CN107910550A - A kind of preparation method of continous way nickel cobalt aluminium ternary precursor - Google Patents
A kind of preparation method of continous way nickel cobalt aluminium ternary precursor Download PDFInfo
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- CN107910550A CN107910550A CN201711125675.9A CN201711125675A CN107910550A CN 107910550 A CN107910550 A CN 107910550A CN 201711125675 A CN201711125675 A CN 201711125675A CN 107910550 A CN107910550 A CN 107910550A
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- H—ELECTRICITY
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- 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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Abstract
The present invention relates to a kind of preparation method of continous way nickel cobalt aluminium ternary precursor, it includes preparing certain density metal salt solution, aluminium alkali, liquid caustic soda, ammonia spirit；It will be reacted in above-mentioned addition reaction kettle, the liquid caustic soda adds reaction kettle by upper inlet tube, and aluminium alkali adds reaction kettle by lower inlet tube, which is connected in parallel to reaction kettle；When liquid level in question response kettle is risen to close to reaction kettle cover, overflow valve is opened, reaction solution is flowed into ageing tank and is aged, until the interior liquid level of reaction kettle is concordant with overflow valve, turn off overflow valve；So circulation；It will be washed after reactant after ageing, it is dry, obtain nickel cobalt aluminium ternary precursor.The present invention is divided to the method for two inlet tube injections using liquid caustic soda, and upper inlet tube shunts a part of liquid caustic soda and enters reaction kettle, can reduce local pH in prior art reaction zone, can obviously reduce nucleus and improve D0；And flow spill valve will be adjusted to intermittently starting state by normally open.
Description
Technical field
The present invention relates to anode material for lithium-ion batteries, specifically a kind of preparation of continous way nickel cobalt aluminium ternary precursor
Method.
Background technology
With the continuous development of China's economy, science and technology, the use to the energy is consequently increased, especially industrial rapid hair
Exhibition, the consumption to battery power is larger, and the hazardous substance of generation be easy to cause the destruction of ecological environment.Therefore, country is to the energy
Use put forward higher requirements, not only require to improve the service efficiency of the energy, and to reach energy-saving and emission-reduction, strengthen nature life
The mesh of state protection.Therefore, it is particularly important to improve preparing for battery power device structure, particularly high purity battery energy and material.
At present, the production method of nickel-cobalt-manganese ternary precursor mainly adds reaction kettle at the same time using metal salt, liquid caustic soda, ammonium hydroxide
Middle to prepare generation, liquid caustic soda participates in reaction using single liquid caustic soda inlet tube injection reaction kettle in adition process, makes material in reactor
Local concentration is high, pH is too high, so that building-up process D0 is generally less than 1 μm, in continuity method preparation process, since side feed liquor becomes
Discharging so that residence time of the material in reaction kettle is different, so as to generate the normal state of the size particles of final products
Distribution.But during follow-up sintering, nucleus（Also nano sized particles are）Easily there is burning, thus be positive electrode manufacturer institute not
It is ready what is seen.Exhausting separates part nucleus when filter or drying are generally worn using filter cloth during filtering by precursor manufacturer, though energy
Meet the requirement of positive electrode manufacturer（3 μm of D0 ＞）, but loss of material is so inevitably resulted in, yield declines, so as to cause into
This rising.
Meanwhile intermittent and two kinds of continous way, wherein continous way are divided into the mode of production of lithium electricity ternary precursor at present
The mode of production occupies industry mainstream.In continous way production process, ascending particle size distribution is in normal distribution, and little particle will
All the time it is present in reaction process, and downstream client will appear from material viscosity when using short grained ternary precursor is contained
Higher situation, although to the phenomenon and insensitive in low-end market, in high-end market, this belongs to " veto by one vote "
Product defects.And during continous way prepares ternary precursor, reaction kettle feed liquor is carried out at the same time with overflow, little particle produces
The reason for be just into reaction kettle material liquid after precipitation reaction occurs, the little particle of the generation residence time mistake in reaction kettle
It is few, have little time long stool and overflow, so as to reduce product quality.
