CN108910965A - A method of preparing ternary hydroxide presoma - Google Patents
A method of preparing ternary hydroxide presoma Download PDFInfo
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- CN108910965A CN108910965A CN201810563049.6A CN201810563049A CN108910965A CN 108910965 A CN108910965 A CN 108910965A CN 201810563049 A CN201810563049 A CN 201810563049A CN 108910965 A CN108910965 A CN 108910965A
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- ternary
- hydroxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides; Hydroxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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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
Abstract
The present invention provides a kind of method for preparing ternary hydroxide presoma, which includes：Prepare initial soln：Dissolution waste and old lithium ion battery tertiary cathode obtains initial soln；Prepare intermediate solution：Oil removal is gone to obtain intermediate solution；Adjust the intermediate solution concentration：The soluble inorganic salt of nickel, cobalt, manganese is added in intermediate solution, adjusts the concentration of the ternary ionic in intermediate solution；Ternary hydroxide presoma is prepared according to the following steps：Inert gas is passed through to the reaction kettle of bottom liquid；Anionic surfactant is added in the aqueous slkali that sodium hydroxide and ammonium hydroxide are prepared and prepares mixed solution；Prepare ternary hydroxide presoma：The solution of ternary ionic and the mixed solution are prepared into ternary hydroxide presoma by coprecipitation reaction in the reaction kettle.Method provided by the invention realizes the control of a secondary growth granule-morphology of ternary hydroxide presoma；Gained tertiary cathode material has excellent high rate performance, can be used as the positive electrode of power-type lithium ion battery.
Description
Technical field
The present invention relates to a kind of methods for preparing ternary hydroxide presoma, in particular, being related to a kind of using waste and old
The method that lithium ion battery tertiary cathode prepares ternary hydroxide presoma.
Background technique
In recent years, to pure electric automobile demand under the fast development of China's new-energy automobile industry, especially policy driving
Growth, be greatly promoted the production of power battery, the quantity of waste and old power battery is also with going up.Waste and old power battery
Recycling is the important component in new-energy automobile industrial life cycle, rationally disposes, especially recycles therein
Transition metal element is most important to industry development.And high efficiente callback both may be used using the transition metal in waste and old lithium ion battery
Reduce cost, it helps promote the sustainable development and industrial upgrading of power battery industry.
The processing disposition of the waste and old power battery in China remains at market and technology breeding phase, the pretreatment of front end at present
Process such as power battery dismantling, echelon utilize, battery core it is broken/sorting technology in terms of had breakthrough, but recycle in resource high-efficiency,
Material regeneration and overall process greenization upgrading etc. still have greater room for improvement.In addition, China's Vehicular dynamic battery recycling network
Network and effective take-back model still need to be established and standardized.With the constantly improve of China's relevant policies, the production of waste and old power battery
Amount be continuously increased and the continuous maturation of the relevant technologies, the waste and old power battery in China recycle management system and industry knot
Structure will be further perfect, and market will gradually be moved towards to standardize.
Ternary battery occupies biggish share due to the high advantage of energy density in the market, in recent years, waste and old lithium
Nickel in ion battery, manganese content be significantly increased, three kinds of nickel, cobalt, manganese elements were being recycled due to the similitude of its physicochemical property
Cheng Zhong is separated extremely difficult.The recovery method of existing big multipair waste and old ternary anode material for lithium-ion batteries, nickel, cobalt, manganese
Separation costs are high, complex process, and easily pollute the environment.
Summary of the invention
In view of this, utilizing waste and old lithium ion battery tertiary cathode material preparation one the purpose of the present invention is to provide a kind of
The method of the controllable ternary hydroxide presoma of secondary granule-morphology.The method dissolves waste and old ternary using acetic acid and hydrogen peroxide
Positive electrode, using the nanometer sheet pattern of presoma primary particle in anionic surfactant control coprecipitation process, the party
Method simple process is efficient, directly from waste and old lithium ion battery tertiary cathode material leach ternary transition metal (nickel, cobalt, manganese) from
Son has saved the cost of separation nickel, cobalt, manganese, leaching process is in waste and old tertiary cathode material for producing ternary precursor
Nickel, cobalt, the rate of recovery of manganese are high, favorable environment protection；The feed rate of coprecipitation process is fast；Ternary hydroxide made from this method
After mixed lithium calcining, gained tertiary cathode material shows object presoma because saving the nano-sheet primary particle of presoma
Excellent high rate performance out can be used as the positive electrode of power-type lithium ion battery.
