CN114014378B - Method for preparing amorphous single crystal positive electrode material by using super mixed flow reactor - Google Patents

Method for preparing amorphous single crystal positive electrode material by using super mixed flow reactor Download PDF

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CN114014378B
CN114014378B CN202111233276.0A CN202111233276A CN114014378B CN 114014378 B CN114014378 B CN 114014378B CN 202111233276 A CN202111233276 A CN 202111233276A CN 114014378 B CN114014378 B CN 114014378B
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CN114014378A (en
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梁国文
田新勇
魏玲
高彦宾
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Shaanxi Hongma Technology Co ltd
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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
    • C01G53/40—Nickelates
    • C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
    • C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
    • C01G53/50—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [MnO2]n-, e.g. Li(NixMn1-x)O2, Li(MyNixMn1-x-y)O2
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Organic Chemistry (AREA)
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  • Battery Electrode And Active Subsutance (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention discloses a method for preparing amorphous monocrystalline anode material by using a super mixed flow reactor, which comprises the following steps: 1. preparing nickel salt, cobalt salt and manganese salt into mixed salt solution; 2. preparing a precipitant solution; 3. continuously adding a mixed salt solution and a precipitant solution into a super mixed flow reactor to synthesize a precursor; 4. washing and drying the precursor obtained in the step 3 to obtain a blocky precursor; 5. the blocky precursor is subjected to jet milling to obtain a powdery precursor; 6. screening and deironing the powdery precursor to obtain a precursor finished product; 7. and mixing the precursor finished product with lithium salt, and sintering, crushing, screening and packaging to obtain the amorphous monocrystalline anode material. The invention creatively uses a super mixed flow reactor, does not use ammonia complexing agent, adds a crushing procedure in the post-treatment stage, and successfully prepares the amorphous single crystal anode material, thereby solving the problems of high wastewater treatment difficulty, low productivity, high cost and the like in the production process of the prior art.

Description

Method for preparing amorphous single crystal positive electrode material by using super mixed flow reactor
Technical Field
The invention relates to the technical field of new energy materials, in particular to a method for preparing an amorphous monocrystalline anode material by using a super mixed flow reactor.
Background
With the rapid development of society, new energy power battery automobiles gradually enter the life of people, and the power batteries are required to have higher capacity, thermal stability and cycle stability. Lithium ion batteries have currently taken a very important place in the energy storage market due to the advantage of having a high capacity. The ternary material combines the advantages of three materials through the synergistic effect of Ni-Co-Mn: liCoO 2 Has good cycle performance, liNiO 2 Has high specific capacity and LiMnO 2 Has high safety and low costAnd the like, and becomes one of the novel lithium ion battery anode materials with the most development prospect at present.
The main method for preparing the nickel-cobalt-manganese precursor at the present stage comprises the following steps: firstly, preparing nickel cobalt manganese solid salt into a mixed solution with a certain concentration and proportion, and coprecipitating and crystallizing the mixed solution, a precipitator and a complexing agent; and secondly, aging, washing, drying, sieving, deferrizing and the like are carried out on the crystal slurry to obtain the nickel cobalt manganese hydroxide precursor.
CN112694139a discloses a preparation method of a monocrystal NCM ternary positive electrode material precursor, which comprises the following steps: s1, adding a Nix:Coy:Mnz sulfate solution with the total concentration of 1.0-2.2 mo1/L, a 4-10 mol/L caustic soda solution and 20% ammonia water into a reaction unit according to a proportion, simultaneously introducing inert gas to perform a first-stage reaction, after particles D50=1.5-1.8 mu m are measured, increasing the ammonia value in a reaction kettle to perform a second-stage reaction, controlling the concentration of the ammonia water to be 2-7g/L, controlling the pH value to be 9.00-11.00, concentrating by using a solid lifting unit to improve the solid content and adjust the clearing speed of a solid lifting device, and finally, measuring the particles D50=3.8-4.5 mu m to stop the reaction; and S3, washing, drying and screening the slurry to obtain the monocrystal NCM ternary cathode material precursor.
