CN107863525A - A kind of preparation method of grade doping cobalt acid lithium - Google Patents
A kind of preparation method of grade doping cobalt acid lithium Download PDFInfo
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- CN107863525A CN107863525A CN201710996093.1A CN201710996093A CN107863525A CN 107863525 A CN107863525 A CN 107863525A CN 201710996093 A CN201710996093 A CN 201710996093A CN 107863525 A CN107863525 A CN 107863525A
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- 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 invention discloses a kind of preparation method of grade doping cobalt acid lithium, using the cobalt salt of certain volume, lithium salts as raw material, certain density ammonium bicarbonate soln, doped chemical soluble salt solution, sodium hydroxide solution and hydrogen peroxide solution are prepared again, pass through synthetic reaction and oxidation reaction, again by filtering, washing and drying and calcination, grade doping cobalt acid lithium product is obtained；The present invention with synthesising reacting time by extending, add the amount gradient increase of dopant in reactor, make doped chemical distribution gradient in the product, Moist chemical synthesis goes out the distribution of doped chemical gradient and the mixed uniformly sediment of lithium, cobalt, cobalt hydroxide is oxidized to hydroxy cobalt oxide again, finally by calcining, the doping cobalt acid lithium product of doped chemical gradient distribution is obtained.Present invention, avoiding being needed the long-time such as doped chemical oxide, cobalt/cobalt oxide, lithium carbonate batch mixing in Traditional dopant cobalt acid lithium preparation process and still can not avoid doped chemical Local enrichment completely, easily it is separated, the shortcomings that weakening material property.
Description
Technical field
The invention belongs to technical field of lithium ion, and in particular to a kind of modified cobalt for anode material for lithium-ion batteries
The preparation method of sour lithium.
Background technology
From Sony corporation of Japan in 1992 successfully by after lithium ion battery commercialization, lithium ion battery relies on its operating voltage
High, energy density height, have extended cycle life.Self discharge is low, it is pollution-free, unique advantage such as have a safety feature, be widely used as moving
The power supply of mobile phone, portable computer, video camera, camera etc. and in space flight, navigation, artificial satellite, small medical
And progressively develop into the energy battery of mainstream applications in military communication apparatus.
Cobalt acid lithium is the main positive electrode of current commercial Li-ion battery.But cobalt acid lithium actual specific capacity only has
140mAh./g or so, it is only its theoretical capacity（274mAh./g）50% or so；And the anti-over-charging poor-performing of cobalt acid lithium,
Reduced rapidly compared with specific capacity under high charge voltage.The problem of to overcome cobalt acid lithium to exist, people's research take a variety of modifications and arranged
Apply and method.Research has shown that, in terms of positive electrode performance, particularly cycle performance is improved, doping be most efficient method it
One, doping can not only improve the stability of lattice, and the cycle performance of material can be greatly improved.
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, uniformity
Difference, it is impossible to meet requirement of the battery industry to doping cobalt acid lithium.
Chinese invention patent CN200710065340.2, disclose " super large particle diameter and high-density lithium cobalt oxide and its preparation side
Method ", specifically will be by cobalt compound, lithium compound, or is mixed simultaneously with a small amount of doping element compound, through 950 ~ 1100 DEG C of height
Temperature sintering 3 ~ 30 hours, block sintered product is formed, then cobalt acid lithium powder body material (molecular formula is obtained after crushing and classification
It is LiaCo1-bMbO2).This patent need to pass through prolonged batch mixing, and preparation technology and the application patent are significantly different, and it is made
Gradient distribution can not be presented in doped chemical in standby doping cobalt acid lithium.Chinese invention patent CN201210011485.5, is disclosed
" a kind of preparation technology for the spherical lithium cobalt for adulterating Ti, Mg, Al ", specifically sinks cobalt salt mixed solution and ammonium bicarbonate soln
Form sediment and react, spherical cobaltous carbonate obtains cobaltosic oxide after being once calcined, and cobaltosic oxide is mixed with lithium source through after baking
Miscellaneous Ti, Mg, Al spherical lithium cobalt.Gradient distribution can not be presented in Doped ions in the doping cobalt acid lithium prepared in such a patent.
The content of the invention
To overcome above-mentioned deficiency, it is an object of the invention to provide a kind of preparation method of grade doping cobalt acid lithium.
