CN110510678A - A kind of preparation method of efficient mixing ternary precursor - Google Patents
A kind of preparation method of efficient mixing ternary precursor Download PDFInfo
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- CN110510678A CN110510678A CN201910913413.1A CN201910913413A CN110510678A CN 110510678 A CN110510678 A CN 110510678A CN 201910913413 A CN201910913413 A CN 201910913413A CN 110510678 A CN110510678 A CN 110510678A
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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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- 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
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Abstract
The present invention relates to anode material for lithium-ion batteries technical fields, and disclose a kind of preparation method of efficiently mixing ternary precursor, specifically the preparation method is as follows: preparing metal salting liquid, liquid alkaline and ammonia spirit；The liquid alkaline, metal salt solution and ammonia spirit of preparation are added separately in reaction kettle by inlet tube, and mixed；Maturation slot material and reaction kettle Matter Transfer are linked, when the liquid level in maturation slot rises to setting liquid level, maturation slot material is delivered in filters pressing dashpot.The preparation method of the efficient mixing ternary precursor, simple process, at low cost, high degree of automation and energy conservation and environmental protection, the nickel cobalt manganese presoma inside solid being synthesized, good sphericity, the anode material of lithium battery performance of back segment preparation is good, is conducive to the raising of the compacted density of lithium battery product；Be divided to two inlet tubes injection circulating pumps using liquid alkaline and ammonium hydroxide, metal salt solution reaction kettle entered by ejector, it can be achieved that reaction zone liquid.
Description
Technical field
The present invention relates to field of lithium ion battery anode, more particularly to a kind of preparation of efficiently mixing ternary precursor
Method.
Background technique
With the continuous development of global economy and science and technology, the serious of conventional petroleum and Coal Energy Source non-renewable energy resources is caused
Consumption, the harmful substance generated in traditional energy consumption process be easy to cause the destruction and global greenhouse effect of ecological environment
Should be obvious, therefore, China puts forward higher requirements the use of the energy, the service efficiency for improving the energy is not only required, but also
Achieve the effect that energy-saving and emission-reduction, and with reaching the mesh for reinforcing natural ecology protection, therefore, the field of new energy is applied
It is promoted to China's strategic level, and lithium ion battery is as the most important thing in new energy application, the system of high purity battery energy and material
It is standby particularly important, as the presoma of most critical in battery material cathode performance, how to realize product quality stability, guarantees to produce
Quality becomes cardinal task.
The production method material in reactor small grain size material of nickel-cobalt-manganese ternary precursor is because of the presence of slurry shearing power at present
The upper limit causes small grain size material not fine and close enough, and small grain size internal voids degree is higher, some particles there are obvious inner vacuum shape,
Cause positive electrode tap density that higher level is not achieved, to influence the compacted density of battery material.
Summary of the invention
(1) goal of the invention
To solve technical problem present in background technique, the present invention proposes a kind of preparation side of efficiently mixing ternary precursor
Method.
(2) technical solution
To solve the above problems, the present invention provides a kind of preparation method of efficiently mixing ternary precursor, specific preparation method
It is as follows:
S1, preparing metal salting liquid, liquid alkaline and ammonia spirit；
S2, the liquid alkaline, metal salt solution and ammonia spirit of preparation are added separately in reaction kettle by inlet tube, and mixed；
S3, maturation slot material and reaction kettle Matter Transfer are linked, it, will be ripe when the liquid level in maturation slot rises to setting liquid level
Grooving material is delivered in filters pressing dashpot；
S4, the reactant after maturation is aged, is washed and is dried, and obtain nickel cobalt aluminium ternary precursor.
Preferably, the concentration of ammonia spirit is 12-25g/L, and controlling the pH value in reaction kettle is 10-12.
Preferably, in S3, pump flow and molten metal feed rate are than controlling the nozzle flow velocity control in 20-30:1
System is in 15-25m/s.
