CN108298596A - A kind of preparation method of big granularity doped cobaltic-cobaltous oxide - Google Patents
A kind of preparation method of big granularity doped cobaltic-cobaltous oxide Download PDFInfo
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Abstract
The present invention proposes a kind of preparation method of big granularity doped cobaltic-cobaltous oxide, it is using certain density cobalt liquor as cobalt source, sodium carbonate liquor is precipitating reagent, ammonia spirit is complexing agent, hydrazine hydrate solution is reducing agent, and doped chemical solution is dopant with complexing agent mixed liquor, and by reducing the modes such as synthesis initial stage nucleus generation quantity, Moist chemical synthesis goes out the cobalt carbonate that granularity is 20~30 μm in the shortest time, during the reaction, it selects the suitable time that doped solution is added in reaction kettle to participate in reacting；After synthesis under certain pH value condition, synthetic product is oxidized to hydroxy cobalt oxide using the hydrogen peroxide solution of certain solubility, then by mixture washing, dry, calcining, obtains big granularity doped cobaltic-cobaltous oxide product.This technique generated time is short only to need 10~15h, and product physical and chemical indexes are good, and for laser particle size at 15~25 μm, tap density is more than 2.0g/cm3, 1.0~3.0m of specific surface area2/ g, can doped chemical include Ni, Mn, Al, Cu, Ce, Y, Nb, Mg.
Description
Technical field
The invention belongs to technical field of lithium ion, and in particular to one kind being used to prepare ion cell anode material lithium cobaltate
The big granularity doped cobaltic-cobaltous oxide preparation method of lithium.
Background technology
Cobalt acid lithium is the lithium ion battery prepared by positive electrode with light-weight, capacity is big, operating voltage higher than energy
Height, electric discharge is steady, is suitble to the features such as heavy-current discharge, good cycle, long lifespan, is mainly used in 3C digital domains.
Cobalt acid lithium just develops towards the direction of high voltage, high-pressure solid, high circulation performance, is wanted to raw material cobaltosic oxide
Ask higher and higher.Co3O4It is a kind of functional material with special construction and performance, regular particle size（5-10 microns）Co3O4City
Field has faced the present situation of gradually atrophy, and big granularity adulterates Co3O4The market demand gradually highlight.How research prepares high-performance
Big granularity doped cobaltic-cobaltous oxide has become hot spot.
Chinese invention patent CN201510881580.4 discloses " a kind of big grain size high-density spherical cobaltic-cobaltous oxide
Preparation method ", specific production method are to pass through segmentation by cobalt carbonate made from multiple circulation crystallization in cobalt carbonate synthesis phase
Formula thermally decomposes, and makes cobalt carbonate exploded in the low temperature predecomposition stage, forms micro channel, in the high temperature thermal decomposition stage, particle
Surface densification, to which big grain size high-density spherical cobaltic-cobaltous oxide be prepared.This patent is needed in cobalt carbonate synthesis phase
Multiple circulation crystallization, process is cumbersome, is unfavorable for industrialized production.Chinese invention patent CN201210486483.1, discloses " one
Doped chemical ion, is specifically incorporated into cobalt salt solution and is configured to mix by the preparation method of kind doping spherical cobaltosic oxide "
Miscellaneous mixed solution is passed into reaction unit simultaneously with hydroxide solution and air, and is constantly stirred and is made its reaction,
Prepare doping spherical cobaltosic oxide.Chinese invention patent CN200810110753.2 discloses a kind of " four oxidation three of doping
Doped chemical ion is specifically incorporated into cobalt salt solution and is configured to doping mixed solution, and contains ammonia by the preparation method of cobalt "
The hydroxide solution of water is passed into reaction unit simultaneously makes its reaction, and doping ball is prepared using washing, drying, calcining
Shape cobaltosic oxide.It is precipitating reagent that this two kinds of preparation methods, which are all made of hydroxide, different from the used precipitating reagent of the application, and
Doped cobaltic-cobaltous oxide preparation method and big granularity cobaltosic oxide preparation method prepared by the application are significantly different.
Invention content
The purpose of the invention is to overcome the shortcomings of above-mentioned technology, it is simple and easy to control to provide a kind of production process to this field
Big granularity doped cobaltic-cobaltous oxide preparation method.
