CN109354077A - A kind of ternary precursor and preparation method thereof of polycrystalline form - Google Patents
A kind of ternary precursor and preparation method thereof of polycrystalline form Download PDFInfo
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- CN109354077A CN109354077A CN201811201588.1A CN201811201588A CN109354077A CN 109354077 A CN109354077 A CN 109354077A CN 201811201588 A CN201811201588 A CN 201811201588A CN 109354077 A CN109354077 A CN 109354077A
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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
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
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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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- 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
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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
- 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
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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
- 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
Abstract
The embodiment of the present invention provides a kind of preparation method of the ternary precursor of polycrystalline form, the preparation method it is simple to operate, it is not high to equipment requirement, it is by metal salt solution via multiple inlet tubes, it is passed into reaction kettle and is reacted using different flow, so that the solution local reaction crystallization condition of each outlet of inlet pipe is different, so as to persistently prepare the equally distributed second particle with a variety of primary particle forms.After the second particle finished product is prepared into final battery, because it is with the advantage of different primary particle forms, so as to greatly improve the comprehensive performance of battery.A kind of ternary precursor of polycrystalline form, the advantages of it uses the preparation method of the ternary precursor of above-mentioned polycrystalline form to be prepared, and is made of the primary particle of a variety of crystal habits, integrates each form, mutual short slab is supplied, realizes the raising of ternary precursor comprehensive performance.
Description
Technical field
The present invention relates to technical field of lithium batteries, a kind of ternary precursor in particular to polycrystalline form and its
Preparation method.
Background technique
Lithium ion battery is the secondary cell of new generation developed rapidly the 1990s, is widely used in miniature portable
Formula electronic communication product and electric vehicle.Battery material manufacture is the core link in lithium battery industry.Battery material point
For positive electrode, negative electrode material, diaphragm, electrolyte etc..Positive electrode is one of the critical material for manufacturing lithium ion battery, is occupied
25% or more of battery cost, performance directly affect the performance indexes of battery, core are occupied in lithium ion battery
Status.
Currently, market anode material for lithium-ion batteries synthesis process is divided into the progress of two steps: before first synthesizing hydroxide
Drive body；Hydroxide precursor and lithium salts are subjected to mixing sintering again, obtain lithium ion battery oxide anode material.Ternary electricity
The presoma of pond positive electrode is usually the powdered spheric granules that D50 reaches 2~25 μm, in the industry referred to as second particle.And
Second particle is accumulated by several nanoscale primary particles, primary particle length be 10~1000nm, form by
Crystallization condition influences, and is divided into fine and soft shape, fine acicular, fusiform, strip, plate, sheet, rodlike, flower-shaped etc..The form of primary particle
The process for sintering tertiary cathode material into for back segment has larger impact, to finally influence electrical property, every kind of primary particle
Form can generate different influences to rear end process, therefore can be realized finally just by controlling the form of primary particle
The difference of the electrical property of pole material.
Different primary particle forms show apparent preference for final electrical property influence, such as: fine acicular is primary
Particle shows preferable high rate performance, but capacity is relatively low；Strip primary particle shows preferable security performance, but multiplying power is inclined
It is low；Sheet primary particle shows preferable volumetric properties, but recycles relatively low etc..However, passing through in traditional preparation process
Temperature, ammonia density, stirring, temperature, solid content, flow, pH in control reaction kettle realize the normal preparation of ternary precursor,
The primary particle form of output is relatively simple.After being finally prepared into battery in this way, it will be influenced, can only be applicable in by the strengths and weaknesses of itself
The specific consumer field of Mr. Yu, for the product in different application direction, product needs to re-start between each other raw material exploitation and work
Skill adaptation, to increase research and development and production cost.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of the ternary precursor of polycrystalline form, sides easy to operate
Just, not high to equipment requirement, the ternary precursor comprising a variety of crystal habits can be prepared.
Another object of the present invention is to provide a kind of ternary precursors of polycrystalline form, use above-mentioned polycrystalline shape
The preparation method of the ternary precursor of state is prepared, and is made of the primary particle of a variety of crystal habits, integrates each form
The advantages of, mutual short slab is supplied, realizes the raising of ternary precursor comprehensive performance.