CN110550668A discloses a process for preparing a power type single crystal NCM622 precursor concentrator, which comprises the following steps: (1) Preparing nickel-cobalt-manganese sulfate solution with a certain concentration by taking soluble salt nickel sulfate, manganese sulfate and cobalt sulfate as raw materials; (2) Adding ammonia water into the prepared nickel-cobalt-manganese solution according to a certain proportion to form a mixed solution, taking sodium hydroxide solution as a precipitator, and performing coprecipitation reaction to obtain mixed slurry; (3) The reaction is carried out in a reaction kettle, when the solid content reaches the requirement, overflow is stopped, concentration is carried out, and the granularity is controlled below 2.6 microns; (4) Finally, the power type single crystal NCM622 precursor is prepared by washing in a washing tank, drying, screening, removing iron and packaging.
CN106920934a discloses a preparation method of cobalt-aluminum co-doped modified ternary precursor based on high nickel material and a positive electrode material, which comprises mixing nickel-cobalt-aluminum mixed solution, ammonia water and sodium hydroxide solution in a heating reaction kettle to generate co-precipitation reaction, so as to obtain the cobalt-aluminum co-doped modified ternary precursor based on high nickel material.
Ammonia water is used as a complexing agent in the method, so that a large amount of ammonia-containing wastewater is generated in the production process of the nickel-cobalt-manganese precursor, and great pressure is brought to environmental protection and subsequent treatment.
Disclosure of Invention
The invention provides a method for preparing an amorphous single crystal positive electrode material by using a super mixed flow reactor, which is creatively characterized in that the super mixed flow reactor is not used, an ammonia complexing agent is not used, and a crushing procedure is added in a post-treatment stage, so that a precursor for the amorphous single crystal positive electrode material is successfully prepared, and the problems of high wastewater treatment difficulty, high environmental protection pressure, low productivity, high cost, difficult post-treatment and the like in the conventional precursor production process for the single crystal positive electrode material are solved.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a method for preparing amorphous single crystal positive electrode material using a super mixed flow reactor, comprising the steps of:
1. preparing nickel salt, cobalt salt and manganese salt into mixed salt solution;
2. preparing a precipitant solution;
3. continuously adding a mixed salt solution and a precipitant solution into a super mixed flow reactor to synthesize a precursor;
4. washing and drying the precursor obtained in the step 3 to obtain a precursor for the bulk amorphous monocrystalline anode material;
5. carrying out jet milling on the blocky precursor obtained in the step 4 to obtain a precursor for the powdery amorphous monocrystalline anode material;
6. screening and removing iron from the powdery precursor obtained in the step 5 to obtain a precursor finished product for the amorphous monocrystalline anode material;
7. and (3) mixing the precursor finished product obtained in the step (6) with lithium salt, and obtaining the amorphous monocrystalline anode material through sintering, crushing, screening and packaging.
Preferably, the mixed salt solution is one or more of a sulfate mixed solution, a nitrate mixed solution, a chloride mixed solution or a carbonate mixed solution of nickel, cobalt and manganese.
Preferably, ni in the mixed salt solution of step 1: co: the molar ratio of Mn is X: y: z; x is more than or equal to 0 and less than or equal to 1.0, Y is more than or equal to 0 and less than or equal to 1.0, Z is more than or equal to 0 and less than or equal to 1.0, and x+y+z=1.0.
Preferably, the precipitant is one or more of sodium hydroxide, sodium carbonate, potassium hydroxide and potassium carbonate.
Preferably, the concentration of the precipitant solution is 1-10mo/L.
Preferably, the flow rate of adding the mixed salt solution into the super mixed flow reactor in the step 3 is 1-100L/min, the flow rate of adding the precipitant solution is 1-500L/min, the rotating speed of a propeller of the super mixed flow reactor is 800-10000r/min, the reaction temperature is 30-90 ℃, and the solid content is controlled at 50-1000g/L.