Technical scheme of the present invention：A kind of preparation method of big granularity doped cobaltic-cobaltous oxide, the method is characterized in that
Specific steps：
A, solution A is prepared
Using cobalt salt as raw material, it is solution A to prepare the cobalt liquor that cobalt concentration is 1~2mol/L；
B, B solution is prepared
The sodium carbonate liquor that compound concentration is 1~2mol/L is B solution, and sodium carbonate molar concentration and cobalt in solution A in B solution
Molar concentration is identical；
C, C solution is prepared
Compound concentration is the ammonia spirit of 5~10mol/L, and it is 30% that 5~20ml mass contents are added in every liter of ammonia spirit
Hydrazine hydrate solution is C solution；
D, solution D is prepared
The hydrogen peroxide solution that configuration concentration is 5~10mol/L is solution D；
E, E solution is prepared
The sodium hydroxide solution that configuration concentration is 2~6mol/L is E solution；
F, F solution is prepared
The doped chemical soluble salt solution that compound concentration is 5~50g/L is F solution；
G, synthetic reaction
When synthetic reaction starts, while solution A, B solution, C solution cocurrent being added in reaction kettle, according to doping element compound
Chemical property selection selects the suitable time that F solution is added in reaction kettle, carries out cobalt carbonate synthetic reaction, reaction under stiring
Solution ammonia density, reaction temperature, A and B solution flow velocity, stirring intensity and reaction time are strictly controlled in reaction kettle in the process；
H, it aoxidizes
After synthesis, D, E solution are added in reaction kettle simultaneously, cobalt carbonate precipitation is oxidized to hydroxyl oxidation under stiring
Cobalt, stringent control ph, reaction temperature, oxidization time in oxidation process；
I, it is filtered, washed and dries
After oxidation process, material is filtered, pulping and washing, drying, obtains big granularity doped cobaltic-cobaltous oxide forerunner
Body product；
J, it calcines
The product of step i is calcined under calcination condition, obtains big granularity doped cobaltic-cobaltous oxide product.
In the step a, the cobalt salt is one or more of cobaltous sulfate, cobalt nitrate or cobalt chloride.
In the step f, the doped chemical soluble salt is in one in Ni, Mn, Al, Cu, Ce, Y, Nb, Mg or several
Chloride or nitric acid object.
It is described to select the suitable time that F solution is added instead according to doping element compound chemical property in the step g
It is described when answering in kettle to select reaction to start according to doping element compound chemical property or in reaction process or after reaction
Solution ammonia density in reaction kettle, reaction temperature, A and B solution flow velocity, stirring intensity and reaction time are strictly controlled in reaction process
In solution ammonia density be 5~10g/L, reaction temperature be 60~80 DEG C, solution A flow velocity be the reaction time section 0~1h flow velocitys
100L/h, reaction time section 1~2h flow velocitys 200L/h, reaction time section 2~3h flow velocitys be 300L/h, reaction time 3~4h of section
It until synthetic reaction terminates flow velocity is 500L/h that flow velocity, which is after 400L/h, 4h, the flow velocity of B solution be solution A flow velocity 1.0~
1.1 times, stirring intensity is 200~500 revs/min, and the reaction time is 10~15h.
PH value in the oxidation process in stringent control ph, reaction temperature, oxidization time is 10~11, reaction temperature
It it is 60~80 DEG C, oxidization time is 1~2h.
In the step i, the material pulping and washing is using 80~100 DEG C of deionized water, the temperature of dry materials
Degree is 100~400 DEG C.
In the step j, calcination condition be under conditions of without being passed through oxidizing gas, calcination temperature be 700 DEG C~
800 DEG C, calcination time is 2~5h.
The physical and chemical indexes of the big granularity doped cobaltic-cobaltous oxide product of gained are in step j：Laser particle size 15~25 μm, shake
Shi Mi Du≤2.0g/cm3, 1.0~3.0m of specific surface area2/ g, doped chemical include Ni, Mn, Al, Cu, Ce, Y, Nb, Mg and doping
Amount is 0~2%, and pattern is spherical or spherical.
The characteristics of this method is：Using certain density cobalt liquor as cobalt source, sodium carbonate liquor is precipitating reagent, and ammonia spirit is
Complexing agent, hydrazine hydrate solution are reducing agent, and doped chemical solution is dopant with complexing agent mixed liquor, by reducing synthesis initial stage
Moist chemical synthesis goes out the cobalt carbonate that granularity is 20~30 μm to the modes such as nucleus generation quantity in the shortest time, during the reaction,
It selects the suitable time that doped solution is added in reaction kettle to participate in reacting；After synthesis under certain pH value condition, profit
Synthetic product is oxidized to hydroxy cobalt oxide with the hydrogen peroxide solution of certain solubility, then mixture is washed, is dry, calcining,
Obtain big granularity doped cobaltic-cobaltous oxide product.
