CN106887585A - A kind of preparation method of new energy battery nickel-cobalt lithium manganate cathode material - Google Patents
A kind of preparation method of new energy battery nickel-cobalt lithium manganate cathode material Download PDFInfo
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- CN106887585A CN106887585A CN201710147663.XA CN201710147663A CN106887585A CN 106887585 A CN106887585 A CN 106887585A CN 201710147663 A CN201710147663 A CN 201710147663A CN 106887585 A CN106887585 A CN 106887585A
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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
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention relates to a kind of preparation method of new energy battery nickel-cobalt lithium manganate cathode material, belong to battery material field.Cobalt liquor is mixed with lithium hydroxide and permanganate, nickel solution, manganese solution are mixed with lithium hydroxide, then by autoclave inner high voltage reaction again after two kinds of mixed liquor mixing and emulsifyings, then sintering prepares nickel-cobalt lithium manganate cathode material in sintering furnace again.The invention provides a kind of preparation method of new energy battery nickel-cobalt lithium manganate cathode material, technological process is short, it is simple to operate, the waste water containing ammonia nitrogen is not produced, the content of nickel cobalt manganese is substantially reduced in waste water, the utilization rate of nickel cobalt manganese is high, low cost, the nickel-cobalt lithium manganate cathode material purity for obtaining is high, and pH is low, it is difficult the moisture absorption, even particle size distribution.
Description
Technical field
The present invention relates to battery material preparation field, and in particular to a kind of new energy battery nickel-cobalt lithium manganate cathode material
Preparation method.
Background technology
Lithium ion battery is the green high-capacity battery of a new generation, with voltage is high, energy density big, good cycle, from
The many merits such as small, memory-less effect, the operating temperature range of discharging be wide, are widely used in mobile phone, notebook computer, number
Camera, video camera, electronic instrument etc., also have in fields such as UPS, electric tool, electric bicycle, electric automobile, energy-storage batteries
There is the application prospect of light.In recent years, the yield of lithium ion battery is skyrocketed through, and application field constantly expands, it has also become two
The eleventh century new high-tech product significant to national economy and people's lives.
Lithium iron phosphate positive material, has prominent advantage in terms of cost, high-temperature behavior, security, it is expected to as dynamic
Power type and the preferable positive electrode of accumulation energy type lithium ion battery.But LiFePO4 has that maximum is as positive electrode
Energy density is relatively low, with the development of electric automobile, requirement more and more higher of the people to course continuation mileage, and the inferior position of LiFePO4
It is just increasingly apparent, and nickel-cobalt lithium manganate cathode material has the advantages that energy density is high, being gradually available on electric automobile, and
And shared ratio is also increasing on electric automobile.
The preparation method of current nickle cobalt lithium manganate is mainly liquid phase synthesis nickel hydroxide cobalt-manganese ternary presoma, then by hydrogen
Cobalt nickel oxide manganses ternary precursor mixing lithium salts, then obtains nickel-cobalt lithium manganate cathode material in oxidizing atmosphere roasting.But this
The problem that technique is present：
1. technological process is long, complex operation, and this technique generally comprises the dispensing of presoma, forerunner's precursor reactant, presoma washing baking
The operations such as batch mixing, calcining, post processing after dry sieving, doping lithium salts, required equipment is more, long flow path, complex operation, production efficiency
It is low.
2. high cost, due to needing to use nickel cobalt manganese salt, precipitating reagent, complexing agent, lithium salts etc., causes supplementary material high cost,
The technological process rate of recovery for causing product long is reduced simultaneously.
3. waste water,waste gas and industrial residue etc. is produced, to environmental pollution, during precursor synthesis, is closed using liquid phase
Into produce largely needs treatment, the danger of the nickel and cobalt containing obtained after to sewage disposal containing ammonia nitrogen, nickel ion, the waste water of cobalt ions
Dangerous discarded object is also required to treatment, while the waste gas containing ammonia for producing during the course of the reaction needs treatment.