The content of the invention
In view of the above-mentioned problems, before present invention offer one kind can reduce nucleus, reduce short grained continous way nickel cobalt aluminium ternary
Drive the preparation method of body.
Technical solution is used by the present invention solves above-mentioned technical problem：A kind of continous way nickel cobalt aluminium ternary precursor
Preparation method, it includes the following steps：
（a）Prepare certain density metal salt solution, aluminium alkali, liquid caustic soda, ammonia spirit；
（b）Above-mentioned metal salt solution, aluminium alkali, liquid caustic soda, ammonia spirit are added in reaction kettle by corresponding inlet tube and reacted,
The liquid caustic soda adds reaction kettle by upper inlet tube, and aluminium alkali adds reaction kettle by lower inlet tube, and upper and lower two inlet tubes are simultaneously
It is coupled to reaction kettle；
（c）When liquid level in question response kettle is risen to close to reaction kettle cover, overflow valve is opened, reaction solution is flowed into ageing tank and carries out
Ageing, until the interior liquid level of reaction kettle is concordant with overflow valve, turns off overflow valve；So circulation；
（d）It will be washed after reactant after ageing, it is dry, obtain nickel cobalt aluminium ternary precursor.
Preferably, the concentration of the ammonia spirit is 12-25g/L, it is 10-11.5 to control the pH in reaction kettle.
Preferably, described, the flow-rate ratio of solution is 1 in two inlet tubes up and down：（0.1-10）.
Preferably, continuing to be passed through nitrogen into the reaction kettle, open agitating paddle and realize stirring, the agitating paddle both ends
The upper strata agitating paddle and lower floor's agitating paddle positioned at lower end, the mixing speed for controlling the agitating paddle being divided into positioned at upper end are 50-
200r/min。
Preferably, the lower inlet tube of conveying aluminum alkali is arranged on same level with metal salt solution inlet tube, ammonium hydroxide inlet tube
Position, and at lower floor's agitating paddle, the upper inlet tube for conveying liquid caustic soda is located at the agitating paddle of upper strata.
Preferably, when reacting in a kettle, the temperature for controlling the reaction kettle is 40-80 DEG C, and material is in reaction kettle
When interior mean residence time is 5-20 small.
Preferably, digestion time is 30-120min, wash time 60-240min, when drying time is 7-8 small.
Preferably, in the reaction kettle close to reaction kettle cover at and the overflow port of reaction kettle at be both provided with liquid level pass
Sensor, the overflow port are provided with overflow valve, and when the liquid level sensor at reaction kettle cover senses reaction solution, which will
Signal is sent to controller control overflow valve and opens, and reaction solution flows into ageing tank by overflow valve and is aged；Liquid at overflow port
When level sensor does not sense reaction solution, which transmits signals to controller control overflow valve and closes.
Compared with prior art, the invention has the advantages that：
1st, technique is simple, cost is low, easy to operate, energy conservation and environmental protection, and the nickle cobalt lithium manganate being synthesized is uniform in size, prepared by back segment
Anode material of lithium battery performance is good, is conducive to the producing line yield of lithium battery product；
2nd, it is divided to the method for two inlet tube injections using liquid caustic soda, upper inlet tube shunts a part of liquid caustic soda and enters reaction kettle, can make existing
There is local pH in technology reaction zone to reduce, can obviously reduce nucleus and improve D0；
3rd, controlling reaction zone pH to reduce makes nucleation quantity few and easily grows up, and to ensure liquid caustic soda total flow, the invention is being reacted
Kettle top is filled into the aluminium lye alkali number in lower part reduction by upper inlet tube, maintains whole reaction balance；
4th, the ternary precursor nickle cobalt lithium manganate prepared using this method can meet that producer's cost is low and consumer product is distributed at the same time
Narrow demand, market potential are big.
