CN108682848A - A kind of preparation method for mixing niobium tungsten tantalum cobalt acid lithium - Google Patents
A kind of preparation method for mixing niobium tungsten tantalum cobalt acid lithium Download PDFInfo
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- CN108682848A CN108682848A CN201810490922.3A CN201810490922A CN108682848A CN 108682848 A CN108682848 A CN 108682848A CN 201810490922 A CN201810490922 A CN 201810490922A CN 108682848 A CN108682848 A CN 108682848A
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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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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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Abstract
The invention discloses a kind of preparation methods for mixing niobium tungsten tantalum cobalt acid lithium, belong to technical field of lithium ion.For this method using certain density cobalt and lithium mixed solution as cobalt, lithium source, sodium carbonate liquor is precipitating reagent, and ammonia spirit is complexing agent, and hydrazine hydrate solution is reducing agent, and aluminium salt ethanol solution is dopant, goes out cobalt carbonate and carbonic acid lithium mixture using Moist chemical synthesis.During the reaction, participation reaction in reaction kettle is added in doped solution by disperseing liquid feeding mode；After synthesis under the conditions of certain pH value, cobalt carbonate is oxidized to hydroxy cobalt oxide using certain density hydrogen peroxide solution, then mixture is washed, is dry, is calcined under certain condition, obtains mixing aluminium cobalt acid lithium product, production efficiency is high；And the niobium tungsten tantalum cobalt acid lithium product of mixing for using that the method for the present invention prepares mixes niobium, tungsten, tantalum amount for 0.2 0.4%, and niobium, tungsten, tantalum element are uniformly distributed, laser particle size is 5 15 μm, Zhen Shi Mi Du≤2.0g/cm3, 0.2 0.6m of specific surface area2/ g, in blocky or spherical pattern.
Description
Technical field
It is specifically a kind of to mix niobium tungsten for anode material for lithium-ion batteries the invention belongs to technical field of lithium ion
The preparation method of tantalum cobalt acid lithium.
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.
Chinese invention patent（200710065340.2）Disclose a kind of " super large grain size and high-density lithium cobalt oxide and its preparation
Method ", specifically will be by cobalt compound, lithium compound, or is mixed simultaneously with a small amount of doping element compound, high temperature sintering 3-
30h forms block sintered product, obtains cobalt acid lithium powder body material using crushing and classification, this method production technology need to be through length
The batch mixing of time and sintering, low production efficiency, high energy consumption.Chinese invention patent（201210011485.5）Disclose that " one kind is mixed
The preparation process of the spherical lithium cobalt of miscellaneous Ti, Mg, Al ", specifically by cobalt salt mixed solution and ammonium bicarbonate soln precipitation reaction,
Spherical cobaltous carbonate obtains cobaltosic oxide after primary roasting, cobaltosic oxide with lithium source through after baking obtain doping Ti, Mg,
The problem of Al spherical lithium cobalts, that there is also roasting times is long for the production method, high energy consumption.
In view of the above technical problems, the Chinese invention patent of 107863526 A of Publication No. CN discloses a kind of " doping
The preparation method of cobalt acid lithium ", this method goes out the sediment of doped chemical by Moist chemical synthesis, then cobalt hydroxide is oxidized to hydroxyl
Cobalt oxide obtains doping cobalt acid lithium product finally by calcining.But this method mixes high-valence state, thick atom amount member being used to prepare
When plain niobium, tungsten, tantalum cobalt acid lithium, there are problems that niobium, tungsten, tantalum chloride as wet method dopant be easy hydrolysis, cause niobium, tungsten,
Tantalum element and lithium, cobalt precipitation are uneven.In addition, the compound of cobalt is very easy to oxidation, the cobalt compound after oxidation can interfere conjunction
At the fast-growth of product, therefore, there is also the relatively low problems of production efficiency for this method.
Invention content
The purpose of the invention is to overcome the shortcomings of above-mentioned prior art, provide that a kind of production efficiency is high, product quality
The good preparation method for mixing niobium, tungsten, tantalum cobalt acid lithium.