The content of the invention
In order to solve the above mentioned problem of prior art presence, the invention provides a kind of new energy battery nickle cobalt lithium manganate
The preparation method of positive electrode, technological process is short, simple to operate, and the waste water containing ammonia nitrogen is not produced, the content of nickel cobalt manganese in waste water
Substantially reduce, the utilization rate of nickel cobalt manganese is high, low cost, the nickel-cobalt lithium manganate cathode material purity for obtaining is high, and pH is low, be difficult to inhale
Tide, even particle size distribution.
The technical solution adopted in the present invention is：
A kind of preparation method of new energy battery nickel-cobalt lithium manganate cathode material, it is characterised in that comprise the following steps：
（1）Cobalt salt crystal is configured to the cobalt liquor that concentration is 0.5-2mol/l, lithium hydroxide is configured to concentration for 4-8mol/
The lithium hydroxide solution of l, is configured to the permanganate solution that concentration is 0.5-2mol/l, by nickel salt crystal and manganese by permanganate
Salt crystal is hybridly prepared into the nickel manganese solution that concentration is 0.5-2mol/l；
（2）Cobalt liquor, lithium hydroxide solution, permanganate solution are mixed and is added, stirring reaction at being 20-100 DEG C in temperature
It is made slurry within 0.5-5 hours, the cobaltⅡ content into solution stops reaction, the cobalt of addition, lithium and permanganic acid less than 0.5g/l
The mol ratio of salt is 1:3-6:0.5-1.5；
（3）Nickel manganese solution is mixed with lithium hydroxide solution, slurry is made within stirring reaction 0.2-2 hours at being 20-100 DEG C in temperature
Material, the mol ratio of the nickel, manganese and lithium of addition is 1:0.125-1:4-12；
（4）By step（2）And step（3）Slurry mixing, stirring and emulsifying 0.5-3 hour, then will emulsify material be put into autoclave
It is interior, then reacted 5-15 hours at 150-300 DEG C, the mol ratio of nickel, cobalt, manganese, lithium and permanganate is 1 in slurry:0.125-
1:0.125-1：4-12:0.06-1.5；
（5）Reaction under high pressure finish after filtering, washing, drying after, material is put into carries out high temperature sintering in sintering furnace, in 800-
1200 DEG C sinter 8-16 hour, then by crushing, batch mixing, screening, obtain nickel-cobalt lithium manganate cathode material except iron.
Further, cobalt salt is at least one in cobaltous sulfate, cobalt nitrate, cobalt acetate, cobalt chloride in described step 1,
Permanganate is at least one in potassium permanganate, violent acid sodium high, permanganic acid, and nickel salt is nickel sulfate, nickel nitrate, nickel acetate, chlorine
Change at least one in nickel, manganese salt is at least one in manganese sulfate, manganese nitrate, manganese acetate, manganese chloride.
Further, speed of agitator is 50-500r/min in described step 2 and step 3.
Further, stirring and emulsifying temperature is 10-80 DEG C in described step 4, and the speed of agitator of emulsification is 500-
1200r/min, the reaction pressure in autoclave is 0.1-0.5mpa, and speed of agitator is 50-500r/min.
Further, washings pH is washed in 7-9 and terminated in washing process in described step 5, and drying to moisture contains
Amount is less than 1wt%, and oxygen or compressed air are passed through in sintering process so that the atmosphere in sintering furnace is oxidizing atmosphere, oxic gas
Concentration >=the 10%vol of oxygen in atmosphere, sieve for 200-400 mesh sieves.
Nickel cobalt manganese is precipitated using lithium hydroxide, nickel cobalt manganese can both be generated the hydroxide of nickel cobalt manganese, while in alkali
Property under the conditions of, cobalt manganese is comparable to be easily oxidized to trivalent cobalt and tetravalent manganese, lithium turn into soluble lithium salts be evenly distributed on it is molten
In liquid, then by reaction under high pressure, liquid phase method has synthesized nickle cobalt lithium manganate tertiary cathode material, then by steps such as washings,
Pure nickle cobalt lithium manganate tertiary cathode material is obtained by high-temperature calcination, the performance of product is improved, while product can be reduced
PH, simultaneous oxidation agent is permanganate, and the manganese of introducing can be used as raw material, it is to avoid the pollution caused to product.