5th, in the present invention, flow spill valve is adjusted to intermittently starting state by normally open.Since overflow port is away from reaction kettle
Lid also has a distance, and closing overflow port can't soon result in reaction kettle and emit groove.Overflow port is closed, extends little particle and is reacting
The residence time of kettle, when question response kettle liquid position is risen to close to reaction kettle cover, opens overflow valve up to liquid level and overflow valve in kettle
Concordantly, overflow valve is turned off at this time, and so circulation carries out.Since mean residence time of the little particle in reaction kettle is shown
Write and extend, this will substantially reduce the quantity of final products small particles.
Embodiment
The present invention is described more detail below, illustrative examples of the invention and explanation are used for explaining the present invention herein,
It is but not as a limitation of the invention.
A kind of preparation method of continous way nickel cobalt aluminium ternary precursor, with metal salt solution, aluminium alkali, liquid caustic soda and ammonia spirit
As raw material, reacted using the uninterrupted cocurrent feed liquor of four inlet tubes to reaction kettle, and by control solution injection rate size,
The parameters such as pH value, reaction temperature, mixing speed, effectively control lithium electricity ternary precursor chemical impurity and crystal structure degree, granularity,
Density etc., through being aged, washing, centrifuging after synthesis, finally obtains the ternary precursor nickle cobalt lithium manganate of continous way.
It should be noted that the flow-rate ratio of two inlet tubes is 1 above and below the invention：0.1 ~ 10, can be enterprising herein
Liquid pipe and the flow-rate ratio of lower inlet tube are 1：0.1~10；Can also be lower inlet tube and the flow-rate ratio of upper inlet tube is 1：0.1~
10, reduction nucleus number can be reached and improve the effect of nucleus diamter.
The preparation method of continous way nickel cobalt aluminium ternary precursor provided by the invention, is divided to two inlet tube injections using liquid caustic soda
Method, to traditional preparation method --- be improved only with a liquid caustic soda inlet tube, there is provided one kind can continuous production, steady
Qualitative nickel cobalt aluminium ternary precursor material strong, nucleus is few, nucleus diamter is big.
In the preparation method of nickel cobalt aluminium ternary precursor, the metal salt solution, liquid caustic soda and ammonia spirit enter reaction
The kettle and position mixed is referred to as reaction zone, reaction zone are most critical zones in reaction kettle, reaction zone pH high then easily nucleation or into
Nuclear volume is more, and reaction zone pH is few then easily to grow up or to be nucleated quantity few.The invention keeps other conditions constant, using aluminium alkali and liquid
Alkali is divided to the method for two inlet tubes injection to reduce the liquid caustic soda amount of reaction zone, can be significantly reduced to nuclear volume or allow new nucleation
Grow up as early as possible, so as to achieve the purpose that to improve D0.Inlet tube feed liquor, which is mainly responsible for, in the invention, on liquid caustic soda adjusts whole system
PH, lower liquid caustic soda pipe feed liquor are mainly responsible for direct synthetic reaction, and since the liquid caustic soda amount for directly participating in reaction is reduced, local pH is lower
（Possibly lower than equalization point）, new nucleus once being formed, all can to grow up rapidly than original considerably more rapid speed so that
Reach and significantly reduce nucleus, the purpose that D0 can also be significantly improved.The invention is participated in anti-using two inlet tubes of liquid caustic soda and aluminium alkali
At once, building-up process D0 can allow D0 to bring up to more than 3 μm at least above 1.5 μm, then by follow-up ageing process.
With three embodiments, the present invention is described in detail below.
