CN108011150A - A kind of method that lithium carbonate is produced from waste and old ternary lithium ion cell electrode powder - Google Patents
A kind of method that lithium carbonate is produced from waste and old ternary lithium ion cell electrode powder Download PDFInfo
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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Abstract
The present invention relates to the recovery process of waste and old ternary lithium ion battery, a kind of more particularly to method that lithium carbonate is produced from waste and old ternary lithium ion cell electrode powder, this method passes through to the electrode powder batch mixing of waste and old ternary lithium ion battery, calcining, generation lithium bicarbonate and spray drying step, obtained carbonic acid lithium content is higher, purity is higher, the rate of recovery is high, and the process route is environmentally protective technique, and being compatible with the environment property is preferable.
Description
Technical field
The present invention relates to the recovery process of waste and old ternary lithium ion battery, more particularly to it is a kind of from waste and old ternary lithium-ion electric
The method that lithium carbonate is produced in the electrode powder of pond.
Background technology
The recovery technology of waste and old lithium ion battery is mainly liquid phase method and solid phase method.Liquid phase method need using substantial amounts of acid and
Alkali, not only cost is higher, but also environment can be polluted, and the Chinese patent literature such as Publication No. CN 101871048A is public
A kind of method of Call Provision from waste and old lithium ion battery, nickel and manganese is opened：Waste lithium ion cell anode material is immersed low
In concentration lye, nonreactive cathode black powder is recycled, low concentration acid dissolving is first carried out to the black powder of recycling, then use
Na2SO5、Na2SO3Or Fe powder enrichings sulfuric acid carries out reduction of dissolved, is finally dissolved in high concentrated acid.Obtained material is consolidated
After liquid separation, using P2O4And P5O7Extractant extracts respective metal, improves the purity of recycling metal, but whole
In a flow, the use of extractant can produce a large amount of organic liquid wastes, and larger harm is caused to environment.For another example Publication No. CN
The Chinese patent literature of 105633500A, which discloses, a kind of prepares tertiary cathode material forerunner using recycling lithium ion battery material
The method of body：With sulfuric acid and hydrogen peroxide dissolving recycling anode material for lithium-ion batteries, leachate is obtained, filter aid is added and goes
Except impurity, then add nickel sulfate, cobalt sulfate and/or mn sulphate, and adjust nickel, cobalt, manganese molar ratio for (0.4 ~
0.6) : (0.1~0.3) :(0.2 ~ 0.4), obtains corresponding solution, and complex precipitant is added into the solution and adjusts solution
PH obtain nickel-cobalt-manganese ternary material precursor precipitation, washed and be dried to obtain ternary anode material precursor；The patent
It make use of the precipitation method to be prepared for corresponding ternary anode material precursor, but effective solution do not suggested that for remaining liquid containing lithium
Certainly measure, stills need the addition of lithium salts in follow-up positive electrode preparation process, while this method is removed using precipitation filtration method
It is miscellaneous, do not efficiently use metallic element therein.Solid phase method can not only discharge substantial amounts of dust in removal process, but also recycle
Product purity it is relatively low, be not suitable for high-quality recycling and profit it is smaller.
The solid phase method of comparative maturity is at present：Waste and old lithium ion battery is burned into organics removal, grinding screen selects big portion
Divide iron and small part copper, aluminium is removed with lye, add acid and hydrogen peroxide or sodium sulfite does reducing agent leaching valuable metal, then
Chemical method is taken tentatively to clean, abstraction impurity removal separation nickel cobalt, crystallizes to obtain nickel product, cobalt product.This method mainly has the disadvantage that：
（1）Contain more than 2% nickel, cobalt and manganese in the most of iron and small part copper of screening, cause the rate of recovery of nickel cobalt manganese low；
（2）Aluminium in battery and the most copper do not selected can consume substantial amounts of auxiliary material, cause of high cost；
（3）Add hydrogen peroxide or sodium sulfite to make reducing agent in leaching process, not only add cost, but also cause pollution.
