CN108557904A - A kind of gradient mixes the preparation method of aluminium cobaltosic oxide - Google Patents
A kind of gradient mixes the preparation method of aluminium cobaltosic oxide Download PDFInfo
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- CN108557904A CN108557904A CN201810489262.7A CN201810489262A CN108557904A CN 108557904 A CN108557904 A CN 108557904A CN 201810489262 A CN201810489262 A CN 201810489262A CN 108557904 A CN108557904 A CN 108557904A
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Abstract
The invention discloses the preparation methods that a kind of gradient mixes aluminium cobaltosic oxide, belong to technical field of lithium ion.This method is using a certain concentration cobalt liquor as cobalt source, sodium hydroxide solution is precipitating reagent, ammonia spirit is complexing agent, hydrogen peroxide solution is oxidant, aluminium salt ethanol solution is doped solution, during the reaction, it will participate in reacting in doped solution addition reaction kettle by disperseing liquid feeding mode, a step prepares gradient and mixes aluminium cobaltosic oxide product.After the present invention utilizes ethanol solution need miscible with water, aluminium salt could participate in the characteristic of reaction, slow down Al3+Settling rate, solve due to Al (OH)3The problem of solubility product constant is too small and reacts violent, and aluminium cannot be co-precipitated with cobalt ensure that and prepare being uniformly distributed for aluminium element in product.The aluminium cobaltosic oxide product of mixing for using that the method for the present invention prepares mixes aluminum amount for 0.5 1.0%, and aluminium element is uniformly distributed in gradient, and laser particle size is 58 μm, Zhen Shi Mi Du≤2.5g/cm3, 1.0 3.0m of specific surface area2/ g, in blocky or spherical pattern.
Description
Technical field
The invention belongs to technical field of lithium ion, specifically a kind of to be used to prepare ion cell anode material lithium cobaltate
The gradient of lithium mixes the preparation method of aluminium cobaltosic oxide.
Background technology
Cobalt acid lithium is the main positive electrode in current commercial Li-ion battery.But cobalt acid lithium actual specific capacity only has
140mAh/g or so, only its theoretical capacity（274mAh/g）50% or so；And the anti-over-charging performance of cobalt acid lithium is poor, compared with
Specific capacity reduces rapidly under high charge voltage.Research has shown that, is improving anode material for lithium-ion batteries performance, especially cyclicity
Energy aspect, doping is one of most efficient method, can not only improve the stability of ionic lattice, but also can increase substantially
The cycle performance of material.
Existing doping cobalt acid lithium production technology mainly mixes doped chemical oxide, cobaltosic oxide, lithium carbonate,
Grinding, high-temperature calcination.This method not only high energy consumption, and Elemental redistribution is uneven in the cobalt acid lithium product prepared, consistency
Difference cannot meet requirement of the battery industry to doping cobalt acid lithium.
Chinese invention patent（201210486483.1）" a kind of preparation method of doping spherical cobaltosic oxide " is disclosed,
Specifically doped chemical ion is incorporated into cobalt salt solution and is configured to doping mixed solution, with hydroxide solution and air
It is passed into reaction unit simultaneously, and is stirred continuously and is reacted, prepare doping spherical cobaltosic oxide.Chinese invention patent
（CN200810110753.2）" a kind of preparation method of doped cobaltic-cobaltous oxide " is disclosed, specifically mixes doped chemical ion
Enter to be configured to doping mixed solution into cobalt salt solution, is passed into reaction unit simultaneously with the hydroxide solution containing ammonium hydroxide
Make its reaction, doping spherical cobaltosic oxide is prepared using washing, drying, calcining.Four oxidations prepared in above-mentioned patent
Gradient distribution cannot be presented in doped chemical in three cobalts.
In view of the above technical problems, the Chinese invention patent of 107768646 A of Publication No. CN discloses a kind of " doping
The cobaltosic oxide preparation method of graded elemental distribution ", this method will synthesis by way of hydrogen peroxide is added into reaction kettle
Product is direct oxidation into cobaltosic oxide, and without calcining, liquid phase one-step has synthesized the cobaltosic oxide product that gradient mixes aluminium.
But this method, there are aluminium salt and alkaline reaction speed are fast, aluminium and cobalt precipitation are uneven, so as to cause member is adulterated in cobaltosic oxide
The problem of element is unevenly distributed.