The embodiment of the present invention is achieved in that
A kind of preparation method of the ternary precursor of polycrystalline form comprising:
Metal salt solution comprising nickel ion, cobalt ions and manganese ion and liquid alkaline solution, ammonia spirit are passed into together
Hybrid reaction in reaction kettle；
Wherein, reaction kettle has multiple for being passed through the inlet tube of metal salt solution, and it is molten that multiple inlet tubes are passed through metal salt
The flow of liquid is different.
A kind of ternary precursor of polycrystalline form, by the preparation method system of the ternary precursor of above-mentioned polycrystalline form
It is standby to obtain.
The beneficial effect of the embodiment of the present invention is:
The embodiment of the present invention provides a kind of preparation method of the ternary precursor of polycrystalline form, the operation of the preparation method
It is simple and convenient, it is not high to equipment requirement, by metal salt solution via multiple inlet tubes, reaction kettle is passed into using different flow
In reacted so that the solution local reaction crystallization condition of each outlet of inlet pipe is different, so as to persistently prepare
The equally distributed second particle with a variety of primary particle forms.After the second particle finished product is prepared into final battery, because
Its with different primary particle forms advantage, so as to greatly improve the comprehensive performance of battery.
The embodiment of the invention also provides a kind of ternary precursors of polycrystalline form, use above-mentioned polycrystalline form
The preparation method of ternary precursor is prepared, and is made of the primary particle of a variety of crystal habits, integrates the excellent of each form
Point supplies mutual short slab, realizes the raising of ternary precursor comprehensive performance.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Ternary precursor of a kind of polycrystalline form of the embodiment of the present invention and preparation method thereof is carried out specifically below
It is bright.
The embodiment of the invention provides a kind of preparation methods of the ternary precursor of polycrystalline form comprising:
Metal salt solution comprising nickel ion, cobalt ions and manganese ion and liquid alkaline solution, ammonia spirit are passed into together
Hybrid reaction in reaction kettle；
Wherein, reaction kettle has multiple for being passed through the inlet tube of metal salt solution, and it is molten that multiple inlet tubes are passed through metal salt
The flow of liquid is different.
In the prior art, the presoma of ternary cell positive material is usually powdered spherical that D50 reaches 2~25 μm
Grain, in the industry referred to as second particle.And second particle is accumulated by several nanoscale primary particles, primary particle is long
Degree is 10~1000nm, and form is influenced by crystallization condition, is divided into fine and soft shape, fine acicular, fusiform, strip, plate, sheet, stick
Shape, flower-shaped etc..Different primary particle forms show apparent preference for final electrical property influence, such as: fine acicular one
Secondary particle shows preferable high rate performance, but capacity is relatively low；Plate primary particle shows preferable security performance, but multiplying power is inclined
It is low；Sheet primary particle shows preferable volumetric properties, but recycles relatively low etc..However, passing through in traditional preparation process
Temperature, ammonia density, stirring, temperature, solid content, flow, pH in control reaction kettle realize the normal preparation of ternary precursor,
The primary particle form of output is relatively simple.After being finally prepared into battery in this way, it will be influenced, can only be applicable in by the strengths and weaknesses of itself
The specific consumer field of Mr. Yu, for the product in different application direction, product needs to re-start between each other raw material exploitation and work
Skill adaptation, to increase research and development and production cost.
In view of the above-mentioned problems, the embodiment of the present invention by metal salt solution via multiple inlet tubes, be passed through using different flow
It is reacted into reaction kettle, so that the solution local reaction crystallization condition of each outlet of inlet pipe is different, so as to hold
It is continuous to prepare the equally distributed second particle with a variety of primary particle forms.The second particle finished product is prepared into final electricity
Chi Hou, because it is with the advantage of different primary particle forms, so as to greatly improve the comprehensive performance of battery.