The content of the invention
It is an object of the invention to overcome it is existing recycling waste and old lithium ion battery during produce pollution and the rate of recovery compared with
Low problem, and a kind of method that lithium carbonate is extracted from waste and old ternary lithium ion cell electrode mixed powder is provided, the party
Method technique is simple, and organic efficiency is high, and being compatible with the environment property is preferable, so as to reach the recycling target of green high-efficient.
The technical solution adopted by the present invention is as follows：One kind extracts carbon from waste and old ternary lithium ion cell electrode mixed powder
The method of sour lithium, comprises the following steps：
（1）Batch mixing
Waste and old ternary lithium ion battery is dismantled, battery positive pole powder material after dismounting and anode powder body material are mixed
Close, ball milling is carried out to mixed powder, ratio of grinding media to material is（5~20）:1, rotational speed of ball-mill is in 100 more than r/min, Ball-milling Time
In 0.1 more than h, it is uniformly mixed the powder after refinement；
（2）Calcining
By step（1）In mixed powder calcined in high-temperature vacuum furnace, the vacuum pressure scope of high-temperature vacuum furnace for-
0.1 MPA of MPa to -0.05, heating rate are 5 ~ 20 DEG C/min, and for calcining heat at 500 ~ 900 DEG C, calcination time is 1 ~ 6
H, stops that material is naturally cooled to environment temperature after calcining；
The chemical equation of the step is：Li(NixCoyMnz)O2 + C → Li2CO3 + xNi + yCo + zMnO +
CO2↑；
（3）Generate lithium bicarbonate
By step（2）Powder immersion stirring after middle calcining, solid-liquid mass ratio 1:(10 ~ 100), after stirring evenly, are passed through two
Carbonoxide reacts with lithium carbonate and water, and carbon dioxide is passed through speed and is not less than 0.5 L/min, and it is water-soluble to obtain lithium bicarbonate
Liquid, filters solution, and filtration apparatus aperture is not less than 200 mesh, and the solution after filtering is stood, and makes little particle insoluble
Thing fully precipitates；
The chemical equation of the step is：Li2CO3 + CO2 + H2O → LiHCO3；
（4）Spray drying
To step（3）In the solution that is obtained by filtration be spray-dried, due to lithium bicarbonate under the conditions of heat drying it is unstable,
Therefore pure lithium carbonate solid can be obtained.
Chemical equation in the step is：LiHCO3 → Li2CO3 + CO2↑+ H2O。
Preferably, step（1）In waste and old ternary lithium ion battery positive pole powder material include ternary active material, bonding
Agent and conductive carbon, the anode powder body material include graphite, binding agent and thickener.
Preferably, step（1）Middle ball milling ratio is（10~20）：1, rotational speed of ball-mill is 250 ~ 500 r/min, and Ball-milling Time is
0.1h~1h。
Preferably, step（2）The heating rate of middle high-temperature vacuum furnace is 5 ~ 10 DEG C/min.
Preferably, step（2）Middle calcining heat is 600 ~ 800 DEG C, and calcination time is 4 ~ 6h.
Preferably, step（3）Solid-liquid mass ratio after middle powder immersion is 1：（50~100）.
Preferably, step（3）It is 0.5 ~ 1.5 L/min that middle carbon dioxide, which is passed through speed,.
Preferably, step（3）In filtration apparatus aperture be 200 ~ 300 mesh.
Preferably, step（4）The yield of middle lithium carbonate is 19 ~ 21%.
Preferably, this method is 88 ~ 91% to the rate of recovery of elemental lithium after the processing of waste and old ternary lithium ion battery.
The invention has the advantages that：The invention discloses one kind from waste and old ternary lithium ion cell electrode powder
The method for producing lithium carbonate, this method new technology, design is reasonable, passes through batch mixing, calcining, dissolution filter and spray drying step
Lithium carbonate in waste and old ternary lithium ion cell electrode powder is extracted, the carbonic acid lithium content extracted is higher, purity
Higher, the rate of recovery is high, which is environmentally protective technique, and being compatible with the environment property is preferable.