The purpose of the present invention is what is be achieved through the following technical solutions：Using certain density cobalt and lithium mixed solution as cobalt,
Lithium source, sodium carbonate liquor are precipitating reagent, and ammonia spirit is complexing agent, hydrazine hydrate solution is reducing agent, niobium, tungsten, tantalum chloride
Ethanol solution is dopant, and Moist chemical synthesis goes out cobalt carbonate and carbonic acid lithium mixture under certain condition.During the reaction,
Participation reaction in reaction kettle is added in doped solution by disperseing liquid feeding mode；After synthesis under the conditions of certain pH value, profit
Cobalt carbonate is oxidized to hydroxy cobalt oxide with certain density hydrogen peroxide solution, then by mixture washing, drying, in certain item
It is calcined under part, obtains mixing aluminium cobalt acid lithium product.Specifically include following steps：
A, the preparation of solution
Using cobalt salt, lithium salts as raw material, it is 1 to keep lithium, cobalt molar ratio:1.1-1.4 is configured to cobalt, lithium concentration is 1-2mol/L
Lithium cobalt mixed solution be solution A；The sodium carbonate liquor that compound concentration is 1-2mol/L is B solution, and sodium carbonate is dense in B solution
Degree is identical as the concentration of cobalt in solution A；Compound concentration is the ammonia spirit of 5-10mol/L, and 5- is added in every liter of ammonia spirit
The hydrazine hydrate solution that 20mL volume fractions are 30% is C solution；Compound concentration is that the niobium tungsten tantalum chloride absolute ethyl alcohol of 2-4g/L is molten
Liquid is solution D；The hydrogen peroxide solution that compound concentration is 5-10mol/L is E solution；Compound concentration is the sodium hydroxide of 2-6mol/L
Solution is F solution；
B, synthetic reaction
So that solution A, B solution and C solution cocurrent is entered reaction kettle, while solution D is added, in the stirring of 200-500r/min
Under reacted, obtain the mixture of cobalt carbonate and lithium carbonate；
C, oxidation reaction
E solution and F solution are added in the mixture of cobalt carbonate and lithium carbonate, is carried out under the stirring of 200-500r/min
Reaction, makes cobalt carbonate be changed into hydroxy cobalt oxide；Wherein, reaction temperature is 70-80 DEG C, reaction time 1-2h, E solution addition
It is 0.5-0.6 times of solution A addition, is 10-11 by adjusting solution D flow control solution ph；
D, it is filtered, washed and dries
After oxidation reaction, material in reaction kettle is filtered, 80-100 DEG C of deionized water pulping and washing, 100-400 DEG C
Lower drying obtains mixing niobium tungsten tantalum cobalt acid lithium presoma；
E, it calcines
The calcining of niobium tungsten tantalum cobalt acid lithium presoma will be mixed, obtains mixing niobium tungsten tantalum cobalt acid lithium product.
As the further preferred of technical solution of the present invention, above-mentioned cobalt salt is one kind in cobaltous sulfate, cobalt nitrate, cobalt chloride
Or several mixtures, lithium salts are the mixture of one or both of lithium nitrate, lithium chloride, the anhydrous second of niobium tungsten tantalum chloride
Alcoholic solution is the ethanol solution of columbium pentachloride, tungsten hexachloride or tantalic chloride.
In synthetic reaction process, a concentration of 5-10g/L of ammonia spirit is controlled, reaction temperature is 70-80 DEG C, solution A flow velocity
For 200L/h, B solution flow velocity is 320-340L/h, and C solution flow velocity is adjusted according to ammonia spirit concentration, and solution D flow velocity is 20L/
H, reaction time 80-100h.
The liquid feeding mode of solution D is solution D charging line to be divided into 6-9 tiny pipelines, each thin liquid-feeding tube is said
Liquid mouth is fixed to middle part or the tail portion dispersion liquid feeding of reaction kettle stirrer paddle.
Calcination process is in confined conditions, 10-20h to be calcined with 800-1000 DEG C of calcination temperature.
Compared with the prior art, the advantageous effect of technical solution of the present invention is：
1. the compound of cobalt is very easy to oxidation, the cobalt compound after oxidation can prevent the quick of synthetic product
Growth, causes the laser particle size of final products to be not easy to grow up, the present invention mixes the preparation method of niobium tungsten tantalum cobalt acid lithium, passes through
It is reducing agent that the hydrazine hydrate that volume fraction is 30%, which is added, cobalt compound can be prevented to aoxidize, and then promotes the quick length of product
Greatly, production efficiency is improved.
