-08-24 | Albemarle Germany Gmbh | Process for recovering lithium from lithium-sulfur accumulators |
| CN104745823A (en) * | 2015-03-12 | 2015-07-01 | 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 |
| CN105742744A (en) * | 2016-03-03 | 2016-07-06 | 中南大学 | Method for extracting lithium from lithium-containing liquid waste generated in waste lithium-ion battery recycling 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 |
| CN106558739A (en) * | 2016-11-28 | 2017-04-05 | 安徽得盈再生资源回收有限公司 | Separating technology is reclaimed 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 |
| CN107910612A (en) * | 2017-12-06 | 2018-04-13 | 贵州红星电子材料有限公司 | A kind of method of the Call Provision nickel 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 |
| CN110323511A (en) * | 2019-07-10 | 2019-10-11 | 泽晖新能源材料研究院(珠海)有限公司 | Chemical method disposes waste lithium cell system and waste lithium battery treatment |
| 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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