In order to meet above-mentioned purpose, the technical solution adopted by the present invention is：
A kind of preparation method of grade doping cobalt acid lithium, is concretely comprised the following steps：
A, solution A is prepared
Using cobalt salt, lithium salts as raw material, the lithium cobalt mixed solution A that cobalt concentration is 1~2mol/L is configured to, and lithium cobalt mol ratio is 1：
1~1：4, precise volume is that x A is standby；
B, B solution is prepared
Compound concentration is 1~2mol/L ammonium bicarbonate soln B, and ammonium hydrogencarbonate concentration is identical with lithium molar concentration in A in B；
C, C solution is prepared
Compound concentration is 5.9~19.6g/L doped chemical soluble salt solution C, is produced according to the concentration of cobalt, x amount, preparation in A
Doped chemical concentration in the doped chemical doping and C of product requirement, according to formula：C solution volume=（X*A solution cobalt solubility *
Doping）/（Cobalt content in C solution doped chemical concentration * cobalt acid lithiums）, be calculated needed for C volume this volume be set to y.
D, compound concentration is 2~8mol/L sodium hydroxide solution D；
E, configuration concentration is 1~5mol/L hydrogen peroxide solution E；
F, synthetic reaction
When synthetic reaction starts, according to the generated time t of determination, C solution is added in solution A with y/t flow and mixed, simultaneously
With（x+y）/ t flow velocity adds A, C mixed solution and B solution, solution D cocurrent in reactor, stirring intensity be 200~
Reacted under 500 revs/min, the cobalt hydroxide and lithium carbonate mixture of the distribution of doped chemical gradient, reaction temperature is prepared
Spend for 50~80 DEG C, the flow velocity of B solution is 0.5~0.7 times of A, C mixing flow velocity, and the flow velocity of solution D is adjusted according to pH value in reaction
Section, pH value in reaction are 8~10, and generated time is 8~40h；
G, oxidation reaction
After end of synthesis, D, E solution are added in reactor with certain flow velocity, are 200~500 revs/min in stirring intensity
Lower that cobalt hydroxide precipitation is oxidized into hydroxy cobalt oxide, reaction temperature is 60~80 DEG C, and oxidization time is 1~2h, and E solution adds
Measure as 0.2~0.5 times of solution A addition, the flow velocity of solution D is adjusted according to pH value in reaction, and pH value in reaction is 10~11；
H, filtering, washing and drying
Material is filtered after the completion of reaction, washed, dries, obtains grade doping cobalt acid lithium presoma product；
I, calcine
The product of step (h) is calcined, obtains grade doping cobalt acid lithium product.
Preferably, in the step (a), the cobalt salt is that the one or more in cobaltous sulfate, cobalt nitrate and cobalt chloride are mixed
Compound, the lithium salts are one or both of lithium nitrate and lithium chloride mixture.
Preferably, in the step (c), the doped chemical soluble salt is Mg, Al, Mn, Cu, Cr, Zr, Ce, Y, Nb, Ni
In one in or several chlorides or nitric acid thing.
Preferably, in the step (h), the washing material is using 80~100 DEG C of deionized water, dried material
Temperature be 100~400 DEG C.
Preferably, in the step (i), the calcination condition is in air atmosphere, calcining heat is 850 DEG C~1050
DEG C, calcination time is 4~6h.
Preferably, in the step (g), the physical and chemical indexes of the grade doping cobalt acid lithium product include：Doped chemical contains
Amount is in the distribution of 0~2%, doped chemical gradient, laser particle size in 5~15 microns, Zhen Shi Mi Du≤2.0g/cm3, specific surface area 0.2
~0.6m2/ g, pattern are block or spherical.
Beneficial effects of the present invention are：
（1）The present invention adds the amount gradient increase of dopant in reactor, makes doping first by extending with synthesising reacting time
Element distribution gradient in the product, Moist chemical synthesis go out the distribution of doped chemical gradient and the mixed uniformly sediment of lithium, cobalt, then by hydrogen
Cobalt oxide is oxidized to hydroxy cobalt oxide, finally by calcining, obtains the doping cobalt acid lithium product of doped chemical gradient distribution.This hair
Bright avoid needs doped chemical oxide, cobalt/cobalt oxide, lithium carbonate etc. for a long time in Traditional dopant cobalt acid lithium preparation process
Batch mixing and doped chemical Local enrichment still can not be avoided completely, be easily separated, the shortcomings that weakening material property.