Further, the embodiment of the present invention is mainly for the preparation of nickel-cobalt-manganternary ternary anode material, the metal salt used
Three metal ion species of nickel ion, cobalt ions and manganese ion are included at least in solution.Metal salt solution is by nickel salt, cobalt salt, manganese salt
It is mixed to get with water.Nickel salt referred herein, cobalt salt, manganese salt refer to the water soluble salt of nickel, cobalt, manganese, such as nitrate, sulphur
Hydrochlorate, chloride etc..Preferably, the concentration of metal ions of metal salt solution is 30~160g/L, is passed through the stream of metal salt solution
Amount is 200~1000L/h.Inventor has found by itself creative work, using above-mentioned concentration and range of flow, reactive crystallization
Effect it is preferable, conducive to the preferable ternary precursor of performance is obtained.
Wherein, inlet tube includes the first inlet tube, and the flow that the first inlet tube is passed through metal salt solution is 200~300L/
h；Preferably, it is 200~280L/h that the first inlet tube, which is passed through the flow of metal salt solution,.Metal liquor is in the range of flow
When, obtained primary particle form is mainly plate.
In addition, inlet tube can also include the second inlet tube, the second inlet tube be passed through metal salt solution flow be 300~
400L/h；Preferably, it is 320~380L/h that the second inlet tube, which is passed through the flow of metal salt solution,.Metal liquor is in the flow
When in range, obtained primary particle form is mainly sheet.
Inlet tube can also include third inlet tube, and the flow that third inlet tube is passed through metal salt solution is 400~700L/
h；Preferably, it is 420~680L/h that third inlet tube, which is passed through the flow of metal salt solution,.Metal liquor is in the range of flow
When, obtained primary particle form is mainly fine acicular.
Inlet tube can also include the 4th inlet tube, the 4th inlet tube be passed through metal salt solution flow be 700~
1000L/h；Preferably, it is 720~1000L/h that the 4th inlet tube, which is passed through the flow of metal salt solution,.Metal liquor is in the stream
When measuring in range, obtained primary particle form is mainly fine and soft shape.
It is worth noting that, " first, second, third, fourth " described herein is only from the range of flow of metal salt solution
Classify, does not emphasize the difference in its structure.Meanwhile the inlet tube of each type, it is not limited to one, can be two
Root or more.For example, the quantity of the first inlet tube can be multiple, the range of flow of multiple first inlet tubes 200~
280L/h.Second inlet tube, third inlet tube and the 4th inlet tube are similarly.In addition, four kinds of inlet tubes are also not required for depositing simultaneously
According to actual needs, also it can choose two or three therein.For example, can only include the first inlet tube in reaction kettle
With two kinds of third inlet tube, two kinds of forms of the main plate of obtained primary particle and fine acicular.
Further, in the embodiment of the present invention, when metal salt solution is with liquid alkaline solution, ammonia spirit hybrid reaction, temperature
It is 40~80 DEG C, pH is 10~13, and ammonia density is 2~30g/L；Preferably, liquid alkaline solution is sodium hydroxide solution and hydroxide
At least one of potassium solution, the concentration of liquid alkaline solution are 10%~35%；Preferably, the concentration of ammonia spirit be 10%~
30%.When being reacted, the flow of liquid alkaline solution is not especially limited, and needs to be adjusted at any time according to the variation of pH, to guarantee
PH is 10~13.Meanwhile the flow of ammonia spirit is also not especially limited, and needs to be adjusted at any time according to the variation of ammonia density, with
Guarantee ammonia density is 2~30g/L.
In addition, Doped ions solution can also be passed through together when being passed through metal salt solution, liquid alkaline solution and ammonia spirit
Hybrid reaction.Preferably, in Doped ions solution, the metal ion to adulterate includes magnesium ion, aluminium ion, zirconium ion, titanium
At least one of ion and tungsten ion.The concentration of Doped ions solution is that 0.1~50g/L according to circumstances can separately set feed liquor
Pipe is individually passed into reaction kettle, can also first be mixed with metal salt solution, then be passed into reaction kettle together with metal salt solution
In.Optionally, when carrying out hybrid reaction, nitrogen is passed through into reaction kettle, the flow of nitrogen is 100~1000L/h.