Preferably, in the step 4, washing is performed by alkali washing and then water washing, and the alkali washing process comprises the following steps: the concentration of alkaline water is between 0 and 5mol/L, and the alkaline washing amount is between 1 and 50m 3 T; the water washing process comprises the following steps: the pH value of the washing water is less than or equal to 10.0, and the washing is qualified.
Further preferably, the drying device in the step 4 is a disc dryer, and the drying moisture is controlled to be less than or equal to 1%.
Preferably, the classification frequency of the airflow equipment is controlled to be 30-300HZ, the airflow pressure is 0.1-10.0MPa, and the induced air frequency is 1-50HZ when the airflow crushing is carried out in the step 5.
Further preferably, the particle size of the precursor for powdery amorphous single crystal positive electrode material obtained after the jet milling in the step 5 is 0.1 to 3.0 μm.
Preferably, in the step 6, 200-500 mesh ultrasonic vibration is used for sieving; the electromagnetic iron remover is used for controlling the magnetic substances to be less than or equal to 100ppb.
Preferably, the lithium source in the step 7 is one or more of lithium carbonate, lithium hydroxide and lithium nitrate; the sintering temperature is 500-1500 ℃ and the sintering time is 10-50h; the screening uses an ultrasonic vibration screen with 200-500 meshes.
Further preferably, the classification frequency of the air flow equipment is controlled to be 30-300HZ, the air flow pressure is 0.1-10.0MPa, and the induced air frequency is 1-50HZ during the crushing in the step 7.
The invention has the beneficial effects that:
the invention provides a method for preparing an amorphous monocrystalline cathode material by using a super mixed flow reactor, which is different from the existing method for intermittently synthesizing a precursor for a conventional monocrystalline cathode material by using a conventional reaction kettle thickener.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only embodiments of the present invention, and that other drawings can be obtained according to the provided drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a super mixed flow reactor apparatus for use in the present invention;
FIG. 2 is a process flow diagram of an amorphous single crystal positive electrode material prepared using a super-mixed flow reactor in accordance with the present invention;
FIG. 3 is an SEM image of a conventional single crystal positive electrode material prepared according to comparative example 1 of the present invention;
FIG. 4 is an SEM image of an amorphous single crystal positive electrode material prepared using a super mixed flow reactor prepared according to example 1 of the present invention;
FIG. 5 is an SEM image of an amorphous single crystal positive electrode material prepared using a super mixed flow reactor prepared according to example 2 of the present invention;
FIG. 6 is an SEM image of an amorphous single crystal positive electrode material prepared using a super mixed flow reactor prepared according to example 3 of the present invention;
in fig. 1:
the method comprises the steps of 1, a propeller blade, 2, a super mixed flow area, 3, an overflow port, 4, a mixed salt solution feeding port and 5, a precipitant solution feeding port.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
As shown in fig. 1, the working principle of the super mixed flow reactor is as follows: the mixed salt solution enters the corresponding chamber through the feed inlet 4, the precipitant solution enters the corresponding chamber through the feed inlet 5, the two solutions in the corresponding chamber are pushed to the super mixed flow area 2 through the high-speed rotation of the spiral propulsion blade 1, the two solutions react instantly to complete high-strength mixing, and then the precipitant solution flows out through the overflow port 3 quickly. The advantages are that: the reactor has good mixing effect, can ensure the large-flow feeding of salt solution and precipitant solution, and ensures continuous feeding and larger productivity.