（2）The present invention is after Moist chemical synthesis terminates, by hydroxide cobalt oxide by way of adding hydrogen peroxide into reactor
Hydroxy cobalt oxide is melted into, the step of so avoiding to need to be passed through compressed air or other oxidizing gas in calcination process,
Production process is not produced dust, it is pollution-free, environment-friendly, and it also avoid being passed through unclean compressed air or other
Oxidizing gas causes the risk of cobalt acid lithium product impurity content exceeding index, and the requirement to calciner is also relatively easy.
Brief description of the drawings
Fig. 1 is the testing result of the synthetic product of embodiment 1；
Fig. 2 is the 2-in-1 testing result into product of embodiment；
Fig. 3 is the testing result of the synthetic product of embodiment 3.
Embodiment
Embodiment one
Production stage is same as above, and the design parameter in each step is as follows：
The solution A of preparation is cobalt chloride and lithium chloride mixed solution, and cobalt concentration is 1mol/L, lithium concentration 1.2mol/L, body
Product is 120L.
The B solution of preparation is 1.2mol/L ammonium bicarbonate soln.
The total amount for preparing magnesium chloride solution 10L, Mg that C solution is 5.9g/L is the 0.5% of end product quality.
Prepare the sodium hydroxide solution that solution D is 2.5mol/L.
Prepare the hydrogen peroxide solution that E solution is 2mol/L.
When synthetic reaction starts, reaction time 16h is determined according to preparation technology, C solution is added with 0.625L/h flow
Enter in solution A, while added A, C mixed solution, B solution, solution D cocurrent in reactor with 8.125L/h flow velocity, stirring
It is to be reacted under 250 revs/min to mix intensity, and the cobalt hydroxide that the distribution of doped chemical gradient is prepared mixes with lithium carbonate
Thing.；The temperature of reaction system is 60 DEG C, and the flow velocity of B solution is 0.55 times of A, C mixing flow velocity, and the flow velocity of solution D is according to anti-
PH value is answered to adjust, the pH value of reaction system is 10.
The flow velocity of solution D is adjusted according to pH value in reaction in oxidizing process, pH value 10.5, and reaction temperature is 60 DEG C, oxidation
Time is 1h, and E solution addition is 0.25 times of solution A addition.
For pulping and washing material using 90 DEG C of deionized water, the temperature of dried material is 150 DEG C.
The condition of calcining materials is in air atmosphere, calcining heat is 900 DEG C, calcination time 4h.
The product indices of preparation are shown in accompanying drawing 1.
Embodiment two
This example and embodiment one are essentially identical, and simply following adjustment parameter is different：
The solution A of preparation is cobalt nitrate and lithium nitrate mixed solution, and cobalt concentration is 1.5mol/L, lithium concentration 2mol/L, body
Product is 250L.
The B solution of preparation is 2mol/L ammonium bicarbonate soln.
The aluminum nitrate and nickel chloride solution 30L that C solution is 12.3g/L are prepared, and the total amount of aluminium and nickel is final products matter
The 1% of amount.
Prepare the sodium hydroxide solution that solution D is 5mol/L.
Prepare the hydrogen peroxide solution that E solution is 3mol/L.
When synthetic reaction starts, reaction time 30h is determined according to preparation technology, C solution is added into A with 1.0L/h flow
In solution, while A, C mixed solution, B solution, solution D cocurrent are added in reactor with 9.3L/h flow velocity, stirring intensity is
Reacted under 350 revs/min, the cobalt hydroxide and lithium carbonate mixture of the distribution of doped chemical gradient is prepared.Reactant
The temperature of system is 70 DEG C, and the flow velocity of B solution is 0.6 times of A, C mixing flow velocity, and the flow velocity of solution D is adjusted according to pH value in reaction,
The pH value of reaction system is 9.0.
The flow velocity of solution D is adjusted according to pH value in reaction in oxidizing process, pH value 10, and reaction temperature is 70 DEG C, during oxidation
Between be 1.5h, E solution addition is 0.3 times of solution A addition.
For pulping and washing material using 80 DEG C of deionized water, the temperature of dried material is 300 DEG C.
The condition of calcining materials is in air atmosphere, calcining heat is 1000 DEG C, calcination time 5h.
The product indices of preparation are shown in accompanying drawing 2.
Embodiment three
This example and embodiment one are essentially identical, and simply following adjustment parameter is different：
The solution A of preparation is cobaltous sulfate and lithium chloride mixed solution, and cobalt concentration is 2mol/L, lithium concentration 2.5mol/L, body
Product is 500L.