The embodiment of the invention also provides a kind of ternary precursors of polycrystalline form, use above-mentioned polycrystalline form
The preparation method of ternary precursor is prepared, and is made of the primary particle of a variety of crystal habits, integrates the excellent of each form
Point supplies mutual short slab, realizes the raising of ternary precursor comprehensive performance.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
The embodiment of the invention provides a kind of ternary precursor of polycrystalline form, preparation method includes:
S1. nickel nitrate, cobalt nitrate and manganese nitrate are dissolved in pure water and are mixed according to the proportion of metal molar ratio 92:6:2
It is even, obtain metal salt solution.Wherein, the concentration of metal ions of metal salt solution is 80g/L.
Aluminum nitrate, magnesium nitrate and zirconium nitrate is soluble in water, it is configured to Doped ions solution.Wherein, doped metal ion
Concentration be 0.5g/L.
The ammonia spirit that compound concentration is 10%.
The sodium hydroxide solution that compound concentration is 35%.
S2. in clean 10m3Above-mentioned ammonia spirit, hydroxide are quantitatively adding by automating PLC control system in reaction kettle
As bottom liquid, last liquid level is reached at overflow port for sodium solution and pure water, and ammonia density control 15 ± 0.5g/L, pH control 11 ±
0.05,60 ± 2 DEG C of temperature, speed of agitator 260rpm/min.
Meanwhile above-mentioned metal salt solution, Doped ions solution, ammonia spirit, sodium hydroxide solution are passed into reaction kettle
Interior carry out coprecipitation reaction, and it is passed through the nitrogen of purity >=99.99%.
Wherein, metal salt solution is passed through by 4 inlet tubes, and flow is respectively 250L/h, 350L/h, 600L/h and
900L/h.The flow of sodium hydroxide solution and ammonia spirit is fed and is adjusted, nitrogen flow by pH and ammonia density variation respectively
800L/h.Reaction process is separated by solid-liquid separation, and solid returns to be continued to grow up in reaction kettle, and it is subsequent that clear liquid is discharged into mother liquor tank waiting
Processing.After the particle size growth of solid particle is to 20.5 ± 0.5 μm, stops reaction, obtain the ternary precursor of polycrystalline form.
Embodiment 2
The embodiment of the invention provides a kind of ternary precursor of polycrystalline form, preparation method includes:
S1. nickel chloride, cobaltous sulfate and manganese sulfate are dissolved in pure water and are mixed according to the proportion of metal molar ratio 90:6:4
It is even, obtain metal salt solution.Wherein, the concentration of metal ions of metal salt solution is 100g/L.
Aluminum nitrate, magnesium nitrate and titanium chloride is soluble in water, it is configured to Doped ions solution.Wherein, doped metal ion
Concentration be 50g/L.
The ammonia spirit that compound concentration is 30%.
The potassium hydroxide solution that compound concentration is 21%.
S2. in clean 10m3Above-mentioned ammonia spirit, hydroxide are quantitatively adding by automating PLC control system in reaction kettle
As bottom liquid, last liquid level is reached at overflow port for sodium solution and pure water, and ammonia density control 25 ± 0.5g/L, pH control 12 ±
0.05,50 ± 2 DEG C of temperature, speed of agitator 300rpm/min.
Meanwhile above-mentioned metal salt solution, Doped ions solution, ammonia spirit, sodium hydroxide solution are passed into reaction kettle
Interior carry out coprecipitation reaction, and it is passed through the nitrogen of purity >=99.99%.
Wherein, metal salt solution is passed through by 4 inlet tubes, and flow is respectively 220L/h, 380L/h, 650L/h and
950L/h.The flow of potassium hydroxide solution and ammonia spirit is fed and is adjusted, nitrogen flow by pH and ammonia density variation respectively
500L/h.Reaction process is separated by solid-liquid separation, and solid returns to be continued to grow up in reaction kettle, and it is subsequent that clear liquid is discharged into mother liquor tank waiting
Processing.After the particle size growth of solid particle is to 18.0 ± 0.5 μm, stops reaction, obtain the ternary precursor of polycrystalline form.