2. when mixing high-valence state, thick atom secondary element niobium, tungsten, tantalum cobalt acid lithium using wet method preparation, there are niobium, tungsten, tantalum chlorine
The problem of compound is easy hydrolysis as wet method dopant keeps niobium, tungsten, tantalum and lithium, cobalt precipitation uneven, causes niobium, tungsten, tantalum in cobalt
It is adulterated in sour lithium uneven.The present invention is used is dissolved in side of the absolute ethyl alcohol as dopant solution using the chloride of niobium, tungsten, tantalum
Method solves the problems, such as that niobium, tungsten, tantalum chloride are easy hydrolysis well；And by will be by the anhydrous second of niobium, tungsten, tantalum chloride
Alcoholic 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 tail portion
The method for disperseing liquid feeding enables niobium in building-up process, tungsten, tantalum to be rapidly and uniformly distributed in reaction kettle and participates in reaction, ensures
Prepare being uniformly distributed for doped chemical in product.
3, the niobium tungsten tantalum cobalt acid lithium product of mixing that the method for the present invention is prepared is used to mix niobium, tungsten, tantalum amount for 0.2-0.4%, and
Niobium, tungsten, tantalum element are uniformly distributed, and laser particle size is 5-15 μm, Zhen Shi Mi Du≤2.0g/cm3, specific surface area 0.2-0.6m2/ g,
In blocky or spherical pattern.
Description of the drawings
Fig. 1 is the testing result of the product synthesized using method in the embodiment of the present invention 1；
Fig. 2 is the testing result of the product synthesized using method in the embodiment of the present invention 2；
Fig. 3 is the testing result 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 niobium tungsten tantalum cobalt acid lithium by specific embodiment below in conjunction with the accompanying drawings is further detailed
It describes in detail bright.
Embodiment 1
Preparation cobalt chloride concentration is 1mol/L, the mixed solution of a concentration of 1.1mol/L of lithium chloride is solution A；Compound concentration is
The sodium carbonate liquor of 1mol/L is B solution；Compound concentration is the ammonia spirit of 5mol/L, and 5mL is added in every liter of ammonia spirit
The hydrazine hydrate solution that volume fraction is 30% is C solution；The columbium pentachloride ethanol solution for preparing a concentration of 2g/L of niobium is solution D；Match
The hydrogen peroxide solution for making a concentration of 5mol/L is E solution；The sodium hydroxide solution that compound concentration is 2mol/L is F solution.
When synthetic reaction starts, solution A, B solution and C solution cocurrent is made to enter reaction kettle, while by solution D charging line
It is divided into 6-9 tiny pipelines, each thin charging line liquid outlet is fixed to middle part or the portion of reaction kettle stirrer paddle
It dissipates and solution D is added, reacted under the stirring of 200r/min, a concentration of 5g/L of ammonia spirit is controlled in reaction process,
70 DEG C of reaction temperature, solution A flow velocity 200L/h, B solution flow velocity be 320L/h, C solution flow velocity 40L/h, solution D flow velocity 20L/h,
Reaction time 80h obtains the mixture of cobalt carbonate and lithium carbonate.
After synthetic reaction, E solution and F solution, control reaction temperature are added in the mixture of cobalt carbonate and lithium carbonate
Degree is 70 DEG C, and E solution additions are 0.5 times of solution A addition, is 10 by adjusting solution D flow control solution ph,
1h is reacted under the stirring of 500r/min, cobalt carbonate is made to be oxidized to hydroxy cobalt oxide.
After above-mentioned oxidation reaction, material in reaction kettle is filtered, 80 DEG C of deionized water pulping and washings, 100 DEG C
Lower drying obtains mixing niobium cobalt acid lithium presoma.
Niobium cobalt acid lithium presoma will be mixed and calcine 20h under confined conditions in be not passed through oxidizing gas 800 DEG C, obtain mixing niobium
Cobalt acid lithium product, product index are as shown in Figure 1.The cobalt acid lithium product mixed niobium amount and be 0.2% prepared, laser particle size are 8 μ
M, Zhen Shi Mi Du≤2.0g/cm3, product pattern is in bulk.
Embodiment 2
Preparation cobalt sulfate concentration is 1.5mol/L, the mixed solution of a concentration of 1.8mol/L of lithium nitrate is solution A；Compound concentration is
The sodium carbonate liquor of 1.5mol/L is B solution；Compound concentration is the ammonia spirit of 8mol/L, and is added in every liter of ammonia spirit
The hydrazine hydrate solution that 15mL volume fractions are 30% is C solution；The tungsten hexachloride ethanol solution for preparing a concentration of 3g/L of tungsten is that D is molten
Liquid；The hydrogen peroxide solution that compound concentration is 8mol/L is E solution；The sodium hydroxide solution that compound concentration is 4mol/L is F solution.
