CN109994730A - A kind of preparation method of stratiform lithium cobaltate cathode material - Google Patents
A kind of preparation method of stratiform lithium cobaltate cathode material Download PDFInfo
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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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 stratiform lithium cobaltate cathode material, this method are as follows: firstly, reaction kettle is added in deionized water, ammonium hydroxide and liquid alkaline, prepares bottom liquid；Then reaction kettle is added in cobalt chloride, lithium chloride, ammonium hydroxide and liquid alkaline, adjusts charging rate to control reaction, reaches certain value to the solid content in reaction kettle, stop charging, obtain reacting slurry；Finally, reacting slurry ageing, centrifuge washing and drying are obtained stratiform lithium cobaltate cathode material；The present invention directly obtains stratiform lithium cobaltate cathode material by liquid phase synthesis, which is conducive to the deintercalation of lithium ion due to special layer structure, to improve the specific capacity of material, high rate performance and cycle performance；The direct step liquid phase synthesis of the preparation method obtains stratiform lithium cobaltate cathode material, greatly shortens synthesis step, will substantially reduce combined coefficient, synthesis cost, the investment of equipment needed for reducing high temperature.
Description
Technical field
The invention belongs to technical field of lithium ion battery positive pole material preparation, and in particular to a kind of stratiform lithium cobaltate cathode material
The preparation method of material.
Background technique
Energy density is high, power density is big, good cycle, memory-less effect, green ring due to having for lithium ion battery
The features such as guarantor, mobile communication equipment such as mobile phone, mobile camera, laptop, in mobile phone various electronic products
Be used widely, at the same be also the following electric car energy supplying system in strong candidate.
In the prior art, cobalt acid lithium is due to realizing at first with the advantages such as simple production process and stable electrochemical property
Commercialization has many advantages, such as that discharge voltage is high, charging/discharging voltage is steady, specific energy is high, has in small consumer field of batteries
There is important application；But it is typically chosen spherical oxidation cobalt precursor at present as raw material, lithium calcining is mixed, cobalt acid lithium is obtained, this
Kind preparation method needs high-temperature calcination, and energy consumption is high, and at high cost, the production time is long.
Summary of the invention
For overcome the deficiencies in the prior art, the purpose of the present invention is intended to provide a kind of system of stratiform lithium cobaltate cathode material
Preparation Method.
The present invention provides a kind of preparation method of stratiform lithium cobaltate cathode material, and method is implemented by following steps:
Step 1, reaction kettle is added in deionized water, ammonium hydroxide and liquid alkaline, is then passed through oxygen to reaction kettle and stirs, obtains
Obtain bottom liquid；
Step 2, reaction kettle is added in prepared cobalt chloride and lithium chloride, while ammonium hydroxide and liquid is added into reaction kettle
Alkali adjusts the charging rate of cobalt chloride and lithium chloride to control reaction, reaches 100~300g/L to the solid content in reaction kettle,
Stop charging, obtains reacting slurry；
Step 3, the reacting slurry that the step 2 obtains is aged, is then centrifuged for washing, finally dries, obtain layer
Shape lithium cobaltate cathode material.
In above scheme, the additional amount of deionized water is 3~4m in the step 13。
In above scheme, the flow that oxygen is passed through in the step 1 is 1~3m3/h。。
In above scheme, mixing speed is 150~350rpm in the step 1, and mixing time is 2~10h.
In above scheme, the content of the ammonium hydroxide in deionized water in the step 1 and step 2 remains 1~5g/L.
In above scheme, the pH value in the reaction process of the step 1 and step 2 remains 8~11.
In above scheme, the concentration of cobalt chloride is 80~120g/L in the step 2, and the charging rate of the cobalt chloride is
20~100L/h.
In above scheme, the concentration of lithium chloride is 80~120g/L in the step 2, and the charging rate of the lithium chloride is
20~100L/h.
In above scheme, digestion time is 1~10h in the step 3.
In above scheme, wash temperature is 50~80 DEG C in the step 3, and drying temperature is 100~150 DEG C.
Compared with prior art, the invention proposes a kind of preparation method of stratiform lithium cobaltate cathode material, this method are as follows:
Firstly, reaction kettle is added in deionized water, ammonium hydroxide and liquid alkaline, bottom liquid is prepared；Then by cobalt chloride, lithium chloride, ammonium hydroxide and liquid
Reaction kettle is added in alkali, adjusts charging rate to control reaction, reaches certain value to the solid content in reaction kettle, stop charging, obtain
Obtain reacting slurry；Finally, reacting slurry ageing, centrifuge washing and drying are obtained stratiform lithium cobaltate cathode material；The present invention is logical
It crosses liquid phase synthesis and directly obtains stratiform lithium cobaltate cathode material, which is conducive to lithium ion due to special layer structure
Deintercalation, to improve the specific capacity of material, high rate performance and cycle performance；The direct step liquid phase synthesis of the preparation method obtains
Stratiform lithium cobaltate cathode material, greatly shortens synthesis step, will substantially reduce combined coefficient, synthesis cost, reduces high temperature
The investment of required equipment.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The embodiment of the present invention provides a kind of preparation method of stratiform lithium cobaltate cathode material, and method passes through following steps reality
It applies:
Step 1,3~4m is weighed3Deionized water is added in reaction kettle, and ammonium hydroxide and liquid alkaline are then added into reaction kettle,
Simultaneously with 1~3m3The speed of/h is passed through oxygen to reaction kettle, stirs 2~10h under oxygen atmosphere with 150~350rpm speed,
Obtain bottom liquid；
Wherein, in reaction process by adjusting the additional amount of ammonium hydroxide and liquid alkaline control ammonium hydroxide content be 1~5g/L and
The pH value of bottom liquid is 8~11；
Wherein, liquid alkaline is sodium hydroxide solution；
Step 2, by the cobalt chloride of prepared 80~120g/L and 80~120g/L lithium chloride, 20~100L/h is pressed respectively
Charging rate and the charging rate of 20~100L/h reaction kettle is added, while ammonium hydroxide and liquid alkaline being added into reaction kettle, reaction
The content by adjusting the additional amount of ammonium hydroxide and liquid alkaline control ammonium hydroxide is 1~5g/L in the process and the pH value of bottom liquid is 8~11,
Reach 100~300g/L to the solid content in reaction kettle, stops that charging is added, obtain reacting slurry；
The present invention controls the progress of reaction, the too big meeting of charging rate by the charging rate of control cobalt chloride and lithium chloride
Cause solution local concentration excessively high, cause to react unstable, little particle can be generated, solid content mainly has shadow to the speed that rises of particle
It rings, solid content is higher, and grain diameter rises fast slower.