Preferably, in S2, the inert gas that regime flow is passed through in reaction kettle is subjected to atmosphere protection, and open stirring
Paddle is stirred, and agitating paddle is two layers of Axial-flow stirrer in upper, and lower layer is turbine impellers, and the mixing speed for controlling agitating paddle is 50-
200r/min。
Preferably, the ejector outlet for conveying metal salt solution is located at third layer blade oblique upper, conveys liquid alkaline and ammonium hydroxide
Inlet tube is located at before pump and bottom valve middle, and circulation liquid outlet is connected to reaction kettle.
Preferably, in S3, when reacting in a kettle, controlling the temperature inside reaction kettle is 40-80 DEG C, and material is anti-
Answering the mean residence time in kettle is 10-25 hours.
Preferably, in S4, digestion time 60-180min, wash time 60-200min, drying time are that 4-6 is small
When.
Preferably, in S3, it is respectively provided with radar level sensor at the upper cover of upper cover and maturation slot in reaction kettle, is overflow
Head piece is equipped with overflow valve, when maturation tank liquor position reaches setting value, automatically turns on maturation slot bottom valve and slurry returns to pump, when ripe
When grooving liquid level reaches the second setting value, opens slurry return pump and remove filters pressing dashpot automatic valve, reach the first level set value
When close；Realize reaction automatically-controlled continuous.
Compared with prior art, the invention has the following advantages:
1, simple process, at low cost, high degree of automation and energy conservation and environmental protection, the nickel cobalt manganese presoma inside solid being synthesized,
The anode material of lithium battery performance of good sphericity, back segment preparation is good, is conducive to the raising of the compacted density of lithium battery product.
2, it is divided to two inlet tube injection circulating pumps using liquid alkaline and ammonium hydroxide, metal salt solution enters reaction by ejector
Kettle, it can be achieved that reaction zone liquid.
3, control reaction zone pH reduction keeps nucleation quantity few and easily grows up.
4, meet that producer is at low cost and client produces simultaneously using the ternary precursor nickel cobalt manganese forerunner physical efficiency of this method preparation
The demand of product high-tap density, great market potential.
Detailed description of the invention
Fig. 1 is flow diagram prepared by the present invention.
Specific embodiment
In order to make the objectives, technical solutions and advantages of the present invention clearer, With reference to embodiment and join
According to attached drawing 1, the present invention is described in more detail.It should be understood that these descriptions are merely illustrative, and it is not intended to limit this hair
Bright range.In addition, in the following description, descriptions of well-known structures and technologies are omitted, to avoid this is unnecessarily obscured
The concept of invention.
In the invention, using metal salt solution, liquid alkaline and ammonia spirit as raw material, feed liquor is uninterruptedly shunted using inlet tube
It is reacted to reaction kettle, the dispersion for realizing solution molecule grade is fed by metal salt jetting type, and pass through control solution injection rate
The parameters such as size, pH value, reaction temperature and mixing speed, effectively control lithium electricity ternary precursor chemical impurity, crystal structure degree,
Granularity and density etc. finally obtain continuous ternary precursor through ageing, washing and centrifugation after synthesis.
It is straight only with inlet tube to traditional preparation method by the way of being fed before liquid alkaline and aqua ammonia pump in the invention
The feed liquor mode for tapping into reaction kettle carries out dispersion by stirring and easily causes part uneven.
In the invention, metal salt solution enters reaction kettle and mixed position is referred to as reaction zone, and reaction zone is reaction kettle
Interior most critical zone, reaction zone dispersing shear power is small to be easy to cause nucleus, the small then Yi Chang great of reaction zone pH numerical value or nucleation quantity
Few, other conditions are constant, greatly improved by the linear velocity and shearing force of the fluid of reaction zone, in turn using the method for jet reaction
It is substantially reduced crystalline core size, to achieve the purpose that improve nucleus consistency and ball-type degree.