The beneficial effects of the invention are as follows：The present invention reduces carbon by way of reducing synthetic reaction incipient stage liquid inventory
Sour cobalt nucleus generation quantity avoids the carbonic acid cobalt oxidation generated by way of reducing agent hydrazine hydrate is added, can be in the short time
Cobalt carbonate product of the laser particle size at 15~25 μm is inside prepared, and then prepares laser particle size at 15~25 μm, tap density
More than 2.0g/cm3, 1.0~3.0m of specific surface area2The spherical or spherical cobaltosic oxide product of/g.
The present invention is by the way that after Moist chemical synthesis, cobalt carbonate is oxidized to hydroxyl by the mode that hydrogen peroxide is added into reaction kettle
Base cobalt oxide makes production the step of avoiding to need to be passed through compressed air or other oxidizing gas in calcination process in this way
Process not will produce dust, pollution-free, environmental-friendly.And it also avoids being passed through unclean compressed air or other oxidisability
Gas causes the risk of cobalt acid lithium product impurity content exceeding index, and the requirement to calciner is also relatively easy.
Description of the drawings
Fig. 1 is the SEM figures of 1 synthetic product of embodiment；
Fig. 2 is the SEM figures of 2 synthetic product of embodiment；
Fig. 3 is the SEM figures of 3 synthetic product of embodiment；
Fig. 4 is the process flow chart of the present invention.
Specific implementation mode
Embodiment 1
Production stage is same as above, and details are not described herein again.Design parameter in each step is as follows：
The solution A of configuration is 1mol/L cobalt chloride solutions.
The B solution of preparation is the sodium carbonate liquor of 1mol/L.
The C solution of configuration is the ammonia spirit of 5mol/L, and it is 30% that 5mL mass contents are added in every liter of ammonia spirit
Hydrazine hydrate solution.
The solution D of configuration is the hydrogen peroxide solution of 5mol/L.
The E solution of configuration is the sodium hydroxide solution of 2mol/L.
The F solution of configuration is the cerous nitrate solution of 8.1g/L.
Synthetic reaction：When synthetic reaction starts, by solution A, B solution, C solution, F solution, reaction kettle is added in cocurrent simultaneously
In, cobalt carbonate synthetic reaction is carried out under vigorous stirring, and the ammonia density that reaction solution is strictly controlled in reaction process is 5g/L, instead
It is 70 DEG C to answer the temperature of system, and solution A flow velocity is reaction time section 0~1h flow velocitys 100L/h, 1~2h of period flow velocity 200L/
H, 2~3h of period flow velocitys are 300L/h, 3~4h of period flow velocity is 400L/h, 4h later until synthetic reaction terminates flow velocity
For 500L/h, the flow velocity of B solution is 1.02 times of the corresponding flow velocity of each period solution A, and the flow velocity of F solution is each period
Corresponding 0.1 times of solution A, stirring intensity are 300 revs/min, reaction time 10h.
Oxidation reaction：After synthesis, D, E solution are added in reaction kettle simultaneously, under vigorous stirring by carbonic acid cobalt oxide
It is melted into hydroxy cobalt oxide, stringent control ph is 10.0 in oxidation process, and reaction temperature is 70 DEG C, oxidization time 1h, dioxygen
Water usage amount is react cobalt mole 0.5 times.
After oxidation process, material is filtered, pulping and washing, drying, obtains big granularity doped cobaltic-cobaltous oxide
Presoma product.The temperature of 80 DEG C of the deionized water that material washing uses, dry materials is 200 DEG C.
Calcining：Calcination temperature is 700 DEG C, calcination time 2h, calcines, obtains without being passed through under conditions of oxidizing gas
Big granularity doped cobaltic-cobaltous oxide product.
The product index of preparation is shown in Table 1, and product shape appearance figure is shown in attached drawing Fig. 1.
The physical and chemical indexes of 1 embodiment of table, 1 product
Embodiment 2
Production stage is same as above, and details are not described herein again.Design parameter in each step is as follows：
The solution A of configuration is 1.5mol/L cobalt sulfate solutions.
The B solution of preparation is the sodium carbonate liquor of 1.5mol/L.
The C solution of configuration is the ammonia spirit of 8mol/L, and it is 30% that 15mL mass contents are added in every liter of ammonia spirit
Hydrazine hydrate solution.
The solution D of configuration is the hydrogen peroxide solution of 6mol/L.
The E solution of configuration is the sodium hydroxide solution of 4mol/L.
The F solution of configuration is the magnesium chloride solution of 16.2g/L.