Invention content
The purpose of the invention is to overcome the shortcomings of above-mentioned prior art, a kind of gradient of aluminium element Uniform Doped is provided
Mix the preparation method of aluminium cobaltosic oxide.
The purpose of the present invention is what is be achieved through the following technical solutions：Using certain density cobalt liquor as cobalt source, hydroxide
Sodium solution is precipitating reagent, and ammonia spirit is complexing agent, and hydrogen peroxide solution is oxidant, and aluminium salt ethanol solution is that doping is molten
Liquid will participate in reacting, a step prepares gradient by disperseing liquid feeding mode in doped solution addition reaction kettle during the reaction
Mix aluminium cobaltosic oxide product.Specifically include following steps：
A, the preparation of solution
Using cobalt salt as raw material, it is solution A to prepare the cobalt liquor that cobalt concentration is 1-2mol/L, and the solution A that accurate measurement volume is x is standby
With；Compound concentration be 2-6mol/L sodium hydroxide solution, be added 0.05 ~ 0.1 times of volume, a concentration of 180g/L ammonia spirit
For B solution；The hydrogen peroxide solution that compound concentration is 5-10mol/L is C solution；Compound concentration is the aluminium salt absolute ethyl alcohol of 4-8g/L
Solution is solution D, according to formula：Solution D volume=（X × solution A concentration × prepares product requirement and mixes aluminum amount）/（Solution D concentration
Cobalt percentage composition in × cobaltosic oxide）, the volume y of required solution D is calculated, and accurately measure the anhydrous second that volume is y
Alcohol is spare；
B, synthetic reaction
When synthetic reaction starts, according to the generated time t that preparation process determines, spare nothing is added with the flow of y/t for solution D
It is E solution in water-ethanol, while solution A is added with the flow velocity of x/t and B solution, C solution cocurrent in reaction kettle, and with 2y/t
Flow velocity E solution is added in reaction kettle by disperseing in a manner of liquid feeding, reacted under the stirring of 200-500r/min, E
After solution is added completely into reaction kettle, synthetic reaction terminates；
C, it is filtered, washed and dries
After synthetic reaction, material in reaction kettle is filtered, 80-100 DEG C of deionized water pulping and washing, 100-400 DEG C
Lower drying obtains gradient and mixes aluminium cobaltosic oxide product.
As the further preferred of technical solution of the present invention, in above-mentioned steps a, cobalt salt is cobaltous sulfate, cobalt nitrate, cobalt chloride
One or more of mixture, aluminium salt ethanol solution is the ethanol solution of alchlor or aluminum nitrate.
In synthetic reaction process, controlling reaction temperature is 70-80 DEG C, pH value in reaction 8.0-9.0, and solution A flow velocity is
300L/h, B solution flow velocity are adjusted according to pH value in reaction, and C solution flow velocity is 30-36L/h, reaction time 15-20h.
In step b, the liquid feeding mode of E solution is that E solution charging lines are divided into 6-9 tiny pipelines, Mei Gexi
Charging line liquid outlet is fixed to middle part or the tail portion dispersion liquid feeding of reaction kettle stirrer paddle.
Compared with the prior art, the advantageous effect of technical solution of the present invention is：
1. mix aluminium cobaltosic oxide with Co deposited synthesis, due to Al (OH)3Solubility product constant at normal temperatures is far smaller than
Co(OH)2Solubility product constant, and Al3+It is difficult that complex reaction occurs with ammonium hydroxide, leads to Al in solution3+Settling rate it is much fast
In Co2+, Al elements is caused to be unevenly distributed in cobaltosic oxide.The present invention is used is dissolved in absolute ethyl alcohol as dopant using aluminium salt
The method of solution, after ethanol solution need are miscible with water, aluminium salt could participate in reacting, and slow down Al3+Settling rate, solve by
In Al (OH)3The problem of solubility product constant is too small and reacts violent, and aluminium cannot be co-precipitated with cobalt；And by by aluminium salt absolute ethyl alcohol
Solution charging line is divided into 6-9 small sized pipeline, and each thin charging line liquid outlet is fixed in the middle part of stirring blade or portion
The method for dissipating liquid feeding, makes Al in building-up process3+It can rapidly and uniformly be distributed in reaction kettle and participate in reaction, ensure that preparation
Go out being uniformly distributed for aluminium element in product.