Embodiment 3
The embodiment of the invention provides a kind of ternary precursor of polycrystalline form, preparation method includes:
S1. nickel nitrate, cobalt nitrate and manganese nitrate are dissolved in pure water and are mixed according to the proportion of metal molar ratio 94:3:3
It is even, obtain metal salt solution.Wherein, the concentration of metal ions of metal salt solution is 120g/L.
The ammonia spirit that compound concentration is 25%.
The sodium hydroxide solution that compound concentration is 20%.
S2. in clean 10m3Above-mentioned ammonia spirit, hydroxide are quantitatively adding by automating PLC control system in reaction kettle
As bottom liquid, last liquid level is reached at overflow port for sodium solution and pure water, and ammonia density control 5 ± 0.5g/L, pH control 10.5 ±
0.05,45 ± 2 DEG C of temperature, speed of agitator 250rpm/min.
Meanwhile above-mentioned metal salt solution, Doped ions solution, ammonia spirit, sodium hydroxide solution are passed into reaction kettle
Interior carry out coprecipitation reaction, and it is passed through the nitrogen of purity >=99.99%.
Wherein, metal salt solution is passed through by 4 inlet tubes, and flow is respectively 280L/h, 360L/h, 480L/h and
740L/h.The flow of sodium hydroxide solution and ammonia spirit is fed and is adjusted, nitrogen flow by pH and ammonia density variation respectively
1000L/h.Reaction process is separated by solid-liquid separation, and solid returns to be continued to grow up in reaction kettle, and it is subsequent that clear liquid is discharged into mother liquor tank waiting
Processing.After the particle size growth of solid particle is to 16.5 ± 0.5 μm, stops reaction, obtain the ternary precursor of polycrystalline form.
Comparative example 1
This comparative example provides a kind of ternary precursor, and preparation method is substantially the same manner as Example 1, and difference is, gold
Belong to salting liquid to be passed into reaction kettle with the flow of 350L/h completely.
Comparative example 2
This comparative example provides a kind of ternary precursor, and preparation method is substantially the same manner as Example 1, and difference is, gold
Belong to salting liquid to be passed into reaction kettle with the flow of 600L/h completely.
Comparative example 3
This comparative example provides a kind of ternary precursor, and preparation method is substantially the same manner as Example 1, and difference is, gold
Belong to salting liquid to be passed into reaction kettle with the flow of 250L/h completely.
Test example
Before ternary provided by polycrystalline form ternary precursor provided by Examples 1 to 3 and comparative example 1~3
It drives body and is prepared into cell positive material after the same method, its capacity, multiplying power conservation rate and circulation conservation rate are surveyed
Examination, test result are as shown in table 1.
1. test result of table
As can be seen from Table 1, the primary particle (comparative example 1) of lamellar morphology has preferable capacity, but multiplying power conservation rate
It is poor with circulation conservation rate.There is the primary particle (comparative example 2) of fine acicular form preferable multiplying power conservation rate and circulation to keep
Rate, but capacity is lower.And the ternary precursor of polycrystalline form provided by the embodiment of the present invention, then combine different crystallines
The advantages of state, that is, possess higher capacity, also possesses preferable multiplying power conservation rate and circulation conservation rate.
In conclusion the embodiment of the present invention provides a kind of preparation method of the ternary precursor of polycrystalline form, the preparation
Method it is simple to operate, it is not high to equipment requirement, it is logical using different flow by metal salt solution via multiple inlet tubes
Enter and is reacted into reaction kettle, so that the solution local reaction crystallization condition of each outlet of inlet pipe is different, so as to
Persistently prepare the equally distributed second particle with a variety of primary particle forms.The second particle finished product is prepared into final
After battery, because it is with the advantage of different primary particle forms, so as to greatly improve the comprehensive performance of battery.