Synthetic reaction：When synthetic reaction starts, solution A, B solution, C solution cocurrent are added in reaction kettle, synthetic reaction
After 50h, by F solution in 0.2 times of addition reaction kettle of cobalt sulfate solution flow velocity, it is anti-to carry out cobalt carbonate synthesis under vigorous stirring
It answers, the ammonia density that reaction solution is strictly controlled in reaction process is 8g/L, and the temperature of reaction system is 65 DEG C, and solution A flow velocity is
Reaction time section 0~1h flow velocitys 100L/h, 1~2h of period flow velocity 200L/h, 2~3h of period flow velocity are 300L/h, time
Section 3~4h flow velocitys are 400L/h, to terminate flow velocity be 500L/h to period 4h~synthetic reaction, and the flow velocity of B solution is each time
1.05 times of the corresponding flow velocity of section solution A, stirring intensity are 200 revs/min, reaction time 12h.
Oxidation reaction：After synthesis, D, E solution are added in reaction kettle simultaneously, under vigorous stirring by carbonic acid cobalt oxide
It is melted into hydroxy cobalt oxide, control ph is 10.5 in oxidation process, and reaction temperature is 65 DEG C, and oxidization time 2h, hydrogen peroxide makes
Dosage is react cobalt mole 0.6 times.
After oxidation process, material is filtered, pulping and washing, drying, obtains big granularity doped cobaltic-cobaltous oxide
Presoma product.Using 90 DEG C of deionized water, the temperature of dry materials is 300 DEG C for material washing.
Calcining：Calcination temperature is 750 DEG C, calcination time 5h, calcines, obtains without being passed through under conditions of oxidizing gas
Big granularity doped cobaltic-cobaltous oxide product.
The product index of preparation is shown in Table 2, and product shape appearance figure is shown in attached drawing Fig. 2.
The physical and chemical indexes of 2 embodiment of table, 2 product
Embodiment 3
Production stage is same as above, and details are not described herein again.Design parameter in each step is as follows：
The solution A of configuration is 2mol/L cobalt nitrate solutions.
The B solution of preparation is the sodium carbonate liquor of 2mol/L.
The C solution of configuration is the ammonia spirit of 10mol/L, and it is 30% that 20mL mass contents are added in every liter of ammonia spirit
Hydrazine hydrate solution.
The solution D of configuration is the hydrogen peroxide solution of 8mol/L.
The E solution of configuration is the sodium hydroxide solution of 6mol/L.
The F solution of configuration is the aluminum trichloride solution of 48.6g/L.
Synthetic reaction：When synthetic reaction starts, solution A, B solution, C solution cocurrent are added in reaction kettle, stirred strongly
Lower progress cobalt carbonate synthetic reaction is mixed, after synthesis, F solution is added with cobalt nitrate solution flow velocity in reaction kettle and is participated in instead
It answers, reaction time 1h, the ammonia density that reaction solution is controlled in reaction process is 6g/L, and the temperature of reaction system is 75 DEG C, solution A
Flow velocity is reaction time section 0~1h flow velocitys 100L/h, reaction time section 1~2h flow velocitys 200L/h, reaction time section 2~3h flow velocitys
For 300L/h, reaction time section 3~4h flow velocitys be 400L/h, to terminate flow velocity be 500L/h, B to reaction time section 4h~synthetic reaction
The flow velocity of solution is 1.1 times of the corresponding flow velocity of each period solution A, and stirring intensity is 500 revs/min, and the reaction time is
15h。
Oxidation reaction：After synthesis, D, E solution are added in reaction kettle simultaneously, under vigorous stirring by carbonic acid cobalt oxide
It is melted into hydroxy cobalt oxide, control ph is 11 in oxidation process, and reaction temperature is 75 DEG C, oxidization time 2h, and hydrogen peroxide uses
Amount is 0.55 times of reaction cobalt mole.
After oxidation process, material is filtered, pulping and washing, drying, obtains big granularity doped cobaltic-cobaltous oxide
Presoma product.The temperature condition of 90 DEG C of the deionized water that washing material uses, dry materials is 400 DEG C.
Calcining：Calcination temperature is 780 DEG C, calcination time 4h, calcines, obtains without being passed through under conditions of oxidizing gas
Big granularity doped cobaltic-cobaltous oxide product.
The product index of preparation is shown in Table 3, and product shape appearance figure is shown in attached drawing Fig. 3.