Brief description of the drawings
Fig. 1 is the process flow chart of the present invention.
Fig. 2 is Li produced by the present invention2CO3XRD spectrum.
Embodiment
Embodiments of the present invention are described further below in conjunction with the accompanying drawings.
Embodiment 1：It is a kind of from waste and old Li (Ni1/3Co1/3Mn1/3)O2Carbonic acid is produced in ternary lithium ion cell electrode powder
The method of lithium, as shown in Figure 1, comprising the following steps：
（1）Batch mixing
By waste and old Li (Ni1/3Co1/3Mn1/3)O2The electrode powder of ternary lithium ion battery carries out dry mixed, and electrode powder is by just
Pole powder and anode powder composition, positive mix include ternary active material, binding agent and conductive carbon, and anode powder body material includes
Graphite, binding agent and thickener.Mixed powder is subjected to mechanical ball mill, ball material mass ratio is 10:1, rotating speed 250
R/min, Ball-milling Time are 0.5 h, are uniformly mixed it；
（2）Calcining
By step（1）In mixed powder calcined in high-temperature vacuum furnace, the vacuum pressure scope of high-temperature vacuum furnace for-
0.1 MPa, heating rate are 10 DEG C/min, and for calcining heat at 600 DEG C, calcination time is 6 h, after stopping calcining by material certainly
So it is cooled to environment temperature；The chemical equation of the step is：Li(NixCoyMnz)O2 + C → Li2CO3 + xNi +
yCo + zMnO + CO2↑；
（3）Generate lithium bicarbonate
By step（2）Powder immersion stirring after middle calcining, solid-liquid mass ratio 1:10, after mixing, it is passed through titanium dioxide
Carbon reacts with lithium carbonate and water, and it is 0.5 L/min that carbon dioxide, which is passed through speed, lithium bicarbonate aqueous solution is obtained, to solution
Filtered, filtration apparatus aperture is not less than 200 mesh, and the solution after filtering is stood, and makes the little particle in solution insoluble
Thing is precipitated；The chemical equation of the step is：Li2CO3 + CO2 + H2O → LiHCO3；
（4）Spray drying
To step（3）In the solution that is obtained by filtration be spray-dried, due to lithium bicarbonate under the conditions of heat drying it is unstable,
Therefore can decompose in heat drying process lithium carbonate, you can obtain pure lithium carbonate solid；Chemistry in the step is anti-
The equation is answered to be：LiHCO3 → Li2CO3 + CO2↑+ H2O。
Embodiment 2：It is a kind of from waste and old Li (Ni0.5Co0.2Mn0.3)O2Carbonic acid is produced in ternary lithium ion cell electrode powder
The method of lithium, as shown in Figure 1, comprising the following steps：
（1）Batch mixing
By waste and old Li (Ni0.5Co0.2Mn0.3)O2The electrode powder of ternary lithium ion battery carries out dry mixed, and electrode powder is by just
Pole powder and anode powder composition, positive mix include ternary active material, binding agent and conductive carbon, and anode powder body material includes
Graphite, binding agent and thickener.Mixed powder carries out mechanical ball mill, and ball material mass ratio is 20:1, rotating speed is 100 r/
Min, Ball-milling Time are 1 h, are uniformly mixed it；
（2）Calcining
By step（1）In mixed powder calcined in high-temperature vacuum furnace, the vacuum pressure scope of high-temperature vacuum furnace for-
0.05 MPa, heating rate are 5 DEG C/min, and for calcining heat at 800 DEG C, calcination time is 4 h, after stopping calcining by material certainly
So it is cooled to environment temperature；The chemical equation of the step is：Li(NixCoyMnz)O2 + C → Li2CO3 + xNi +
yCo + zMnO + CO2↑；
（3）Generate lithium bicarbonate