The purpose of the present invention is what is be achieved through the following technical solutions：
The step of method that kind prepares ternary hydroxide presoma, the method, is as follows：
One, initial soln is prepared：Initial soln is obtained with acetic acid and hydrogen peroxide dissolution waste and old lithium ion battery tertiary cathode；
Two, intermediate solution is prepared：After ammonium hydroxide is added into the initial soln, oil removal is gone to obtain intermediate solution；
Three, the intermediate solution concentration is adjusted：The soluble inorganic salt is added in the intermediate solution, adjusts intermediate
The concentration of ternary ionic in solution；
Four, ternary hydroxide presoma is prepared：
1) inert gas is passed through to the reaction kettle of bottom liquid；
2) anionic surfactant is added in the aqueous slkali that sodium hydroxide and ammonium hydroxide are prepared and prepares mixed solution；
3) ternary hydroxide presoma is prepared：
The solution of ternary ionic and the mixed solution are prepared into ternary hydrogen by coprecipitation reaction in the reaction kettle
Oxide precursor.
In first preferred method provided by the invention, the solute of acetic acid solution and the molar ratio of hydrogen peroxide are 4:1~1:1；
The solute of acetic acid solution and the mass ratio of waste and old lithium ion battery tertiary cathode material are 1:4~1:1；
In second preferred method provided by the invention, ammonium hydroxide is added into the initial soln and removes impurity aluminum, iron, copper,
The wherein additional amount of ammonium hydroxide is 50 by the mass ratio of tertiary cathode material and ammonium hydroxide solute:1~100:1.
In third preferred method provided by the invention, the soluble inorganic salt of the ternary be nickel, cobalt and manganese sulfate,
Nitrate or chlorate, nickel, cobalt and manganese ion concentration ratio are 0.6:0.2:0.2, metal ion total concentration is 3.0~6.0mol
L-1。
In 4th preferred method provided by the invention, wherein sodium hydroxide and ammonium hydroxide are configured to hydrogen according to molar ratio 0.5~5
Aoxidize 1~5mol of na concn L-1Mixed liquor.
In 5th preferred method provided by the invention, the anionic surfactant is fatty acid salt, sulfate, sulfonic acid
The one or more mixtures selected in salt and phosphate；The mass ratio of sodium hydroxide and surfactant is 12~20.
In 6th preferred method provided by the invention, the bottom liquid is deionized water, and ammonium hydroxide, which is added, makes the pH 12 of dropping liquid
~13.
In 7th preferred method provided by the invention, continue after mixing 6~12h at 30~42 DEG C in the reaction kettle
It is passed through inert gas and continues 1~4h of stirring.
In 8th preferred method provided by the invention, be filtered, washed after mixing in the vacuum oven at 60~70 DEG C
Dry at least 12h.
Compared with the latest prior art, technical solution provided by the invention has the advantages that：
Method provided by the invention, it is high to the recovery efficiency of the nickel of waste and old lithium ion battery, cobalt, manganese, it is environmental-friendly, without dirt
Dye；The anionic surfactant of presoma is added in method provided by the invention in hydroxide coprecipitation process
Amount and type, realize the control of a secondary growth granule-morphology of ternary precursor, this method coprecipitation process feed time
It is shorter, it is simple and efficient.After mixed lithium calcining, gained tertiary cathode material has excellent forthright again presoma made from this method
Can, it can be used as the positive electrode of power-type lithium ion battery.
Detailed description of the invention
Fig. 1 is a kind of scanning electron microscope (SEM) for preparing ternary hydroxide presoma that the embodiment of the present invention 1 is prepared
Figure.
Fig. 2 is a kind of scanning electron microscope (SEM) for preparing ternary hydroxide presoma that the embodiment of the present invention 2 is prepared
Figure.
Specific embodiment
To be best understood from the present invention, the invention will be described in further detail combined with specific embodiments below.
In following example 1~2, used phenetic analysis means are as follows：
Scanning electron microscope (SEM) test：Instrument model：FEI Quanta 250, the U.S.；
Embodiment 1
Using acetic acid and hydrogen peroxide, (molar ratio of solute is 2:1) the waste and old lithium ion battery tertiary cathode material of dissolution recycling
Material, wherein the ratio of acetic acid solute and waste and old ternary cell positive material is 1:3, obtain initial soln I, through measuring, waste and old lithium from
The leaching rate of nickel, cobalt, manganese in sub- battery tertiary cathode material is 98.2%；
Ammonium hydroxide mass ratio by waste and old tertiary cathode material and 25% is 75:4, ammonium hydroxide is added into solution I and makees filter aid,
It is filtered, removes impurity aluminum, iron, copper, through measuring, the removal rate of impurity is 97.0%, obtains intermediate solution II, measures solution II
In Ni2+、Co2+、Mn2+Ion concentration be 0.57:0.22:0.21；
NiSO is added into intermediate solution II4·6H2O、CoSO4·7H2O、MnSO4·H2O is configured to nickel, cobalt, manganese ion
Concentration ratio be 0.6:0.2:0.2 solution, and ternary ionic total concentration is 4mol L-1Solution, by this solution labeled as molten
Liquid III；
With NaOH and ammonium hydroxide in molar ratio 2:1 is configured to naoh concentration as 2mol L-1Mixed ammonium/alkali solutions.