The physical and chemical indexes of 3 embodiment of table, 3 product
。
Claims (7)
1. a kind of preparation method of big granularity doped cobaltic-cobaltous oxide, the method is characterized in that specific steps：
A, solution A is prepared
Using cobalt salt as raw material, it is solution A to prepare the cobalt liquor that cobalt concentration is 1~2mol/L；
B, B solution is prepared
The sodium carbonate liquor that compound concentration is 1~2mol/L is B solution, and sodium carbonate molar concentration and cobalt in solution A in B solution
Molar concentration is identical；
C, C solution is prepared
Compound concentration is the ammonia spirit of 5~10mol/L, and it is 30% that 5~20ml mass contents are added in every liter of ammonia spirit
Hydrazine hydrate solution is C solution；
D, solution D is prepared
The hydrogen peroxide solution that configuration concentration is 5~10mol/L is solution D；
E, E solution is prepared
The sodium hydroxide solution that configuration concentration is 2~6mol/L is E solution；
F, F solution is prepared
The doped chemical soluble salt solution that compound concentration is 5~50g/L is F solution；
G, synthetic reaction
When synthetic reaction starts, while solution A, B solution, C solution cocurrent being added in reaction kettle, according to doping element compound
Chemical property selects the suitable time that F solution is added in reaction kettle, carries out cobalt carbonate synthetic reaction, reaction process under stiring
In strictly control solution ammonia density in reaction kettle, reaction temperature, A and B solution flow velocity, stirring intensity and reaction time；
H, it aoxidizes
After synthesis, D, E solution are added in reaction kettle simultaneously, cobalt carbonate precipitation is oxidized to hydroxyl oxidation under stiring
Cobalt, stringent control ph, reaction temperature, oxidization time in oxidation process；
I, it is filtered, washed and dries
After oxidation process, material is filtered, pulping and washing, drying, obtains big granularity doped cobaltic-cobaltous oxide forerunner
Body product；
J, it calcines
The product of step i is calcined under certain conditions, obtains big granularity doped cobaltic-cobaltous oxide product.
2. a kind of preparation method of big granularity doped cobaltic-cobaltous oxide according to claim 1, it is characterized in that：The step
In a, the cobalt salt is one or more of cobaltous sulfate, cobalt nitrate or cobalt chloride.
3. a kind of preparation method of big granularity doped cobaltic-cobaltous oxide according to claim 1, it is characterized in that：The step
In f, the doped chemical soluble salt be in Ni, Mn, Al, Cu, Ce, Y, Nb, Mg one in or several chlorides or nitric acid object.
4. a kind of preparation method of big granularity doped cobaltic-cobaltous oxide according to claim 1, it is characterized in that：The step
It is described to select the suitable time that F solution is added in reaction kettle as according to doping according to doping element compound chemical property in g
Element compound chemical property is strictly controlled when reacting beginning or in reaction process or after reaction in the reaction process
Solution ammonia density, reaction temperature, A and B solution flow velocity, stirring intensity and the solution ammonia density in the reaction time are 5 in reaction kettle
~10g/L, reaction temperature are 60~80 DEG C, solution A flow velocity is reaction time section 0~1h flow velocitys 100L/h, reaction time section 1~
2h flow velocitys 200L/h, reaction time section 2~3h flow velocitys are 300L/h, reaction time section 3~4h flow velocitys are straight after 400L/h, 4h
It is 500L/h to terminate flow velocity to synthetic reaction, and the flow velocity of B solution is 1.0~1.1 times of synthetic reaction process solution A flow velocity, is stirred
It is 200~500 revs/min to mix intensity, and the reaction time is 10~15h.
5. a kind of preparation method of big granularity doped cobaltic-cobaltous oxide according to claim 1, it is characterized in that：The oxidation
The pH value in stringent control ph, reaction temperature, oxidization time is 10~11 in the process, and reaction temperature is 60~80 DEG C, oxidation
Time is 1~2h.
6. a kind of preparation method of big granularity doped cobaltic-cobaltous oxide according to claim 1, it is characterized in that：The step
In i, for the material pulping and washing using 80~100 DEG C of deionized water, the temperature of dry materials is 100~400 DEG C.
7. a kind of preparation method of big granularity doped cobaltic-cobaltous oxide according to claim 1, it is characterized in that：The step
In j, calcination condition is under conditions of without being passed through oxidizing gas, and calcination temperature is 700 DEG C~800 DEG C, calcination time 2
~5h.
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| CN108946824A (en) * | 2018-09-14 | 2018-12-07 | 兰州金川新材料科技股份有限公司 | A kind of preparation method of big granularity cobaltosic oxide |
| CN108946825A (en) * | 2018-09-14 | 2018-12-07 | 兰州金川新材料科技股份有限公司 | A kind of preparation method of small grain size cobaltosic oxide |
| CN109205684A (en) * | 2018-09-14 | 2019-01-15 | 兰州金川新材料科技股份有限公司 | A kind of preparation method of small grain size cobaltosic oxide |
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