Comparative example 1 (conventional monocrystalline cathode material)
1. Preparing nickel sulfate, cobalt sulfate and manganese sulfate into mixed salt solution with the concentration of 2mol/L according to the mol ratio of 50:20:30 by using a sulfate system; preparing a sodium hydroxide solution with the concentration of 4mo/L by using sodium hydroxide as a precipitator; using 20% ammonia water solution as complexing agent;
2. simultaneously pumping the mixed salt solution, the sodium hydroxide solution and the ammonia water solution into a reaction kettle, wherein the flow rate of the sulfate mixed solution is 10L/min, the flow rate of the sodium hydroxide solution is 11L/min, the flow rate of the ammonia water solution is 2L/min, the reaction temperature is controlled to be 50 ℃, the stirring speed is 200r/min, the solid content is 200g/L, the synthesis is carried out by a continuous method, and the particle size is controlled to be 2.8 mu m;
3. the materials obtained in the step 2 are treated with 1mol/L alkaline water according to 1m 3 Alkaline washing is carried out on the washing water quantity of/T, and the pH value of the washing water is controlled to be 9.5; drying the washed material by using a tray dryer, and controlling the water content to be 0.5%; screening the dried material by using a 300-mesh ultrasonic vibration screen; feeding the sieved material by using an electromagnetic iron removerAnd removing iron, wherein the magnetic substance is 30ppb, so as to obtain the precursor for the conventional monocrystalline cathode material.
4. Fully mixing the precursor obtained in the step 3 with lithium carbonate, and sintering at 800 ℃ for 20 hours; crushing the sintered material by using an air flow mill, controlling the air flow pressure to be 1.1MPa, the classification frequency to be 120HZ and the induced air frequency to be 25HZ; and screening the crushed material by using a 300-mesh ultrasonic vibration sieve to obtain the conventional monocrystalline anode material.
Example 1
1. The salt solution uses a sulfate system, and nickel sulfate, cobalt sulfate and manganese sulfate are prepared into a sulfate mixed solution with the concentration of 2mol/L according to the mol ratio of 50:20:30.
2.6 mol/L sodium hydroxide solution was prepared using potassium hydroxide as a precipitant.
3. The flow rate of the sulfate mixed solution is 50L/min, the flow rate of the potassium hydroxide solution is 36.7L/min, the sulfate mixed solution and the potassium hydroxide solution are continuously added into the super-mixed flow reactor, the rotating speed of a propeller is controlled to be 2000r/min, the temperature is 50 ℃, the solid content is controlled to be 280g/L, and the mixed solution is continuously synthesized.
4. The material obtained in the step 3 is treated with 0.5mol/L alkaline water according to 3m 3 Alkaline washing is carried out on the washing water quantity of/T, and the pH value of the washing water is controlled to be 9.0; and drying the washed material by using a tray dryer, and controlling the water content to be 0.5% to obtain a precursor for the bulk amorphous monocrystalline cathode material.
5. And (3) carrying out jet milling on the blocky precursor obtained in the step (4), controlling the grading frequency to be 180HZ, the jet pressure to be 0.2MPa, the induced air frequency to be 35HZ, and milling the blocky precursor into powder with the particle size of 3.0 mu m.
6. Screening and deironing the powdery precursor in the step 5, and screening by using a 250-mesh ultrasonic vibration screen; and (3) removing iron from the sieved material by using an electromagnetic iron remover, wherein the magnetic substance is 50ppb, so as to obtain a precursor finished product for the amorphous single crystal positive electrode material prepared by using the super-mixed flow reactor.
7. Fully mixing the precursor obtained in the step 6 with lithium carbonate, and sintering at 920 ℃ for 23h; crushing the sintered material by using an air flow mill, controlling the air flow pressure to be 0.5MPa, the classification frequency to be 200HZ and the induced air frequency to be 40HZ; and screening the crushed material by using a 300-mesh ultrasonic vibration sieve to obtain the amorphous single crystal anode material prepared by using the super mixed flow reactor.
Example 2
1. The salt solution uses a chloride salt system, and nickel chloride, cobalt chloride and aluminum chloride are prepared into a chloride salt mixed solution with the concentration of 2mo/L according to the mol ratio of 50:20:30;
2. preparing 8mo/L sodium carbonate solution by using sodium carbonate as a precipitator;
3. continuously adding the mixed solution of chloride and sodium carbonate into a super-mixed flow reactor, controlling the rotating speed of a propeller to be 7000r/min, controlling the temperature to be 60 ℃ and controlling the solid content to be 300g/L, and continuously synthesizing;
4. the material obtained in the step 3 is treated with 0.1mol/L alkaline water according to 1.5m 3 Alkaline washing is carried out on the washing water quantity of/T, and the pH value of the washing water is controlled to be 8.5; and drying the washed material by using a tray dryer, and controlling the water content to be 0.5% to obtain a precursor for the bulk amorphous monocrystalline cathode material.