The embodiment of the invention also provides a kind of ternary precursors of polycrystalline form, use above-mentioned polycrystalline form
The preparation method of ternary precursor is prepared, and is made of the primary particle of a variety of crystal habits, integrates the excellent of each form
Point supplies mutual short slab, realizes the raising of ternary precursor comprehensive performance.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of the ternary precursor of polycrystalline form characterized by comprising
Metal salt solution comprising nickel ion, cobalt ions and manganese ion is passed into together with liquid alkaline solution, ammonia spirit and is reacted
Hybrid reaction in kettle；
Wherein, the reaction kettle has multiple for being passed through the inlet tube of the metal salt solution, and multiple inlet tubes are passed through
The flow of the metal salt solution is different.
2. preparation method according to claim 1, which is characterized in that the concentration of metal ions of the metal salt solution is 30
~160g/L, the flow for being passed through the metal salt solution is 200~1000L/h.
3. preparation method according to claim 2, which is characterized in that the inlet tube includes the first inlet tube, and described the
The flow that one inlet tube is passed through the metal salt solution is 200~300L/h；Preferably, first inlet tube is passed through the gold
The flow for belonging to salting liquid is 200~280L/h.
4. preparation method according to claim 2, which is characterized in that the inlet tube includes the second inlet tube, and described the
The flow that two inlet tubes are passed through the metal salt solution is 300~400L/h；Preferably, second inlet tube is passed through the gold
The flow for belonging to salting liquid is 320~380L/h.
5. preparation method according to claim 2, which is characterized in that the inlet tube includes third inlet tube, and described
The flow that three inlet tubes are passed through the metal salt solution is 400~700L/h；Preferably, the third inlet tube is passed through the gold
The flow for belonging to salting liquid is 420~680L/h.
6. preparation method according to claim 2, which is characterized in that the inlet tube includes the 4th inlet tube, and described the
The flow that four inlet tubes are passed through the metal salt solution is 700~1000L/h；Preferably, the 4th inlet tube is passed through described
The flow of metal salt solution is 720~1000L/h.
7. preparation method according to claim 1, which is characterized in that the metal salt solution and the liquid alkaline solution, institute
When stating ammonia spirit hybrid reaction, temperature is 40~80 DEG C, and pH is 10~13, and ammonia density is 2~30g/L；Preferably, the liquid
The concentration of aqueous slkali is 10%~35%；Preferably, the concentration of the ammonia spirit is 10%~30%.
8. preparation method according to claim 1, which is characterized in that being passed through, the metal salt solution, the liquid alkaline are molten
When liquid and the ammonia spirit, it is passed through Doped ions solution hybrid reaction together；Preferably, it in the Doped ions solution, uses
Metal ion with doping includes at least one of magnesium ion, aluminium ion, zirconium ion, titanium ion and tungsten ion.
9. preparation method according to claim 1, which is characterized in that when carrying out hybrid reaction, into the reaction kettle
It is passed through nitrogen, the flow of nitrogen is 100~1000L/h.
10. a kind of ternary precursor of polycrystalline form, which is characterized in that by polycrystalline according to any one of claims 1 to 9
The preparation method of the ternary precursor of form is prepared.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111106345A (en) * | 2020-01-04 | 2020-05-05 | 华友新能源科技（衢州）有限公司 | Microcrystalline refined nickel-cobalt-manganese composite hydroxide and ternary cathode material prepared from same |
| CN113023795A (en) * | 2021-05-24 | 2021-06-25 | 昆山宝创新能源科技有限公司 | Multi-element positive electrode precursor and preparation method and application thereof |
| CN115012036A (en) * | 2022-05-31 | 2022-09-06 | 宁波容百新能源科技股份有限公司 | Fine-whisker small-particle-size nickel-cobalt-manganese hydroxide and preparation method thereof |
| CN115092974A (en) * | 2022-06-20 | 2022-09-23 | 天津巴莫科技有限责任公司 | Doped ternary precursor and preparation method thereof, ternary cathode material and lithium ion battery |
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| CN115092974B (en) * | 2022-06-20 | 2024-03-19 | 天津巴莫科技有限责任公司 | Doped ternary precursor, preparation method thereof, ternary positive electrode material and lithium ion battery |
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