Beneficial effects of the present invention are：
1. flow is short, low cost, simple to operate, using this technique, nickle cobalt lithium manganate is prepared by liquid phase synthesis-high-temperature calcination
Tertiary cathode material, by presoma prepare, mix lithium mix be connected as a single entity with preparation, flow is greatly shortened, and operation is greatly simplified, nickel
The utilization rate of cobalt manganese is greatly improved, while reducing cost.
2. the sewage containing ammonia nitrogen is not produced, while the content of nickel cobalt manganese is substantially reduced in sewage, reduces processing cost, it is right
Environment does not produce harm substantially.
3. the nickel-cobalt lithium manganate cathode material purity for being obtained using the method is high, and pH is low, is difficult the moisture absorption, and size distribution is equal
Even, good product performance obtains positive electrode using liquid phase synthesis, can pass through the pH that washing reduces positive electrode so that in battery
The moisture absorption is difficult in preparation process and influence is produced on battery performance, using the technique of liquid phase synthesis, can easily control product
Granularity and size distribution, size distribution are more uniform, and product purity is higher.
Specific embodiment
Below in conjunction with specific example, to a kind of new energy battery nickle cobalt lithium manganate positive pole material described in the present patent application
The preparation method of material is described and illustrates, in order to which the public is better understood from technology contents of the invention, rather than right
The limitation of the technology contents, under identical or approximate principle, the improvement carried out to the processing step, including reaction bar
Part, agents useful for same improve and replace, reach identical purpose, then all the present patent application technical scheme required for protection it
It is interior.
Embodiment one
A kind of preparation method of new energy battery nickel-cobalt lithium manganate cathode material, it is characterised in that comprise the following steps：
（1）Cobalt salt crystal is configured to the cobalt liquor that concentration is 1.5mol/l, it is 6mol/l's that lithium hydroxide is configured into concentration
Lithium hydroxide solution, the permanganate solution that concentration is 1.5mol/l is configured to by permanganate, and nickel salt crystal and manganese salt is brilliant
Body is hybridly prepared into the nickel manganese solution that concentration is 1.5mol/l；
（2）Cobalt liquor, lithium hydroxide solution, permanganate solution are mixed and is added, stirring reaction 3 hours at being 60 DEG C in temperature
Slurry is made, the cobaltⅡ content into solution stops reaction, the mol ratio of the cobalt, lithium and permanganate of addition less than 0.5g/l
It is 1:4:1；
（3）Nickel manganese solution is mixed with lithium hydroxide solution, stirring reaction is made slurry in 1 hour at being 60 DEG C in temperature, adds
Nickel, manganese and lithium mol ratio be 1:1:6；
（4）By step（2）And step（3）Slurry mixing, stirring and emulsifying 2 hours, then will emulsification material be put into autoclave, so
Reacted 10 hours at 200 DEG C afterwards, the mol ratio of nickel, cobalt, manganese, lithium and permanganate is 1 in slurry:1:1：6:1；
（5）Reaction under high pressure finish after filtering, washing, drying after, material is put into carries out high temperature sintering in sintering furnace, at 1000 DEG C
Sintering 12 hours, then by broken, batch mixing, screening, except iron obtains nickel-cobalt lithium manganate cathode material.
Further, cobalt salt is cobaltous sulfate in described step 1, and permanganate is potassium permanganate, and nickel salt is nickel nitrate, manganese
Salt is manganese sulfate.
Further, described step 2 speed of agitator is 200r/min, and speed of agitator is 250r/min in step 3.
Further, stirring and emulsifying temperature is 70 DEG C in described step 4, and the speed of agitator of emulsification is 1000r/min,
Reaction pressure in autoclave is 0.15mpa, and speed of agitator is 400r/min.
Further, washings pH is washed at 7.2 and terminated in washing process in described step 5, and drying to moisture contains
Amount is less than 1wt%, and oxygen or compressed air are passed through in sintering process so that the atmosphere in sintering furnace is oxidizing atmosphere, oxic gas
Concentration >=the 10%vol of oxygen in atmosphere, sieve for 300 mesh sieves.
The final positive electrode pH for preparing is 8.5, and in 2.5-4.2V, charging capacity is up to 165.8mAh/g, discharge capacity
Up to 162.5mAh/g.
The content of cobalt nickel manganese is respectively 2.1mg/l, 5.8mg/l and 1.5mg/l, the utilization rate of nickel cobalt manganese in the waste water of generation
Reach more than 99.6%.