5. And (3) carrying out jet milling on the blocky precursor obtained in the step (4), controlling the grading frequency to be 150HZ, the jet pressure to be 1MPa, the induced air frequency to be 45HZ, and milling the blocky precursor to the grain size of 3.2 mu m.
6. Screening and deironing the powdery precursor in the step 5, and screening by using a 300-mesh ultrasonic vibration screen; and (3) removing iron from the sieved material by using an electromagnetic iron remover, wherein the magnetic substance is 50ppb, so as to obtain a precursor finished product for the amorphous single crystal positive electrode material prepared by using the super-mixed flow reactor.
7. Fully mixing the precursor obtained in the step 6 with lithium carbonate, and sintering for 26 hours at 860 ℃; crushing the sintered material by using an air flow mill, controlling the air flow pressure to be 0.8MPa, the classification frequency to be 180HZ and the induced air frequency to be 40HZ; and screening the crushed material by using a 300-mesh ultrasonic vibration sieve to obtain the amorphous single crystal anode material prepared by using the super mixed flow reactor.
Example 3
1. The salt solution uses a nitrate system, and nickel nitrate, cobalt nitrate and manganese nitrate are prepared into a nitrate mixed solution with the concentration of 2mo/L according to the mol ratio of 50:20:30;
2. preparing 10mo/L sodium hydroxide solution by using potassium carbonate as a precipitator;
3. the flow rate of the nitrate mixed solution is 45L/min, the flow rate of the sodium hydroxide solution is 10L/min, the nitrate mixed solution and the sodium hydroxide solution are continuously added into the super mixed flow reactor, the rotating speed of a propeller is controlled to be 8800r/min, the temperature is 52 ℃, the solid content is controlled to be 380g/L, and the mixture is continuously synthesized;
4. the material obtained in the step 3 is treated with 3.5mol/L alkaline water according to 0.5m 3 Alkaline washing is carried out on the washing water quantity of/T, and the pH value of the washing water is controlled to be 8.5; and drying the washed material by using a tray dryer, and controlling the water content to be 0.5% to obtain a precursor for the bulk amorphous monocrystalline cathode material.
5. And (3) carrying out jet milling on the blocky precursor obtained in the step (4), controlling the grading frequency to 175HZ, the jet pressure to 1.3MPa and the induced air frequency to 45HZ, and milling the blocky precursor to the grain size of 3.5 mu m.
6. Screening and deironing the powdery precursor in the step 5, and screening by using a 300-mesh ultrasonic vibration screen; and (3) removing iron from the sieved material by using an electromagnetic iron remover, wherein the magnetic substance is 50ppb, so as to obtain a precursor finished product for the amorphous single crystal positive electrode material prepared by using the super-mixed flow reactor.
7. Fully mixing the precursor obtained in the step 6 with lithium hydroxide, and sintering at 780 ℃ for 26 hours; crushing the sintered material by using an air flow mill, controlling the air flow pressure to be 1.5MPa, the classification frequency to be 200HZ and the induced air frequency to be 40HZ; and screening the crushed material by using a 300-mesh ultrasonic vibration sieve to obtain the amorphous single crystal anode material prepared by using the super mixed flow reactor.
Table 1: comparative example 1 and examples 1-3 production efficiency and productivity control Table
As can be seen from fig. 3 to 6, the precursor obtained in examples 1 to 3 using the super-mixed flow reactor was sintered, and the final obtained cathode material SEM was close to the SEM image synthesized in comparative example 1 using the conventional method, and SEM was a key index for judging the quality of the cathode material.