2, the aluminium cobaltosic oxide product of mixing that the method for the present invention is prepared is used to mix aluminum amount for 0.5-1.0%, and aluminium element is in
Gradient uniformity is distributed, and laser particle size is 5-8 μm, Zhen Shi Mi Du≤2.5g/cm3, specific surface area 1.0-3.0m2/ g, in blocky or class
Spherical morphology.
Description of the drawings
Fig. 1 is the testing result figure of the product synthesized using method in the embodiment of the present invention 1；
Fig. 2 is the testing result figure of the product synthesized using method in the embodiment of the present invention 2；
Fig. 3 is the testing result figure of the product synthesized using method in the embodiment of the present invention 3.
Specific implementation mode
The preparation method work for mixing the present invention aluminium cobaltosic oxide by specific embodiment below in conjunction with the accompanying drawings is further detailed
It describes in detail bright.
Embodiment 1
The cobalt chloride solution that compound concentration is 1mol/L is solution A, and it is spare accurately to measure 4500L；Compound concentration is 2mol/L
Sodium hydroxide solution, be added 0.05 times of volume, a concentration of 180g/L ammonia spirit be B solution；Compound concentration is 5mol/L
Hydrogen peroxide solution be C solution；The aluminium salt ethanol solution that compound concentration is 4g/L is solution D, according to formula：Solution D body
Product=（X × solution A concentration × prepares product requirement and mixes aluminum amount）/（Cobalt percentage composition in solution D concentration × cobaltosic oxide）, meter
It calculates and show that the volume of required solution D is 450L, the accurate absolute ethyl alcohol for measuring 450L is spare；
When synthetic reaction starts, determines that generated time is 15h, solution D is added with the flow of 30L/h in spare absolute ethyl alcohol
For E solution, while solution A being added in reaction kettle with the flow velocity of 300L/h and B solution, C solution cocurrent, while E solution being added
Liquid pipe road is divided into the tiny pipelines of 6-9, each thin charging line liquid outlet be fixed to reaction kettle stirrer paddle middle part or
Tail portion, and disperse to be added in reaction kettle by E solution with the flow velocity of 60L/h, it is reacted under the stirring of 500r/min, E
After solution is added completely into reaction kettle, synthetic reaction terminates；In synthetic reaction process, controlling reaction temperature is 70 DEG C, reacts pH
Value is 8.0, and solution A flow velocity is 300L/h, and B solution flow velocity is adjusted according to pH value in reaction, and C solution flow velocity is 30L/h.
After synthetic reaction, material in reaction kettle is filtered, 80 DEG C of deionized water pulping and washings, is done at 200 DEG C
It is dry, obtain gradient and mix aluminium cobaltosic oxide product.Its product index is as shown in Figure 1.It mixes aluminium cobaltosic oxide product and mixes aluminum amount and be
0.5%, and aluminium element is uniformly distributed in gradient, laser particle size is 5 μm, Zhen Shi Mi Du≤2.5g/cm3, specific surface area 1.0-
3.0m2/ g, in blocky or spherical pattern.
Embodiment 2
The cobalt sulfate solution that compound concentration is 1.5mol/L is solution A, and it is spare accurately to measure 5400L；Compound concentration is 4mol/
0.08 times of volume is added in the sodium hydroxide solution of L, the ammonia spirit of a concentration of 180g/L is B solution；Compound concentration is 8mol/L
Hydrogen peroxide solution be C solution；The aluminium salt ethanol solution that compound concentration is 6g/L is solution D, according to formula：Solution D body
Product=（X × solution A concentration × prepares product requirement and mixes aluminum amount）/（Cobalt percentage composition in solution D concentration × cobaltosic oxide）, meter
It calculates and show that the volume of required solution D is 540L, the accurate absolute ethyl alcohol for measuring 540L is spare；
When synthetic reaction starts, determines that generated time is 18h, solution D is added with the flow of 30L/h in spare absolute ethyl alcohol
For E solution, while solution A being added in reaction kettle with the flow velocity of 300L/h and B solution, C solution cocurrent, while E solution being added
Liquid pipe road is divided into the tiny pipelines of 6-9, each thin charging line liquid outlet be fixed to reaction kettle stirrer paddle middle part or
Tail portion, and disperse to be added in reaction kettle by E solution with the flow velocity of 60L/h, it is reacted under the stirring of 350r/min, E
After solution is added completely into reaction kettle, synthetic reaction terminates；In synthetic reaction process, controlling reaction temperature is 75 DEG C, reacts pH
Value is 8.5, and solution A flow velocity is 300L/h, and B solution flow velocity is adjusted according to pH value in reaction, and C solution flow velocity is 31L/h.