By step（2）Powder immersion stirring after middle calcining, solid-liquid mass ratio 1:50, after mixing, it is passed through carbon dioxide
React with lithium carbonate and water, it is 1 L/min that carbon dioxide, which is passed through speed, obtains lithium bicarbonate aqueous solution, to mixture into
Row filtering, filtration apparatus aperture is 300 mesh, and the solution after filtering is stood, and makes the little particle insoluble in solution fully heavy
Form sediment；The chemical equation of the step is：Li2CO3 + CO2 + H2O → LiHCO3；
（4）Spray drying
To step（3）In the solution that is obtained by filtration be spray-dried, due to lithium bicarbonate under the conditions of heat drying it is unstable,
Therefore can decompose in heat drying process lithium carbonate, you can obtain pure lithium carbonate solid；Chemistry in the step is anti-
The equation is answered to be：LiHCO3 → Li2CO3 + CO2↑+ H2O。
Embodiment 3：It is a kind of from waste and old Li (Ni0.7Co0.15Mn0.15)O2Carbonic acid is produced in ternary lithium ion cell electrode powder
The method of lithium, as shown in Figure 1, comprising the following steps：
（1）Batch mixing
By waste and old Li (Ni0.7Co0.15Mn0.15)O2The electrode powder of ternary lithium ion battery carries out dry mixed, electrode powder by
Positive mix and anode powder composition, positive mix include ternary active material, binding agent and conductive carbon, anode powder body material bag
Include graphite, binding agent and thickener.Mixed powder carries out mechanical ball mill, and ball material mass ratio is 5:1, rotating speed is 500 r/
Min, Ball-milling Time are 0.1 h, are uniformly mixed it；
（2）Calcining
By step（1）In mixed powder calcined in high-temperature vacuum furnace, the vacuum pressure scope of high-temperature vacuum furnace for-
0.1 MPa, heating rate are 10 DEG C/min, and for calcining heat at 700 DEG C, calcination time is 5 h, after stopping calcining by material certainly
So it is cooled to environment temperature；The chemical equation of the step is：Li(NixCoyMnz)O2 + C → Li2CO3 + xNi +
yCo + zMnO + CO2↑；
（3）Generate lithium bicarbonate
By step（2）Powder immersion stirring after middle calcining, solid-liquid mass ratio 1:100, after mixing, it is passed through titanium dioxide
Carbon reacts with lithium carbonate and water, and it is 1.5 L/min that carbon dioxide, which is passed through speed, obtains lithium bicarbonate aqueous solution, to mixing
Thing is filtered, and filtration apparatus aperture is 200 mesh, and the solution after filtering is stood, and fills the little particle insoluble in solution
Fractional precipitation；
（4）Spray drying
To step（3）In the solution that is obtained by filtration be spray-dried, due to lithium bicarbonate under the conditions of heat drying it is unstable,
Therefore can decompose in heat drying process lithium carbonate, you can obtain pure lithium carbonate solid；Chemistry in the step is anti-
The equation is answered to be：LiHCO3 → Li2CO3 + CO2↑+ H2O。
Description of test：In three above embodiment, embodiment 3 is most preferred embodiment, is to embodiment 1, embodiment 2 below
With the experimental analysis of the lithium carbonate finished product of embodiment 3：
1st, the carbonic acid reason finished product that embodiment 1-3 is made is by X-ray diffraction analysis test result referring to Figure of description 2：
Li in the diffraction maximum of lithium carbonate made from embodiment 1,2 and 3 and standard PDF cards2CO3Diffraction maximum match completely,
And exist without the diffraction maximum of other impurities, accordingly, it can be determined that by the method for the present invention to from waste and old ternary lithium ion battery
The lithium carbonate purity produced in electrode powder is higher.