Embodiment two
A kind of preparation method of new energy battery nickel-cobalt lithium manganate cathode material, it is characterised in that comprise the following steps：
（1）Cobalt salt crystal is configured to the cobalt liquor that concentration is 1.5mol/l, it is 5mol/l's that lithium hydroxide is configured into concentration
Lithium hydroxide solution, the permanganate solution that concentration is 1.5mol/l is configured to by permanganate, and nickel salt crystal and manganese salt is brilliant
Body is hybridly prepared into the nickel manganese solution of concentration respectively 1.8mol/l and 1.08mol/l；
（2）Cobalt liquor, lithium hydroxide solution, permanganate solution are mixed and is added, stirring reaction 2 hours at being 60 DEG C in temperature
Slurry is made, the cobaltⅡ content into solution stops reaction, the mol ratio of the cobalt, lithium and permanganate of addition less than 0.5g/l
It is 1:5:1；
（3）Nickel manganese solution is mixed with lithium hydroxide solution, stirring reaction is made slurry in 1 hour at being 60 DEG C in temperature, adds
Nickel, manganese and lithium mol ratio be 1:0.6:5；
（4）By step（2）And step（3）Slurry mixing, stirring and emulsifying 2 hours, then will emulsification material be put into autoclave, so
Reacted 10 hours at 200 DEG C afterwards, the mol ratio of nickel, cobalt, manganese, lithium and permanganate is 1 in slurry:0.4:0.6：5:0.4；
（5）Reaction under high pressure finish after filtering, washing, drying after, material is put into carries out high temperature sintering in sintering furnace, at 1000 DEG C
Sintering 14 hours, then by broken, batch mixing, screening, except iron obtains nickel-cobalt lithium manganate cathode material.
Further, cobalt salt is cobaltous sulfate in described step 1, and permanganate is permanganic acid, and nickel salt is nickel nitrate, manganese salt
It is manganese acetate.
Further, described step 2 speed of agitator is 200r/min, and speed of agitator is 450r/min in step 3.
Further, stirring and emulsifying temperature is 60 DEG C in described step 4, and the speed of agitator of emulsification is 1100r/min,
Reaction pressure in autoclave is 0.25mpa, and speed of agitator is 400r/min.
Further, washings pH is washed at 7.5 and terminated in washing process in described step 5, and drying to moisture contains
Amount is less than 1wt%, and oxygen or compressed air are passed through in sintering process so that the atmosphere in sintering furnace is oxidizing atmosphere, oxic gas
Concentration >=the 10%vol of oxygen in atmosphere, sieve for 350 mesh sieves.
The final positive electrode pH for preparing is 8.2, and in 2.5-4.2V, charging capacity is up to 167.5mAh/g, discharge capacity
Up to 164.5mAh/g.
The content of cobalt nickel manganese is respectively 2.5mg/l, 10.1mg/l and 1.5mg/l, the utilization of nickel cobalt manganese in the waste water of generation
Rate reaches more than 99.5%.
Embodiment three
A kind of preparation method of new energy battery nickel-cobalt lithium manganate cathode material, it is characterised in that comprise the following steps：
（1）Cobalt salt crystal is configured to the cobalt liquor that concentration is 1mol/l, lithium hydroxide is configured to the hydrogen that concentration is 5mol/l
Lithia solution, is configured to the permanganate solution that concentration is 1.5mol/l, by nickel salt crystal and manganese salt crystal by permanganate
It is hybridly prepared into the nickel manganese solution of concentration respectively 2mol/l, 0.67mol/l；
（2）Cobalt liquor, lithium hydroxide solution, permanganate solution are mixed and is added, stirring reaction 2 hours at being 90 DEG C in temperature
Slurry is made, the cobaltⅡ content into solution stops reaction, the mol ratio of the cobalt, lithium and permanganate of addition less than 0.5g/l
It is 1:5:1.25；
（3）Nickel manganese solution is mixed with lithium hydroxide solution, stirring reaction is made slurry in 1.5 hours at being 80 DEG C in temperature, plus
The mol ratio of the nickel, manganese and the lithium that enter is 1:0.33:5；
（4）By step（2）And step（3）Slurry mixing, stirring and emulsifying 2 hours, then will emulsification material be put into autoclave, so
Reacted 12 hours at 180 DEG C afterwards, the mol ratio of nickel, cobalt, manganese, lithium and permanganate is 1 in slurry:0.33:0.33：6:0.42；
（5）Reaction under high pressure finish after filtering, washing, drying after, material is put into carries out high temperature sintering in sintering furnace, at 1050 DEG C
Sintering 12 hours, then by broken, batch mixing, screening, except iron obtains nickel-cobalt lithium manganate cathode material.