After synthetic reaction, material in reaction kettle is filtered, 90 DEG C of deionized water pulping and washings, is done at 300 DEG C
It is dry, obtain gradient and mix aluminium cobaltosic oxide product.Its product index is as shown in Figure 2.It mixes aluminium cobaltosic oxide product and mixes aluminum amount and be
0.75%, and aluminium element is uniformly distributed in gradient, laser particle size is 7 μm, Zhen Shi Mi Du≤2.5g/cm3, specific surface area 1.0-
3.0m2/ g, in blocky or spherical pattern.
Embodiment 3
The cobalt nitrate solution that compound concentration is 2mol/L is solution A, and it is spare accurately to measure 6000L；Compound concentration is 6mol/L
Sodium hydroxide solution, be added 0.1 times of volume, a concentration of 180g/L ammonia spirit be B solution；Compound concentration is 10mol/L
Hydrogen peroxide solution be C solution；The aluminium salt ethanol solution that compound concentration is 8g/L is solution D, according to formula：Solution D body
Product=（X × solution A concentration × prepares product requirement and mixes aluminum amount）/（Cobalt percentage composition in solution D concentration × cobaltosic oxide）, meter
It calculates and show that the volume of required solution D is 600L, the accurate absolute ethyl alcohol for measuring 600L is spare；
When synthetic reaction starts, determines that generated time is 20h, solution D is added with the flow of 30L/h in spare absolute ethyl alcohol
For E solution, while solution A being added in reaction kettle with the flow velocity of 300L/h and B solution, C solution cocurrent, while E solution being added
Liquid pipe road is divided into the tiny pipelines of 6-9, each thin charging line liquid outlet be fixed to reaction kettle stirrer paddle middle part or
Tail portion, and disperse to be added in reaction kettle by E solution with the flow velocity of 60L/h, it is reacted under the stirring of 200r/min, E
After solution is added completely into reaction kettle, synthetic reaction terminates；In synthetic reaction process, controlling reaction temperature is 80 DEG C, reacts pH
Value is 9.0, and solution A flow velocity is 300L/h, and B solution flow velocity is adjusted according to pH value in reaction, and C solution flow velocity is 36L/h.
After synthetic reaction, material in reaction kettle is filtered, 100 DEG C of deionized water pulping and washings, is done at 400 DEG C
It is dry, obtain gradient and mix aluminium cobaltosic oxide product.Its product index is as shown in Figure 3.It mixes aluminium cobaltosic oxide product and mixes aluminum amount and be
1.0%, and aluminium element is uniformly distributed in gradient, laser particle size is 8 μm, Zhen Shi Mi Du≤2.5g/cm3, specific surface area 1.0-
3.0m2/ g, in blocky or spherical pattern.
Claims (5)
1. a kind of gradient mixes the preparation method of aluminium cobaltosic oxide, it is characterized in that, this approach includes the following steps：
A, the preparation of solution
Using cobalt salt as raw material, it is solution A to prepare the cobalt liquor that cobalt concentration is 1-2mol/L, and the solution A that accurate measurement volume is x is standby
With；Compound concentration be 2-6mol/L sodium hydroxide solution, be added 0.05 ~ 0.1 times of volume, a concentration of 180g/L ammonia spirit
For B solution；The hydrogen peroxide solution that compound concentration is 5-10mol/L is C solution；Compound concentration is the aluminium salt absolute ethyl alcohol of 4-8g/L
Solution is solution D, according to formula：Solution D volume=（X × solution A concentration × prepares product requirement and mixes aluminum amount）/（Solution D concentration
Cobalt percentage composition in × cobaltosic oxide）, the volume y of required solution D is calculated, and accurately measure the anhydrous second that volume is y
Alcohol is spare；
B, synthetic reaction
When synthetic reaction starts, according to the generated time t that preparation process determines, spare nothing is added with the flow of y/t for solution D
It is E solution in water-ethanol, while solution A is added with the flow velocity of x/t and B solution, C solution cocurrent in reaction kettle, and with 2y/t
Flow velocity E solution is added in reaction kettle by disperseing in a manner of liquid feeding, reacted under the stirring of 200-500r/min, E
After solution is added completely into reaction kettle, synthetic reaction terminates；
C, it is filtered, washed and dries
After synthetic reaction, material in reaction kettle is filtered, 80-100 DEG C of deionized water pulping and washing, 100-400 DEG C
Lower drying obtains gradient and mixes aluminium cobaltosic oxide product.