Embodiment one：Aluminium alkali that metal salt solution that compound concentration is 120g/L, concentration are 4g/L, concentration are 32g/L's
Liquid caustic soda, the ammonia spirit that concentration is 12g/L；Above-mentioned metal salt solution, liquid caustic soda, ammonia spirit are added by corresponding inlet tube
It is 5m to enter size3Reaction kettle in react；The liquid caustic soda adds reaction kettle by upper inlet tube, and aluminium alkali is added by lower inlet tube
Reaction kettle, upper and lower two inlet tubes are connected in parallel to reaction kettle, and the flow of upper inlet tube is 60L/h, and the flow of lower inlet tube is
20L/h；It is 10 to control the pH in reaction kettle, the temperature of reaction kettle is 40 DEG C, mean residence time of the material in reaction kettle is 5
Hour, continue to be passed through nitrogen into the reaction kettle, open agitating paddle and realize stirring, the agitating paddle both ends are divided into positioned at upper end
Upper strata agitating paddle and lower floor's agitating paddle positioned at lower end, the mixing speed for controlling the agitating paddle be 50r/min, aluminium alkali
Lower inlet tube is arranged on the same horizontal position with metal salt solution inlet tube, ammonium hydroxide inlet tube, and at lower floor's agitating paddle, liquid caustic soda
Upper inlet tube be located at the agitating paddle of upper strata,；When liquid level in question response kettle is risen to close to reaction kettle cover, overflow valve is opened,
Make reaction solution flow into ageing tank to be aged, until the interior liquid level of reaction kettle is concordant with overflow valve, turn off overflow valve；So follow
Ring；The reactant in ageing tank is set to be aged 30min again；Wash 60min；After when drying 7 is small, nickel cobalt aluminium ternary precursor is obtained.
Ternary precursor is made from the prior art：D0：0.32； D10：5.54；D50：9.85；D90：16.66；With institute
The method products obtained therefrom for stating embodiment one is：D0：0.32 ；D10：5.54 ；D50：9.85 ；D90：16.66.
Embodiment two：Aluminium alkali that metal salt solution that compound concentration is 120g/L, concentration are 6g/L, concentration are 32g/L's
Liquid caustic soda, the ammonia spirit that concentration is 25g/L；Above-mentioned metal salt solution, liquid caustic soda, ammonia spirit are added by corresponding inlet tube
It is 5m to enter size3Reaction kettle in react；The liquid caustic soda adds reaction kettle by upper inlet tube, and aluminium alkali is added by lower inlet tube
Reaction kettle, upper and lower two inlet tubes are connected in parallel to reaction kettle, and the flow of upper inlet tube is 40L/h, and the flow of lower inlet tube is
20L/h；It is 11.5 to control the pH in reaction kettle, the temperature of reaction kettle is 80 DEG C, mean residence time of the material in reaction kettle
For 20 it is small when, continue to be passed through nitrogen into the reaction kettle, open agitating paddle and realize stirring, the agitating paddle both ends, which are divided into, to be located at
The upper strata agitating paddle of upper end and lower floor's agitating paddle positioned at lower end, the mixing speed for controlling the agitating paddle are 200r/min, aluminium
The lower inlet tube of alkali is arranged on the same horizontal position with metal salt solution inlet tube, ammonium hydroxide inlet tube, and at lower floor's agitating paddle,
The upper inlet tube of liquid caustic soda is located at the agitating paddle of upper strata；When liquid level in question response kettle is risen to close to reaction kettle cover, overflow is opened
Valve, makes reaction solution flow into ageing tank and is aged, until the interior liquid level of reaction kettle is concordant with overflow valve, turn off overflow valve；Such as
This circulation；The reactant in ageing tank is set to be aged 120min again；Wash 240min；After when drying 8 is small, before obtaining nickel cobalt aluminium ternary
Drive body.
Ternary precursor is made from the prior art：D0：0.32； D10：5.54；D50：9.85；D90：16.66；With institute
The method products obtained therefrom for stating embodiment two is：D0：0.31 ；D10：5.50 ；D50：9.73 ；D90：16.42.