Make anionic surfactant mixture with lauryl sodium sulfate and neopelex, the two by mole
Than 4:1 ratio is configured to anionic surfactant mixture.
By the sodium hydroxide in the mixed ammonium/alkali solutions with the surfactant qualities than 16:1 ratio be added yin from
Sub- surfactant.It is 1000r/min by mixing speed, reaction temperature is set as 40 DEG C, and is passed through indifferent gas in a kettle
Body protection.After mixing speed, temperature, atmosphere are stablized, the solution III, mixed ammonium/alkali solutions are slowly at the uniform velocity pumped into reaction kettle
In, feed rate is adjusted, stablizes pH 12.5.Feed time is 8h, continues to be passed through argon gas stirring 2h after charging.It will sink
Form sediment filtering, cleaning, dry, obtained ternary hydroxide presoma Ni0.6Co0.2Mn0.2(OH)2。
Using Ni obtained by scanning electronic microscope observation0.6Co0.2Mn0.2(OH)2Pattern.As shown in Figure 1, primary particle
It is presented relatively thin nano-sheet, and more lax accumulates for spherical second particle.Gained particle obtains ternary after mixed lithium calcining
Material LiNi0.6Co0.2Mn0.2O2, assembled principle battery (to electrode be lithium metal) 10C (1C=200mAh g-1) multiplying power, 3
Charge and discharge under~4.25V voltage range, discharge capacity are 196mAh g-1, these data illustrate the embodiment of the invention be made
Product shown good high rate performance.
Embodiment 2
Using acetic acid and hydrogen peroxide, (molar ratio of solute is 2:1) the waste and old lithium ion battery tertiary cathode material of dissolution recycling
Material, wherein the ratio of acetic acid solute and waste and old ternary cell positive material is 1:3, obtain initial soln I, through measuring, waste and old lithium from
The leaching rate of nickel, cobalt, manganese in sub- battery tertiary cathode material is 98.0%；
Ammonium hydroxide mass ratio by waste and old tertiary cathode material and 25% is 75:4, ammonium hydroxide is added into the initial soln I
Make filter aid, filtered, removes impurity aluminum, iron, copper, through measuring, the removal rate of impurity is 97.4%, intermediate solution II is obtained,
Measure Ni in solution II2+、Co2+、Mn2+Ion concentration be 0.57:0.22:0.21；
Appropriate NiSO is added into solution II4·6H2O、CoSO4·7H2O、MnSO4·H2O is configured to nickel, cobalt, manganese ion
Concentration ratio be 0.8:0.1:0.1, and ternary ionic total concentration is 4mol L-1Solution, be labeled as solution III；
With NaOH and ammonium hydroxide in molar ratio 2:1 is configured to naoh concentration as 2mol L-1Mixed ammonium/alkali solutions.
Make anionic surfactant with lauryl sodium sulfate and neopelex, in molar ratio 1:1 prepares
At anionic surfactant mixture.
According to sodium hydroxide and surfactant qualities than 16 in the mixed ammonium/alkali solutions:Anion is added in 1 ratio
Surfactant mixture.It is 1000r/min by mixing speed, reaction temperature is set as 40 DEG C, and is passed through in a kettle lazy
Property gas shield.After mixing speed, temperature, atmosphere are stablized, the solution III, mixed ammonium/alkali solutions are slowly at the uniform velocity pumped into anti-
It answers in kettle, adjusts feed rate, stablize pH 12.5.Feed time is 8h, continues to be passed through argon gas stirring 2h after charging.
By precipitating filtering, cleaning, dry, obtained ternary hydroxide presoma Ni0.8Co0.1Mn0.1(OH)2。
Using Ni obtained by scanning electronic microscope observation0.8Co0.1Mn0.1(OH)2Pattern.As shown in Figure 1, primary particle
Relatively thick nano-sheet is presented, bulk density is larger with respect to embodiment 1.The embodiment particle is after mixed lithium calcining, gained
Ternary material LiNi0.8Co0.1Mn0.1O2Principle battery (being lithium metal to electrode) 10C (1C=200mAh g of assembling-1) multiplying power,
Charge and discharge under 3~4.25V voltage range, discharge capacity are 208mAh g-1, show good high rate performance.