2. a kind of gradient according to claim 1 mixes the preparation method of aluminium cobaltosic oxide, it is characterised in that：In step a,
The cobalt salt is the mixture of one or more of cobaltous sulfate, cobalt nitrate, cobalt chloride, and aluminium salt ethanol solution is tri-chlorination
The ethanol solution of aluminium or aluminum nitrate.
3. a kind of gradient according to claim 1 mixes the preparation method of aluminium cobaltosic oxide, it is characterised in that：The synthesis
In reaction process, controlling reaction temperature is 70-80 DEG C, pH value in reaction 8.0-9.0, and solution A flow velocity is 300L/h, B solution stream
Speed is adjusted according to pH value in reaction, and C solution flow velocity is 30-36L/h, reaction time 15-20h.
4. a kind of gradient according to claim 2 mixes the preparation method of aluminium cobaltosic oxide, it is characterised in that：The synthesis
In reaction process, controlling reaction temperature is 70-80 DEG C, pH value in reaction 8.0-9.0, and solution A flow velocity is 300L/h, B solution stream
Speed is adjusted according to pH value in reaction, and C solution flow velocity is 30-36L/h, reaction time 15-20h.
5. mixing the preparation method of aluminium cobaltosic oxide according to a kind of gradient of claim 1-4 any one of them, it is characterised in that：
In step b, the liquid feeding mode of the E solution is that E solution charging lines are divided into 6-9 tiny pipelines, each thin liquid-feeding tube
Road liquid outlet is fixed to middle part or the tail portion dispersion liquid feeding of reaction kettle stirrer paddle.
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Cited By (7)
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| CN109326781A (en) * | 2018-09-29 | 2019-02-12 | 湖南长远锂科有限公司 | A kind of preparation method of high voltage lithium cobalt oxide anode |
| CN110078133A (en) * | 2019-04-29 | 2019-08-02 | 湖南雅城新材料有限公司 | Spherical cobaltosic oxide of a kind of aluminium doping and the preparation method and application thereof |
| CN111994964A (en) * | 2020-07-28 | 2020-11-27 | 格林美股份有限公司 | Aluminum concentration gradient doped and titanium coated cobaltosic oxide material and preparation method thereof |
| CN112125350A (en) * | 2019-06-24 | 2020-12-25 | 荆门市格林美新材料有限公司 | Aluminum-doped cobaltosic oxide with multilayer core-shell structure and preparation method thereof |
| CN112408499A (en) * | 2020-11-09 | 2021-02-26 | 格林美（江苏）钴业股份有限公司 | Method for synthesizing cobaltosic oxide by adopting high-pressure reaction |
| CN114736535A (en) * | 2022-04-22 | 2022-07-12 | 宜宾天原海丰和泰有限公司 | Method for coating titanium dioxide by parallel flow aluminum |
| CN116081704A (en) * | 2023-03-15 | 2023-05-09 | 格林美（江苏）钴业股份有限公司 | Modified cobaltosic oxide and preparation method and application thereof |
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| CN110078133B (en) * | 2019-04-29 | 2021-10-12 | 湖南雅城新材料有限公司 | Aluminum-doped spheroidal cobaltosic oxide and preparation method and application thereof |
| CN112125350A (en) * | 2019-06-24 | 2020-12-25 | 荆门市格林美新材料有限公司 | Aluminum-doped cobaltosic oxide with multilayer core-shell structure and preparation method thereof |
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| CN112408499A (en) * | 2020-11-09 | 2021-02-26 | 格林美（江苏）钴业股份有限公司 | Method for synthesizing cobaltosic oxide by adopting high-pressure reaction |
| CN114736535A (en) * | 2022-04-22 | 2022-07-12 | 宜宾天原海丰和泰有限公司 | Method for coating titanium dioxide by parallel flow aluminum |
| CN116081704A (en) * | 2023-03-15 | 2023-05-09 | 格林美（江苏）钴业股份有限公司 | Modified cobaltosic oxide and preparation method and application thereof |
| CN116081704B (en) * | 2023-03-15 | 2024-04-16 | 格林美（江苏）钴业股份有限公司 | Modified cobaltosic oxide and preparation method and application thereof |
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