The B solution of preparation is 2.5mol/L ammonium bicarbonate soln.
The total amount of the copper nitrate and yttrium chloride solution 100L that preparation C solution is 19.6g/L, copper and yttrium is end product quality
2%.
Prepare the sodium hydroxide solution that solution D is 4mol/L.
Prepare the hydrogen peroxide solution that E solution is 4mol/L.
When synthetic reaction starts, according to preparation technology, reaction time 40h is determined, C solution is added with 1.67L/h flow
Enter in solution A, while added A, C mixed solution, B solution, solution D cocurrent in reactor with 10L/h flow velocity, stirring intensity
To be reacted under 450 revs/min, the cobalt hydroxide and lithium carbonate mixture of the distribution of doped chemical gradient is prepared.Reaction
The temperature of system is 75 DEG C, and the flow velocity of B solution is 0.65 times of A, C mixing flow velocity, and the flow velocity of solution D is adjusted according to pH value in reaction
Section, the pH value of reaction system is 8.5.
The flow velocity of solution D is adjusted according to pH value in reaction in oxidizing process, pH value 11, and reaction temperature is 75 DEG C, during oxidation
Between be 2h, E solution addition is 0.4 times of solution A addition.
For pulping and washing material using 95 DEG C of deionized water, the temperature of dried material is 400 DEG C.
The condition of calcining materials is in air atmosphere, calcining heat is 950 DEG C, calcination time 6h.
The product index of preparation is shown in accompanying drawing 3.
Claims (6)
1. a kind of preparation method of grade doping cobalt acid lithium, it is characterised in that concretely comprise the following steps：
A, solution A is prepared
Using cobalt salt, lithium salts as raw material, the lithium cobalt mixed solution A that cobalt concentration is 1~2mol/L is configured to, and lithium cobalt mol ratio is 1：
1~1：4, precise volume is that x A is standby；
B, B solution is prepared
Compound concentration is 1~2mol/L ammonium bicarbonate soln B, and ammonium hydrogencarbonate concentration is identical with lithium molar concentration in A in B；
C, C solution is prepared
Compound concentration is 5.9~19.6g/L doped chemical soluble salt solution C, is produced according to the concentration of cobalt, x amount, preparation in A
Doped chemical concentration in the doped chemical doping and C of product requirement, according to formula：C solution volume=（X*A solution cobalt solubility *
Doping）/（Cobalt content in C solution doped chemical concentration * cobalt acid lithiums）, be calculated needed for C volume this volume be set to y；
D, compound concentration is 2~8mol/L sodium hydroxide solution D；
E, configuration concentration is 1~5mol/L hydrogen peroxide solution E；
F, synthetic reaction
When synthetic reaction starts, according to the generated time t of determination, C solution is added in solution A with y/t flow and mixed, simultaneously
With（x+y）/ t flow velocity adds A, C mixed solution and B solution, solution D cocurrent in reactor, stirring intensity be 200~
Reacted under 500 revs/min, the cobalt hydroxide and lithium carbonate mixture of the distribution of doped chemical gradient, reaction temperature is prepared
Spend for 50~80 DEG C, the flow velocity of B solution is 0.5~0.7 times of A, C mixing flow velocity, and the flow velocity of solution D is adjusted according to pH value in reaction
Section, pH value in reaction are 8~10, and generated time is 8~40h；
G, oxidation reaction
After end of synthesis, D, E solution are added in reactor with certain flow velocity, are 200~500 revs/min in stirring intensity
Lower that cobalt hydroxide precipitation is oxidized into hydroxy cobalt oxide, reaction temperature is 60~80 DEG C, and oxidization time is 1~2h, and E solution adds
Measure as 0.2~0.5 times of solution A addition, the flow velocity of solution D is adjusted according to pH value in reaction, and pH value in reaction is 10~11；
H, filtering, washing and drying
Material is filtered after the completion of reaction, washed, dries, obtains grade doping cobalt acid lithium presoma product；
I, calcine
The product of step (h) is calcined, obtains grade doping cobalt acid lithium product.
A kind of 2. preparation method of grade doping cobalt acid lithium according to claim 1, it is characterised in that：The step (a)
In, the cobalt salt is one or more of mixtures in cobaltous sulfate, cobalt nitrate and cobalt chloride, and the lithium salts is lithium nitrate and chlorination
One or both of lithium mixture.