When synthetic reaction starts, solution A, B solution and C solution cocurrent is made to enter reaction kettle, while by solution D charging line
It is divided into 8 tiny pipelines, each thin charging line liquid outlet is fixed to middle part or the tail portion dispersion of reaction kettle stirrer paddle
Solution D is added, is reacted under the stirring of 350r/min, a concentration of 8g/L of ammonia spirit is controlled in reaction process, instead
Answer 75 DEG C of temperature, solution A flow velocity 200L/h, B solution flow velocity is 330L/h, C solution flow velocity 50L/h, solution D flow velocity 20L/h, instead
90h between seasonable, obtains the mixture of cobalt carbonate and lithium carbonate.
After synthetic reaction, E solution and F solution, control reaction temperature are added in the mixture of cobalt carbonate and lithium carbonate
Degree is 75 DEG C, and E solution additions are 0.55 times of solution A addition, is by adjusting solution D flow control solution ph
10.5,1.5h is reacted under the stirring of 350r/min, cobalt carbonate is made to be oxidized to hydroxy cobalt oxide.
After above-mentioned oxidation reaction, material in reaction kettle is filtered, 90 DEG C of deionized water pulping and washings, 300 DEG C
Lower drying obtains mixing tungsten cobalt acid lithium presoma.
Tungsten cobalt acid lithium presoma will be mixed and calcine 15h under confined conditions in be not passed through oxidizing gas 900 DEG C, obtain mixing tungsten
Cobalt acid lithium product, product index are as shown in Figure 2.The cobalt acid lithium product mixed tungsten amount and be 0.3% prepared, laser particle size are 10 μ
M, Zhen Shi Mi Du≤2.0g/cm3, product pattern is in bulk.
Embodiment 3
Prepare a concentration of 2mol/L of cobalt nitrate, the mixed solution of a concentration of 2mol/L of lithium chloride is solution A；Compound concentration is
The sodium carbonate liquor of 2mol/L is B solution；Compound concentration is the ammonia spirit of 10mol/L, and is added in every liter of ammonia spirit
The hydrazine hydrate solution that 20mL volume fractions are 30% is C solution；The tantalic chloride ethanol solution for preparing a concentration of 4g/L of tantalum is that D is molten
Liquid；The hydrogen peroxide solution that compound concentration is 10mol/L is E solution；The sodium hydroxide solution that compound concentration is 6mol/L is F molten
Liquid.
When synthetic reaction starts, solution A, B solution and C solution cocurrent is made to enter reaction kettle, while by solution D charging line
It is divided into 9 tiny pipelines, each thin charging line liquid outlet is fixed to middle part or the tail portion dispersion of reaction kettle stirrer paddle
Solution D is added, is reacted under the stirring of 500r/min, a concentration of 10g/L of ammonia spirit is controlled in reaction process, instead
Answer 80 DEG C of temperature, solution A flow velocity 200L/h, B solution flow velocity is 340L/h, C solution flow velocity 60L/h, solution D flow velocity 20L/h, instead
100h between seasonable, obtains the mixture of cobalt carbonate and lithium carbonate.
After synthetic reaction, E solution and F solution, control reaction temperature are added in the mixture of cobalt carbonate and lithium carbonate
Degree is 80 DEG C, and E solution additions are 0.6 times of solution A addition, is 11 by adjusting solution D flow control solution ph,
2h is reacted under the stirring of 200r/min, cobalt carbonate is made to be oxidized to hydroxy cobalt oxide.
After above-mentioned oxidation reaction, material in reaction kettle is filtered, 100 DEG C of deionized water pulping and washings, 400 DEG C
Lower drying obtains mixing tantalum cobalt acid lithium presoma.
Tantalum cobalt acid lithium presoma will be mixed and calcine 20h under confined conditions in be not passed through oxidizing gas 1000 DEG C, mixed
Tantalum cobalt acid lithium product, product index are as shown in Figure 3.The cobalt acid lithium product mixed tantalum amount and be 0.4% prepared, laser particle size are
10 μm, Zhen Shi Mi Du≤2.0g/cm3, product pattern is in bulk.