In the invention, due to fluid through ejector nozzle formed high-velocity fluid, metal salt solution through volume inhale after with high velocity stream
Body is mixed reaction, and the cutter shearing line speed that fluid is formed is 3 times or more of current volume production reaction kettle, and the feed pressure with pump
Power and jet size are related, when greatly reducing crystalline core size and sphericity, and being reacted using jet mixing mode, synthesis process
D50 is compared with traditional handicraft compared to initial particle size integrally low 1/2, and tap density is than traditional big 0.2g/cm3.
With two embodiments, the present invention is described in detail below:
Embodiment one: the ammonia that liquid alkaline that metal salt solution that compound concentration is 120g/L, concentration are 6mol/L, concentration are 20g/L
Aqueous solution；The reaction kettle that size is 10m3 is added by corresponding inlet tube in above-mentioned metal salt solution, liquid alkaline, ammonia spirit
Middle reaction；Metal salt is in such a way that jet stream is fed, and jet stream pump discharge 20m3/h, NCM liquid inventory rate control is in 0.5m3/
h；PH value in control reaction kettle is 11.8, the temperature of reaction kettle is 500 degree, mean residence time of the material in reaction kettle is
25 hours, continuing to be passed through nitrogen into reaction kettle, opens agitating paddle and realize stirring, agitating paddle is two layers of Axial-flow stirrer leaf in upper, under
Layer turbine impellers, the mixing speed for controlling agitating paddle is 150r/min, and reaction mass is pumped into filters pressing dashpot and cures 60min；
Wash 80min；After 4 hours dry, nickel-cobalt-manganese ternary presoma is obtained.
Ternary precursor initial reaction granularity made from the prior art are as follows: D10:1.434um, D502.635um, D90:
3.536um D100:4.933；TD1.5g/cm3, with the method gained initial particle size of embodiment one are as follows: D10:0.683um, D50:
1.274um, D90:2.426um, D100:3.014um, 2.15g/cm3.
Embodiment two: liquid alkaline that metal salt solution that compound concentration is 120g/L, concentration are 6mol/L, concentration 20g/L
Ammonia spirit；It is the anti-of 10m3 that size, which is added, by corresponding inlet tube in above-mentioned metal salt solution, liquid alkaline, ammonia spirit
It answers in kettle and reacts；In such a way that jet stream is fed, pump flow 30m3/h, NCM liquid inventory is controlled in 1m3/h metal salt；
PH value in control reaction kettle is 11.5, the temperature of reaction kettle is 500, mean residence time of the material in reaction kettle is 20 small
When, continue to be passed through nitrogen into reaction kettle, opens agitating paddle and realize stirring, agitating paddle is two layers of Axial-flow stirrer leaf in upper, lower layer whirlpool
Blade is taken turns, the mixing speed for controlling agitating paddle is 120r/min, and reaction mass is pumped into filters pressing dashpot and cures 60min；Washing
80min；After 4 hours dry, nickel-cobalt-manganese ternary presoma is obtained.
Ternary precursor made from the prior art are as follows: D10:1.643um, D50:3.687um, D90:4.993um,
D1005.652；The method products obtained therefrom of TD:1.4g/cm3 embodiment two is D10:0.868um, D50:1.986um, D90:
2.833um, D100:3.287um, TD:2.1g/cm3.
It should be understood that above-mentioned specific embodiment of the invention is used only for exemplary illustration or explains of the invention
Principle, but not to limit the present invention.Therefore, that is done without departing from the spirit and scope of the present invention is any
Modification, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.In addition, appended claims purport of the present invention
Covering the whole variations fallen into attached claim scope and boundary or this range and the equivalent form on boundary and is repairing
Change example.
Claims (8)
1. a kind of preparation method of efficiently mixing ternary precursor, which is characterized in that it is specific the preparation method is as follows:
S1, preparing metal salting liquid, liquid alkaline and ammonia spirit；
S2, the liquid alkaline, metal salt solution and ammonia spirit of preparation are added separately in reaction kettle by inlet tube, and mixed；
S3, maturation slot material and reaction kettle Matter Transfer are linked, it, will be ripe when the liquid level in maturation slot rises to setting liquid level
Grooving material is delivered in filters pressing dashpot；
S4, the reactant after maturation is aged, is washed and is dried, and obtain nickel cobalt aluminium ternary precursor.