2nd, result of the lithium carbonate made from embodiment 1-3 by elemental analysis test is as follows：
| Embodiment | Li | Ni | Co | Mn | Cu | Al |
| 1 | 84.91% | 2.02% | 1.92% | 7.13% | 0.51% | 3.51% |
| 2 | 84.63% | 3.43% | 1.31% | 6.52% | 0.54% | 3.57% |
| 3 | 85.87% | 4.96% | 0.93% | 4.01% | 0.51% | 3.72% |
It follows that 85% is accounted for by the content of elemental lithium in lithium carbonate made from the method for the present invention, nickel element, cobalt element, manganese
The content of element, copper and aluminium element is very low, further proves the method by the present invention to from waste and old ternary lithium ion
The lithium carbonate purity produced in battery electrode powder is higher.
3rd, in embodiment 1-3 the rate of recovery of elemental lithium and electrode powder produce lithium carbonate yield results it is as follows：
| Embodiment | Li | Li2CO3 |
| Embodiment 1 | 88.95% | 19.32% |
| Embodiment 2 | 89.33% | 19.43% |
| Embodiment 3 | 90.05% | 20.16% |
It follows that the elemental lithium in waste and old ternary lithium ion cell electrode powder is effectively recycled by the method for the present invention,
The rate of recovery reaches more than 88.95%, and the yield of lithium carbonate reaches more than 19%, and therefore, method of the invention can be efficiently to useless
Elemental lithium in old ternary lithium ion battery is recycled, and the lithium carbonate yield that extraction obtains is higher.
Claims (10)
- A kind of 1. method that lithium carbonate is produced from waste and old ternary lithium ion cell electrode powder, it is characterised in that：Including following Step：（1）Batch mixingWaste and old ternary lithium ion battery is dismantled, battery positive pole powder material after dismounting and anode powder body material are mixed Close, ball milling is carried out to mixed powder, ratio of grinding media to material is（5~20）:1, rotational speed of ball-mill is 100 more than r/min, Ball-milling Time For 0.1 more than h, it is uniformly mixed the powder after refinement；（2）CalciningBy step（1）In mixed powder calcined in high-temperature vacuum furnace, the vacuum pressure scope of high-temperature vacuum furnace for- 0.1 MPa of MPa to -0.05, heating rate are 5 ~ 20 DEG C/min, and for calcining heat at 500 ~ 900 DEG C, calcination time is 1 ~ 6 H, stops that material is naturally cooled to environment temperature after calcining；The chemical equation of the step is：Li(NixCoyMnz)O2 + C → Li2CO3 + xNi + yCo + zMnO + CO2↑；（3）Generate lithium bicarbonateBy step（2）Powder immersion stirring after middle calcining, solid-liquid mass ratio 1:(10 ~ 100), after stirring evenly, are passed through two Carbonoxide reacts with lithium carbonate and water, and carbon dioxide is passed through speed and is not less than 0.5 L/min, and it is water-soluble to obtain lithium bicarbonate Liquid, filters solution, and filtration apparatus aperture is not less than 200 mesh, and the solution after filtering is stood, is made in solution Little particle insoluble is precipitated；The chemical equation of the step is：Li2CO3 + CO2 + H2O → LiHCO3；（4）Spray dryingTo step（3）In the solution that is obtained by filtration be spray-dried, you can obtain pure lithium carbonate solid；Chemical equation in the step is：LiHCO3 → Li2CO3 + CO2↑+ H2O。
- 2. a kind of method that lithium carbonate is produced from waste and old ternary lithium ion cell electrode powder according to claim 1, It is characterized in that：Step（1）In waste and old ternary lithium ion battery positive pole powder material include ternary active material, binding agent and Conductive carbon, the anode powder body material include graphite, binding agent and thickener.
- 3. a kind of method that lithium carbonate is produced from waste and old ternary lithium ion cell electrode powder according to claim 1, It is characterized in that：Step（1）Middle ball milling ratio is（5~20）：1, rotational speed of ball-mill is 250 ~ 500 r/min, Ball-milling Time for 0.1h ~ 1h。
- 4. a kind of method that lithium carbonate is produced from waste and old ternary lithium ion cell electrode powder according to claim 1, It is characterized in that：Step（2）The heating rate of middle high-temperature vacuum furnace is 5 ~ 10 DEG C/min.