Claims (6)
1. a kind of preparation method for mixing niobium tungsten tantalum cobalt acid lithium, is characterized in that, this approach includes the following steps：
A, the preparation of solution
Using cobalt salt, lithium salts as raw material, it is 1 to keep lithium, cobalt molar ratio:1.1-1.4 is configured to cobalt, lithium concentration is 1-2mol/L
Lithium cobalt mixed solution be solution A；The sodium carbonate liquor that compound concentration is 1-2mol/L is B solution, and sodium carbonate is dense in B solution
Degree is identical as the concentration of cobalt in solution A；Compound concentration is the ammonia spirit of 5-10mol/L, and 5- is added in every liter of ammonia spirit
The hydrazine hydrate solution that 20mL volume fractions are 30% is C solution；Compound concentration is that the absolute ethyl alcohol of 2-4g/L niobium tungsten tantalum chlorides is molten
Liquid is solution D；The hydrogen peroxide solution that compound concentration is 5-10mol/L is E solution；Compound concentration is the sodium hydroxide of 2-6mol/L
Solution is F solution；
B, synthetic reaction
So that solution A, B solution and C solution cocurrent is entered reaction kettle, while solution D is added, in the stirring of 200-500r/min
Under reacted, obtain the mixture of cobalt carbonate and lithium carbonate；
C, oxidation reaction
E solution and F solution are added in the mixture of cobalt carbonate and lithium carbonate, is carried out under the stirring of 200-500r/min
Reaction, makes cobalt carbonate be changed into hydroxy cobalt oxide；Wherein, reaction temperature is 70-80 DEG C, reaction time 1-2h, E solution addition
It is 0.5-0.6 times of solution A addition, is 10-11 by adjusting solution D flow control solution ph；
D, it is filtered, washed and dries
After oxidation reaction, material in reaction kettle is filtered, 80-100 DEG C of deionized water pulping and washing, 100-400 DEG C
Lower drying obtains mixing niobium tungsten tantalum cobalt acid lithium presoma；
E, it calcines
The calcining of niobium tungsten tantalum cobalt acid lithium presoma will be mixed, obtains mixing niobium tungsten tantalum cobalt acid lithium product.
2. a kind of preparation method for mixing niobium tungsten tantalum cobalt acid lithium according to claim 1, it is characterised in that：It is described in step a
Cobalt salt is the mixture of one or more of cobaltous sulfate, cobalt nitrate, cobalt chloride, and lithium salts is one kind in lithium nitrate, lithium chloride
Or two kinds of mixture, the ethanol solution of niobium tungsten tantalum chloride is the anhydrous of columbium pentachloride, tungsten hexachloride or tantalic chloride
Ethanol solution.
3. a kind of preparation method for mixing niobium tungsten tantalum cobalt acid lithium according to claim 1, it is characterised in that：The synthetic reaction
In the process, a concentration of 5-10g/L of ammonia spirit is controlled, reaction temperature is 70-80 DEG C, and solution A flow velocity is 200L/h, B solution stream
Speed is 320-340L/h, and C solution flow velocity is adjusted according to ammonia spirit concentration, and solution D flow velocity is 20L/h, reaction time 80-
100h。
4. according to a kind of preparation method for mixing niobium tungsten tantalum cobalt acid lithium of claim 1-3 any one of them, it is characterised in that：Step
In b, the liquid feeding mode of the solution D is solution D charging line to be divided into 6-9 tiny pipelines, each thin liquid-feeding tube is said
Liquid mouth is fixed to middle part or the tail portion dispersion liquid feeding of reaction kettle stirrer paddle.
5. according to a kind of preparation method for mixing niobium tungsten tantalum cobalt acid lithium of claim 1-3 any one of them, it is characterised in that：It is described
Calcination process is in confined conditions, 10-20h to be calcined with 800-1000 DEG C of calcination temperature.
6. a kind of preparation method for mixing niobium tungsten tantalum cobalt acid lithium according to claim 4, it is characterised in that：The calcination process
In confined conditions, 10-20h to be calcined with 800-1000 DEG C of calcination temperature.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110247049A (en) * | 2019-04-30 | 2019-09-17 | 上海德朗能动力电池有限公司 | A kind of lithium battery metal oxide negative electrode material and its preparation method and application |
| WO2021060095A1 (en) * | 2019-09-26 | 2021-04-01 | Ｄｏｗａエレクトロニクス株式会社 | Solution containing lithium, niobium complex and hydrazine, method for producing same, and method for producing active material for lithium secondary batteries |
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| Publication number | Priority date | Publication date | Assignee | Title |
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Application publication date: 20181019 |