Embodiment three：Aluminium alkali that metal salt solution that compound concentration is 120g/L, concentration are 5g/L, concentration are 32g/L's
Liquid caustic soda, the ammonia spirit that concentration is 20g/L；Above-mentioned metal salt solution, liquid caustic soda, ammonia spirit are added by corresponding inlet tube
It is 5m to enter size3Reaction kettle in react；The liquid caustic soda adds reaction kettle by upper inlet tube, and aluminium alkali is added by lower inlet tube
Reaction kettle, upper and lower two inlet tubes are connected in parallel to reaction kettle, and the flow of upper inlet tube is 10L/h, and the flow of lower inlet tube is
50L/h；It is 11 to control the pH in reaction kettle, the temperature of reaction kettle is 60 DEG C, mean residence time of the material in reaction kettle is
10 it is small when, continue to be passed through nitrogen into the reaction kettle, open agitating paddle and realize stirring, the agitating paddle both ends are divided into positioned at upper
The upper strata agitating paddle at end and lower floor's agitating paddle positioned at lower end, the mixing speed for controlling the agitating paddle are 150r/min, aluminium alkali
Lower inlet tube and metal salt solution inlet tube, ammonium hydroxide inlet tube be arranged on the same horizontal position, and be located at lower floor's agitating paddle, liquid
The upper inlet tube of alkali is located at the agitating paddle of upper strata；When liquid level in question response kettle is risen to close to reaction kettle cover, overflow valve is opened,
Make reaction solution flow into ageing tank to be aged, until the interior liquid level of reaction kettle is concordant with overflow valve, turn off overflow valve；So follow
Ring；The reactant in ageing tank is set to be aged 80min again；Wash 180min；After when drying 7.5 is small, nickel cobalt aluminium ternary forerunner is obtained
Body.
Ternary precursor is made from the prior art：D0：0.32； D10：5.54；D50：9.85；D90：16.66；With institute
The method products obtained therefrom for stating embodiment three is：D0：0.30 ；D10：5.56 ；D50：9.805 ；D90：16.62.
The technical solution provided above the embodiment of the present invention is described in detail, specific case used herein
The principle and embodiment of the embodiment of the present invention are set forth, the explanation of above example is only applicable to help and understands this
The principle of inventive embodiments；Meanwhile for those of ordinary skill in the art, according to the embodiment of the present invention, in specific embodiment party
There will be changes in formula and application range, in conclusion this specification content should not be construed as limiting the invention.
Claims (8)
1. a kind of preparation method of continous way nickel cobalt aluminium ternary precursor, it includes the following steps：
（a）Prepare certain density metal salt solution, aluminium alkali, liquid caustic soda, ammonia spirit；
（b）Above-mentioned metal salt solution, aluminium alkali, liquid caustic soda, ammonia spirit are added in reaction kettle by corresponding inlet tube and reacted,
The liquid caustic soda adds reaction kettle by upper inlet tube, and aluminium alkali adds reaction kettle by lower inlet tube, and upper and lower two inlet tubes are simultaneously
It is coupled to reaction kettle；
（c）When liquid level in question response kettle is risen to close to reaction kettle cover, overflow valve is opened, reaction solution is flowed into ageing tank and carries out
Ageing, until the interior liquid level of reaction kettle is concordant with overflow valve, turns off overflow valve；So circulation；
（d）It will be washed after reactant after ageing, it is dry, obtain nickel cobalt aluminium ternary precursor.
2. the preparation method of continous way nickel cobalt aluminium ternary precursor according to claim 1, it is characterised in that：The ammonium hydroxide is molten
The concentration of liquid is 12-25g/L, and it is 10-11.5 to control the pH in reaction kettle.
3. the preparation method of continous way nickel cobalt aluminium ternary precursor according to claim 1, it is characterised in that：Two above and below described
The flow-rate ratio of solution is 1 in root inlet tube：（0.1-10）.