Further, cobalt salt is cobalt acetate in described step 1, and permanganate is violent acid sodium high, and nickel salt is nickel chloride, manganese
Salt is manganese chloride.
Further, speed of agitator is 400r/min in described step 2 and step 3.
Further, stirring and emulsifying temperature is 65 DEG C in described step 4, and the speed of agitator of emulsification is 850r/min,
Reaction pressure in autoclave is 0.25mpa, and speed of agitator is 400r/min.
Further, washings pH is washed at 8.1 and terminated in washing process in described step 5, and drying to moisture contains
Amount is less than 1wt%, and oxygen or compressed air are passed through in sintering process so that the atmosphere in sintering furnace is oxidizing atmosphere, oxic gas
Concentration >=the 10%vol of oxygen in atmosphere, sieve for 225 mesh sieves.
The final positive electrode pH for preparing is 8.4, and in 2.5-4.2V, charging capacity is up to 165.5mAh/g, discharge capacity
Up to 163.1mAh/g.
The content of cobalt nickel manganese is respectively 2.8mg/l, 9.1mg/l and 1.4mg/l, the utilization rate of nickel cobalt manganese in the waste water of generation
Reach more than 99.5%.
Example IV
A kind of preparation method of new energy battery nickel-cobalt lithium manganate cathode material, it is characterised in that comprise the following steps：
（1）Cobalt salt crystal is configured to the cobalt liquor that concentration is 1.2mol/l, lithium hydroxide is configured to concentration for 5.5mol/l
Lithium hydroxide solution, by permanganate be configured to concentration be 1.4mol/l permanganate solution, by nickel salt crystal and manganese salt
Crystal is hybridly prepared into the nickel manganese solution that concentration is 1mol/l；
（2）Cobalt liquor, lithium hydroxide solution, permanganate solution are mixed and is added, stirring reaction 2 hours at being 90 DEG C in temperature
Slurry is made, the cobaltⅡ content into solution stops reaction, the mol ratio of the cobalt, lithium and permanganate of addition less than 0.5g/l
It is 1:5:1.4；
（3）Nickel manganese solution is mixed with lithium hydroxide solution, stirring reaction is made slurry in 1.5 hours at being 80 DEG C in temperature, plus
The mol ratio of the nickel, manganese and the lithium that enter is 1:0.33:5；
（4）By step（2）And step（3）Slurry mixing, stirring and emulsifying 2 hours, then will emulsification material be put into autoclave, so
Reacted 12 hours at 180 DEG C afterwards, the mol ratio of nickel, cobalt, manganese, lithium and permanganate is 1 in slurry:0.5:1：5:0.7；
（5）Reaction under high pressure finish after filtering, washing, drying after, material is put into carries out high temperature sintering in sintering furnace, at 1150 DEG C
Sintering 14 hours, then by broken, batch mixing, screening, except iron obtains nickel-cobalt lithium manganate cathode material.
Further, cobalt salt is cobalt chloride in described step 1, and permanganate is violent acid sodium high, and nickel salt is nickel chloride, manganese
Salt is manganese chloride.
Further, speed of agitator is 400r/min in described step 2 and step 3.
Further, stirring and emulsifying temperature is 65 DEG C in described step 4, and the speed of agitator of emulsification is 950r/min,
Reaction pressure in autoclave is 0.21mpa, and speed of agitator is 350r/min.
Further, washings pH is washed at 8.2 and terminated in washing process in described step 5, and drying to moisture contains
Amount is less than 1wt%, and oxygen or compressed air are passed through in sintering process so that the atmosphere in sintering furnace is oxidizing atmosphere, oxic gas
Concentration >=the 10%vol of oxygen in atmosphere, sieve for 325 mesh sieves.