2. a kind of preparation method of efficiently mixing ternary precursor according to claim 1, it is characterised in that: ammonia spirit
Concentration be 12-25g/L, control reaction kettle in pH value be 10-12.
3. a kind of preparation method of efficiently mixing ternary precursor according to claim 1, it is characterised in that: in S3,
Pump flow and molten metal feed rate are than controlling in 20-30:1, and nozzle flow control is in 15-25m/s.
4. a kind of preparation method of efficiently mixing ternary precursor according to claim 1, it is characterised in that: in S2,
The inert gas for being passed through regime flow in reaction kettle is subjected to atmosphere protection, and opens agitating paddle and is stirred, agitating paddle is upper
In two layers of Axial-flow stirrer, lower layer is turbine impellers, control agitating paddle mixing speed be 50-200r/min.
5. a kind of preparation method of efficiently mixing ternary precursor according to claim 4, it is characterised in that: conveying metal
The ejector outlet of salting liquid is located at third layer blade oblique upper, conveys liquid alkaline and ammonium hydroxide inlet tube is located at before pump and bottom
Valve middle, circulation liquid outlet are connected to reaction kettle.
6. a kind of preparation method of efficiently mixing ternary precursor according to claim 1, it is characterised in that: in S3,
When reacting in a kettle, controlling temperature inside the reaction kettle is 40-80 DEG C, when average stop of the material in reaction kettle
Between be 10-25 hours.
7. a kind of preparation method of efficiently mixing ternary precursor according to claim 1, it is characterised in that: in S4,
Digestion time is 60-180min, and wash time 60-200min, drying time is 4-6 hours.
8. a kind of preparation method of efficiently mixing ternary precursor according to claim 1, it is characterised in that: in S3,
It is respectively provided with radar level sensor at the upper cover of upper cover and maturation slot in reaction kettle, overflow port is equipped with overflow valve, when ripe
When grooving liquid level reaches setting value, automatically turns on maturation slot bottom valve and slurry returns to pump, when maturation tank liquor position reaches the second setting
When value, opens slurry return pump and go filters pressing dashpot automatic valve, closing when reaching the first level set value；Realize reaction continuously certainly
Dynamic control.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114931919A (en) * | 2022-04-08 | 2022-08-23 | 成都思达能环保设备有限公司 | Positive electrode material precursor coprecipitation reaction equipment and coprecipitation reaction system |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107910550A (en) * | 2017-11-16 | 2018-04-13 | 湖南中伟新能源科技有限公司 | A kind of preparation method of continous way nickel cobalt aluminium ternary precursor |
| CN208385525U (en) * | 2018-04-25 | 2019-01-15 | 纳威科技（深圳）有限公司 | A kind of equipment continuously preparing ternary material |
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- 2019-09-25 CN CN201910913413.1A patent/CN110510678A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107910550A (en) * | 2017-11-16 | 2018-04-13 | 湖南中伟新能源科技有限公司 | A kind of preparation method of continous way nickel cobalt aluminium ternary precursor |
| CN208385525U (en) * | 2018-04-25 | 2019-01-15 | 纳威科技（深圳）有限公司 | A kind of equipment continuously preparing ternary material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114931919A (en) * | 2022-04-08 | 2022-08-23 | 成都思达能环保设备有限公司 | Positive electrode material precursor coprecipitation reaction equipment and coprecipitation reaction system |
| CN114931919B (en) * | 2022-04-08 | 2024-03-22 | 成都思达能环保设备有限公司 | Positive electrode material precursor coprecipitation reaction equipment and coprecipitation reaction system |
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Application publication date: 20191129 |