4. the preparation method of continous way nickel cobalt aluminium ternary precursor according to claim 1, it is characterised in that：Continue to described
Be passed through nitrogen in reaction kettle, open agitating paddle and realize stirring, the agitating paddle both ends be divided into positioned at upper end upper strata agitating paddle and
Lower floor's agitating paddle positioned at lower end, the mixing speed for controlling the agitating paddle are 50-200r/min.
5. the preparation method of continous way nickel cobalt aluminium ternary precursor according to claim 4, it is characterised in that：Conveying aluminum alkali
Lower inlet tube is arranged on the same horizontal position with metal salt solution inlet tube, ammonium hydroxide inlet tube, and at lower floor's agitating paddle, conveying
The upper inlet tube of liquid caustic soda is located at the agitating paddle of upper strata.
6. the preparation method of continous way nickel cobalt aluminium ternary precursor according to claim 1, it is characterised in that：In a kettle
During reaction, the temperature for controlling the reaction kettle is 40-80 DEG C, when mean residence time of the material in reaction kettle is 5-20 small.
7. the preparation method of continous way nickel cobalt aluminium ternary precursor according to claim 1, it is characterised in that：Digestion time is
30-120min, wash time 60-240min, when drying time is 7-8 small.
8. the preparation method of continous way nickel cobalt aluminium ternary precursor according to claim 1, it is characterised in that：In the reaction
Close to reacting at kettle cover and being both provided with liquid level sensor at the overflow port of reaction kettle in kettle, the overflow port is provided with overflow
Valve, when the liquid level sensor at reaction kettle cover senses reaction solution, which transmits signals to controller control overflow
Valve is opened, and reaction solution flows into ageing tank by overflow valve and is aged；Liquid level sensor at overflow port does not sense reaction solution
When, which transmits signals to controller control overflow valve and closes.
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| CN109502657A (en) * | 2018-12-26 | 2019-03-22 | 柳州申通汽车科技有限公司 | A kind of preparation method of continous way nickel-cobalt-manganese ternary presoma |
| CN109574094A (en) * | 2019-01-24 | 2019-04-05 | 广东迈纳科技有限公司 | A kind of preparation method of stable particle size and its distribution nickel cobalt aluminium hydroxide |
| CN109847683A (en) * | 2019-02-27 | 2019-06-07 | 中机国际工程设计研究院有限责任公司 | Reaction kettle is used in ternary anode material precursor preparation |
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| CN110600683A (en) * | 2018-06-13 | 2019-12-20 | 浙江帕瓦新能源股份有限公司 | Preparation method of semi-continuous ternary precursor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110600683A (en) * | 2018-06-13 | 2019-12-20 | 浙江帕瓦新能源股份有限公司 | Preparation method of semi-continuous ternary precursor |
| CN110600683B (en) * | 2018-06-13 | 2020-07-31 | 浙江帕瓦新能源股份有限公司 | Preparation method of semi-continuous ternary precursor |
| CN109502657A (en) * | 2018-12-26 | 2019-03-22 | 柳州申通汽车科技有限公司 | A kind of preparation method of continous way nickel-cobalt-manganese ternary presoma |
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| CN109574094B (en) * | 2019-01-24 | 2022-03-08 | 广东迈纳科技有限公司 | Preparation method of nickel-cobalt-aluminum hydroxide with stable particle size and particle size distribution |
| CN109847683A (en) * | 2019-02-27 | 2019-06-07 | 中机国际工程设计研究院有限责任公司 | Reaction kettle is used in ternary anode material precursor preparation |
| CN110510678A (en) * | 2019-09-25 | 2019-11-29 | 湖南双富新材料科技有限公司 | A kind of preparation method of efficient mixing ternary precursor |
| CN110611097A (en) * | 2019-09-25 | 2019-12-24 | 湖南双富新材料科技有限公司 | Preparation method of high-nickel ternary precursor |
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