The final positive electrode pH for preparing is 8.7, and in 2.5-4.2V, charging capacity is up to 169.5mAh/g, discharge capacity
Up to 163.8mAh/g.
The content of cobalt nickel manganese is respectively 3.1mg/l, 9.2mg/l and 1.3mg/l, the utilization rate of nickel cobalt manganese in the waste water of generation
Reach more than 99.5%.
The present invention is not limited to above-mentioned preferred forms, and anyone can show that other are various under enlightenment of the invention
The product of form, however, make any change in its shape or structure, it is every with skill identical or similar to the present application
Art scheme, is within the scope of the present invention.
Claims (5)
1. a kind of preparation method of new energy battery nickel-cobalt lithium manganate cathode material, it is characterised in that comprise the following steps：
Cobalt salt crystal is configured to the cobalt liquor that concentration is 0.5-2mol/l, it is 4-8mol/l's that lithium hydroxide is configured into concentration
Lithium hydroxide solution, is configured to the permanganate solution that concentration is 0.5-2mol/l, by nickel salt crystal and manganese salt by permanganate
Crystal is hybridly prepared into the nickel manganese solution that concentration is 0.5-2mol/l；
Cobalt liquor, lithium hydroxide solution, permanganate solution are mixed and is added, stirring reaction 0.5- at being 20-100 DEG C in temperature
It is made slurry within 5 hours, the cobaltⅡ content into solution stops reaction less than 0.5g/l, the cobalt of addition, lithium and permanganate
Mol ratio is 1:3-6:0.5-1.5；
Nickel manganese solution is mixed with lithium hydroxide solution, slurry is made within stirring reaction 0.2-2 hours at being 20-100 DEG C in temperature,
The mol ratio of the nickel, manganese and lithium of addition is 1:0.125-1:4-12；
By step（2）And step（3）Slurry mixing, stirring and emulsifying 0.5-3 hour, then will emulsify material be put into autoclave,
Then reacted 5-15 hours at 150-300 DEG C, the mol ratio of nickel, cobalt, manganese, lithium and permanganate is 1 in slurry:0.125-1:
0.125-1：4-12:0.06-1.5；
Reaction under high pressure finish after filtering, washing, drying after, material is put into carries out high temperature sintering in sintering furnace, in 800-1200
DEG C sintering 8-16 hour, then by crushing, batch mixing, screening, obtain nickel-cobalt lithium manganate cathode material except iron.
2. a kind of preparation method of new energy battery nickel-cobalt lithium manganate cathode material according to claim 1, its feature
It is that cobalt salt is at least one in cobaltous sulfate, cobalt nitrate, cobalt acetate, cobalt chloride in described step 1, permanganate is height
At least one in potassium manganate, acid sodium high violent, permanganic acid, nickel salt be in nickel sulfate, nickel nitrate, nickel acetate, nickel chloride at least
One kind, manganese salt is at least one in manganese sulfate, manganese nitrate, manganese acetate, manganese chloride.
3. a kind of preparation method of new energy battery nickel-cobalt lithium manganate cathode material according to claim 1, its feature
It is that speed of agitator is 50-500r/min in described step 2 and step 3.
4. a kind of preparation method of new energy battery nickel-cobalt lithium manganate cathode material according to claim 1, its feature
It is that stirring and emulsifying temperature is 10-80 DEG C in described step 4, the speed of agitator of emulsification is 500-1200r/min, in high pressure
Reaction pressure in kettle is 0.1-0.5mpa, and speed of agitator is 50-500r/min.
5. a kind of preparation method of new energy battery nickel-cobalt lithium manganate cathode material according to claim 1, its feature
It is that washings pH is washed in 7-9 and terminated in washing process in described step 5, drying to moisture is less than 1wt%, burns
Oxygen or compressed air are passed through during knot so that the atmosphere in sintering furnace is oxidizing atmosphere, the concentration of oxygen in oxidizing atmosphere
>=10%vol, sieve for 200-400 mesh sieves.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109585812A (en) * | 2018-11-13 | 2019-04-05 | 广东邦普循环科技有限公司 | A kind of lithium cobalt positive polar material and its preparation method and application |
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