The present invention includes but is not limited to above embodiments, and the present invention expands to any new feature disclosed in the present specification
Or any new combination, and disclose any new method or process the step of or any new combination.
Claims (9)
1. a kind of method for preparing ternary hydroxide presoma, it is characterised in that：The method includes the following steps：
One, initial soln is prepared：Initial soln is obtained with acetic acid and hydrogen peroxide dissolution waste and old lithium ion battery tertiary cathode；
Two, intermediate solution is prepared：After ammonium hydroxide is added into the initial soln, oil removal is gone to obtain intermediate solution；
Three, the intermediate solution concentration is adjusted：Soluble inorganic salt is added in the intermediate solution, adjusts three in intermediate solution
The concentration of first ion；
Four, ternary hydroxide presoma is prepared：
1) inert gas is passed through to the reaction kettle of bottom liquid；
2) anionic surfactant is added in the aqueous slkali that sodium hydroxide and ammonium hydroxide are prepared and prepares mixed solution；
3) ternary hydroxide presoma is prepared：
The solution of ternary ionic and the mixed solution are prepared into ternary hydroxide by coprecipitation reaction in the reaction kettle
Object presoma.
2. a kind of method for preparing ternary hydroxide presoma as described in claim 1, it is characterised in that：Acetic acid solution it is molten
Matter and the molar ratio of hydrogen peroxide are 4:1~1:1；The solute of acetic acid solution and the quality of waste and old lithium ion battery tertiary cathode material
Than being 1:4~1:1.
3. a kind of method for preparing ternary hydroxide presoma as described in claim 1, it is characterised in that：To described initial molten
Ammonium hydroxide is added in liquid and removes foreign metal, wherein the additional amount of ammonium hydroxide, the mass ratio by tertiary cathode material and ammonium hydroxide solute are
50:1~100:1.
4. a kind of method for preparing ternary hydroxide presoma as described in claim 1, it is characterised in that：The ternary can
Soluble inorganic salt is nickel, the sulfate of cobalt and manganese, nitrate or chlorate, and nickel, cobalt and manganese ion concentration ratio are 0.6:0.2:
0.2, metal ion total concentration is 3.0~6.0mol L-1。
5. a kind of method for preparing ternary hydroxide presoma as described in claim 1, it is characterised in that：Wherein sodium hydroxide
1~5mol of naoh concentration L is configured to according to molar ratio 0.5~5 with ammonium hydroxide-1Mixed liquor.
6. a kind of method for preparing ternary hydroxide presoma as described in claim 1, it is characterised in that：The anion table
Face activating agent is the one or more mixtures selected in fatty acid salt, sulfate, sulfonate and phosphate；Sodium hydroxide with
The mass ratio of surfactant is 12~20.
7. a kind of method for preparing ternary hydroxide presoma as described in claim 1, it is characterised in that：The bottom liquid is to go
Ionized water, ammonium hydroxide, which is added, makes the pH 12~13 of bottom liquid.
8. a kind of method for preparing ternary hydroxide presoma as described in claim 1, it is characterised in that：In the reaction kettle
In mix to continue to be passed through inert gas after 6~12h at 30~42 DEG C and continue 1~4h of stirring.
9. a kind of method for preparing ternary hydroxide presoma as described in claim 1, it is characterised in that：Filtered after mixing,
Dry at least 12h in vacuum oven at washing and 60~70 DEG C.
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Cited By (3)
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| CN112054168A (en) * | 2019-06-06 | 2020-12-08 | 惠州比亚迪实业有限公司 | Method for preparing regenerated ternary precursor from regenerated ternary precursor and ternary precursor waste |
| CN112645394A (en) * | 2020-12-15 | 2021-04-13 | 荆门市格林美新材料有限公司 | Nickel-cobalt-manganese ternary precursor material and preparation method thereof |
| CN116143198A (en) * | 2023-04-18 | 2023-05-23 | 新乡天力锂能股份有限公司 | Method for regulating and controlling crystal face area of layered cathode material precursor (010) through anions |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112054168A (en) * | 2019-06-06 | 2020-12-08 | 惠州比亚迪实业有限公司 | Method for preparing regenerated ternary precursor from regenerated ternary precursor and ternary precursor waste |
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| CN116143198A (en) * | 2023-04-18 | 2023-05-23 | 新乡天力锂能股份有限公司 | Method for regulating and controlling crystal face area of layered cathode material precursor (010) through anions |
| CN116143198B (en) * | 2023-04-18 | 2023-09-22 | 新乡天力锂能股份有限公司 | Method for regulating and controlling crystal face area of layered cathode material precursor (010) through anions |
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