A kind of 3. preparation method of grade doping cobalt acid lithium according to claim 1 or 2, it is characterised in that：The step
(c) in, the doped chemical soluble salt be Mg, Al, Mn, Cu, Cr, Zr, Ce, Y, Nb, Ni in one in or several chlorides or
Nitric acid thing.
A kind of 4. preparation method of grade doping cobalt acid lithium according to claim 3, it is characterised in that：The step (h)
In, for the washing material using 80~100 DEG C of deionized water, the temperature of dried material is 100~400 DEG C.
A kind of 5. preparation method of grade doping cobalt acid lithium according to claim 1 or 4, it is characterised in that：The step
(i) in, the calcination condition is in air atmosphere, calcining heat is 850 DEG C~1050 DEG C, and calcination time is 4~6h.
A kind of 6. preparation method of grade doping cobalt acid lithium according to claim 5, it is characterised in that：The step (g)
In, the physical and chemical indexes of the grade doping cobalt acid lithium product include：Doped chemical content 0~2%, doped chemical gradient be distributed,
Laser particle size is in 5~15 microns, Zhen Shi Mi Du≤2.0g/cm3, 0.2~0.6m of specific surface area2/ g, pattern are block or class ball
Shape.
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Cited By (6)
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| CN108545783A (en) * | 2018-04-03 | 2018-09-18 | 兰州金川新材料科技股份有限公司 | A kind of preparation method for lithium ion cell anode material lithium cobaltate |
| CN108649205A (en) * | 2018-05-15 | 2018-10-12 | 哈尔滨工业大学 | A kind of anode material for lithium-ion batteries and its preparation with variable slope concentration gradient doped structure |
| CN110518217A (en) * | 2019-09-03 | 2019-11-29 | 中伟新材料有限公司 | A kind of preparation method of grade doping spherical nucleocapsid cobalt acid lithium material, its presoma and the two |
| CN112531154A (en) * | 2020-11-23 | 2021-03-19 | 合肥国轩高科动力能源有限公司 | Preparation method of tungsten trioxide micro-nano particle gradient doped ternary material, prepared ternary material and application |
| WO2021120040A1 (en) * | 2019-12-17 | 2021-06-24 | 格林美（江苏）钴业股份有限公司 | Method for preparing high-density aluminum-doped cobalt oxide |
| CN115275209A (en) * | 2022-09-28 | 2022-11-01 | 四川启睿克科技有限公司 | High-first-efficiency silicon cathode with stable structure, preparation method and lithium ion battery |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108545783A (en) * | 2018-04-03 | 2018-09-18 | 兰州金川新材料科技股份有限公司 | A kind of preparation method for lithium ion cell anode material lithium cobaltate |
| CN108649205A (en) * | 2018-05-15 | 2018-10-12 | 哈尔滨工业大学 | A kind of anode material for lithium-ion batteries and its preparation with variable slope concentration gradient doped structure |
| CN110518217A (en) * | 2019-09-03 | 2019-11-29 | 中伟新材料有限公司 | A kind of preparation method of grade doping spherical nucleocapsid cobalt acid lithium material, its presoma and the two |
| CN110518217B (en) * | 2019-09-03 | 2020-10-30 | 中伟新材料股份有限公司 | Gradient doped spherical core-shell lithium cobaltate material, precursor thereof and preparation methods of gradient doped spherical core-shell lithium cobaltate material and precursor |
| WO2021120040A1 (en) * | 2019-12-17 | 2021-06-24 | 格林美（江苏）钴业股份有限公司 | Method for preparing high-density aluminum-doped cobalt oxide |
| CN112531154A (en) * | 2020-11-23 | 2021-03-19 | 合肥国轩高科动力能源有限公司 | Preparation method of tungsten trioxide micro-nano particle gradient doped ternary material, prepared ternary material and application |
| CN112531154B (en) * | 2020-11-23 | 2022-04-22 | 合肥国轩高科动力能源有限公司 | Preparation method of tungsten trioxide micro-nano particle gradient doped ternary material, prepared ternary material and application |
| CN115275209A (en) * | 2022-09-28 | 2022-11-01 | 四川启睿克科技有限公司 | High-first-efficiency silicon cathode with stable structure, preparation method and lithium ion battery |
| CN115275209B (en) * | 2022-09-28 | 2023-03-10 | 四川启睿克科技有限公司 | High-first-efficiency silicon cathode with stable structure, preparation method and lithium ion battery |
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Application publication date: 20180330 |