In the present specification, each embodiment is described in a progressive manner, and each embodiment is mainly described in a different point from other embodiments, and identical and similar parts between the embodiments are all enough to refer to each other. For the device disclosed in the embodiment, since it corresponds to the method disclosed in the embodiment, the description is relatively simple, and the relevant points refer to the description of the method section.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (10)

1. A method for preparing amorphous single crystal positive electrode material using a super mixed flow reactor, comprising the steps of:
(1) Preparing nickel salt, cobalt salt and manganese salt into mixed salt solution;
(2) Preparing a precipitant solution;
(3) Continuously adding a mixed salt solution and a precipitant solution into a super mixed flow reactor to synthesize a precursor; adding mixed salt solution into a super mixed flow reactor at a flow rate of 1-100L/min, adding precipitant solution at a flow rate of 1-500L/min, rotating a propeller of the super mixed flow reactor at a speed of 800-10000r/min, reacting at a temperature of 30-90 ℃ and controlling the solid content at 50-1000g/L;
(4) Washing and drying the precursor obtained in the step (3) to obtain a precursor for the bulk amorphous monocrystalline anode material;
(5) Carrying out jet milling on the blocky precursor obtained in the step (4) to obtain a precursor for the powdery amorphous monocrystalline anode material;
(6) Screening and removing iron from the powdery precursor obtained in the step (5) to obtain a precursor finished product for the amorphous monocrystalline anode material;
(7) Mixing the precursor finished product obtained in the step (6) with lithium salt, and obtaining an amorphous single crystal anode material through sintering, crushing, screening and packaging;
the super mixed flow reactor comprises a propelling propeller blade, a super mixed flow area, an overflow port, a mixed salt solution feed port and a precipitant solution feed port.
2. The preparation method according to claim 1, wherein the mixed salt solution is one or more of a sulfate mixed solution, a nitrate mixed solution, a chloride mixed solution or a carbonate mixed solution of nickel, cobalt and manganese.
3. The method of claim 1, wherein Ni in the mixed salt solution of step (1): co: the molar ratio of Mn is X: y: z; x is more than or equal to 0 and less than or equal to 1.0, Y is more than or equal to 0 and less than or equal to 1.0, Z is more than or equal to 0 and less than or equal to 1.0, and x+y+z=1.0.
4. The method according to claim 1, wherein the concentration of the mixed salt solution in the step (1) is 0.5 to 5mol/L.
5. The preparation method according to claim 1, wherein the precipitant in the step (2) is one or more of sodium hydroxide, sodium carbonate, potassium hydroxide and potassium carbonate; the concentration of the precipitant solution is 1-10mol/L.
6. The method according to claim 1, wherein the washing in step (4) is performed by alkali washing and then water washing, and the alkali washing process comprises: the concentration of the alkaline water is between 0 and 5mol/L, and the alkaline washing amount is 1 to 50m 2/T; the water washing process comprises the following steps: the pH value of the washing water is less than or equal to 10.0, and the washing is qualified;
the drying equipment in the step (4) is a disc dryer, and the drying moisture is controlled to be less than or equal to 1%.
7. The method according to claim 1, wherein the classification frequency of the air flow equipment is controlled to be 30-300HZ, the air flow pressure is 0.1-10.0MPa, and the induced air frequency is 1-50HZ when the air flow crushing is carried out in the step (5); the particle size of the precursor for the powdery amorphous monocrystalline cathode material obtained after jet milling is 0.1-4.0 mu m.
8. The method of claim 1, wherein step (6) uses 200-500 mesh ultrasonic vibration for sieving; the electromagnetic iron remover is used for controlling the magnetic substances to be less than or equal to 100ppb.
9. The method according to claim 1, wherein the lithium source in the step (7) is one or more of lithium carbonate, lithium hydroxide and lithium nitrate; the sintering temperature is 500-1500 ℃ and the sintering time is 10-50h; the screening uses an ultrasonic vibration screen with 200-500 meshes.
10. The method according to claim 1, wherein the classification frequency of the air flow device is controlled to be 30-300HZ, the air flow pressure is 0.1-10.0MPa, and the induced air frequency is 1-50HZ during the pulverization in the step (7).
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