- 5. a kind of method that lithium carbonate is produced from waste and old ternary lithium ion cell electrode powder according to claim 1, It is characterized in that：Step（2）Middle calcining heat is 600 ~ 800 DEG C, and calcination time is 4 ~ 6h.
- 6. a kind of method that lithium carbonate is produced from waste and old ternary lithium ion cell electrode powder according to claim 1, It is characterized in that：Step（3）Solid-liquid mass ratio after middle powder immersion is 1：（50~100）.
- 7. a kind of method that lithium carbonate is produced from waste and old ternary lithium ion cell electrode powder according to claim 1, It is characterized in that：Step（3）It is 0.5 ~ 1.5 L/min that middle carbon dioxide, which is passed through speed,.
- 8. a kind of method that lithium carbonate is produced from waste and old ternary lithium ion cell electrode powder according to claim 1, It is characterized in that：Step（3）In filtration apparatus aperture be 200 ~ 300 mesh.
- 9. a kind of method that lithium carbonate is produced from waste and old ternary lithium ion cell electrode powder according to claim 1, It is characterized in that：Step（4）The yield of middle lithium carbonate is 19 ~ 21%.
- 10. a kind of method that lithium carbonate is produced from waste and old ternary lithium ion cell electrode powder according to claim 1, It is characterized in that：This method is 88 ~ 91% to the rate of recovery of elemental lithium after the processing of waste and old ternary lithium ion battery.
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| CN108760586A (en) * | 2018-05-23 | 2018-11-06 | 广州能源检测研究院 | A kind of method that overlay material particle size is distributed in detection lithium battery pole slice |
| CN108808155A (en) * | 2018-08-17 | 2018-11-13 | 湖南金凯循环科技有限公司 | A method of by waste lithium ion cell anode material preparation battery-level lithium carbonate |
| CN108933308A (en) * | 2018-07-13 | 2018-12-04 | 江西环锂新能源科技有限公司 | A kind of comprehensive reutilization method for scrapping lithium battery positive and negative anodes |
| CN110029226A (en) * | 2019-05-05 | 2019-07-19 | 中南大学 | One kind recycling valuable metal method from waste and old ternary lithium ion anode material |
| CN110029225A (en) * | 2019-05-05 | 2019-07-19 | 浙江省冶金研究院有限公司 | One kind recycling valuable metal method from waste and old ternary anode material for lithium-ion batteries |
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| CN108760586A (en) * | 2018-05-23 | 2018-11-06 | 广州能源检测研究院 | A kind of method that overlay material particle size is distributed in detection lithium battery pole slice |
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| CN110029226A (en) * | 2019-05-05 | 2019-07-19 | 中南大学 | One kind recycling valuable metal method from waste and old ternary lithium ion anode material |
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| CN110029226B (en) * | 2019-05-05 | 2020-11-24 | 中南大学 | Method for recycling valuable metal from waste ternary lithium ion positive electrode material |
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| CN111825110A (en) * | 2020-05-12 | 2020-10-27 | 宁夏百川新材料有限公司 | Recycling method of waste lithium ion battery anode material |
| CN112479235A (en) * | 2020-12-23 | 2021-03-12 | 江苏容汇通用锂业股份有限公司 | Preparation method of hollow spherical lithium carbonate |
| CN114149016A (en) * | 2021-12-15 | 2022-03-08 | 天齐锂业股份有限公司 | Method for recovering lithium-copper composite belt |
| CN115216620B (en) * | 2022-07-11 | 2024-03-22 | 埃索凯循环能源科技(广西)有限公司 | Method for recovering nickel, cobalt and manganese from waste ternary lithium battery by fractional precipitation |
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