Step 3, the reacting slurry step 2 obtained carries out 1~10h of ageing, is then centrifuged and washes at 50~80 DEG C
It washs, is finally dried at 100~150 DEG C, obtain stratiform lithium cobaltate cathode material.
The present invention directly obtains stratiform lithium cobaltate cathode material by liquid phase synthesis, and the material is due to special stratiform knot
Structure, is conducive to the deintercalation of lithium ion, to improve the specific capacity of material, high rate performance and cycle performance；The preparation method is straight
Connect a step liquid phase synthesis and obtain stratiform lithium cobaltate cathode material, greatly shorten synthesis step, will substantially reduce combined coefficient,
Synthesis cost, the investment of equipment needed for reducing high temperature.
Embodiment 1
The embodiment of the present invention 1 also provides a kind of preparation method of the preparation method of stratiform lithium cobaltate cathode material, method
Implemented by following steps:
Step 1,3m is weighed3Deionized water is added in reaction kettle, ammonium hydroxide and liquid alkaline is then added into reaction kettle, simultaneously
With 1.5m3The speed of/h is passed through oxygen to reaction kettle, stirs 6h under oxygen atmosphere with 200rpm speed, obtains bottom liquid；
It wherein, is 2.5g/L and bottom by adjusting the content of the additional amount of ammonium hydroxide and liquid alkaline control ammonium hydroxide in reaction process
The pH value of liquid is 9.2；
Wherein, liquid alkaline is sodium hydroxide solution；
Step 2, by the lithium chloride of the cobalt chloride of prepared 100g/L and 100g/L, the charging rate of 80L/h is pressed respectively
Reaction kettle is added with the charging rate of 80L/h, while ammonium hydroxide and liquid alkaline being added into reaction kettle, by adjusting ammonia in reaction process
The content of the additional amount of water and liquid alkaline control ammonium hydroxide is 2.5g/L and the pH value of bottom liquid is 9.2, to the solid content in reaction kettle
Reach 200g/L, stops that charging is added, obtain reacting slurry；
Step 3, the reacting slurry step 2 obtained carries out ageing 5h, then the centrifuge washing at 50~80 DEG C, most
It is dried at 100~150 DEG C afterwards, obtains stratiform lithium cobaltate cathode material.
The stratiform lithium cobaltate cathode material obtained using above-described embodiment is as anode, and metal lithium sheet is as cathode, assembly
Button cell；Using traditional lithium cobaltate cathode material as anode, metal lithium sheet assembles button cell, as right as cathode
According to group；It will carry out above-described embodiment and control group and carry out charge-discharge test, control group test result is, under 0.5C multiplying power for the first time
Specific discharge capacity reaches 160mAh/g；Capacity retention ratio is reduced to 95.3% after 100 charge-discharge cycles, and under 2C multiplying power, discharge ratio
Capacity is only 138.2mAh/g；The test result of above-described embodiment is that first discharge specific capacity reaches under 0.5C multiplying power
168.4mAh/g；Capacity retention ratio is up to 97.1% after 100 charge-discharge cycles；Under 2C multiplying power, specific discharge capacity reaches
145.4mAh/g。
Embodiment 2
The embodiment of the present invention 2 also provides a kind of preparation method of the preparation method of stratiform lithium cobaltate cathode material, method
Implemented by following steps:
Step 1,3m is weighed3Deionized water is added in reaction kettle, ammonium hydroxide and liquid alkaline is then added into reaction kettle, simultaneously
With 1.5m3The speed of/h is passed through oxygen to reaction kettle, stirs 6h under oxygen atmosphere with 200rpm speed, obtains bottom liquid；
It wherein, is 3g/L and bottom liquid by adjusting the content of the additional amount of ammonium hydroxide and liquid alkaline control ammonium hydroxide in reaction process
PH value be 9.4；
Wherein, liquid alkaline is sodium hydroxide solution；
Step 2, by the lithium chloride of the cobalt chloride of prepared 80g/L and 100g/L, respectively by 20L/h charging rate and
Reaction kettle is added in the charging rate of 80L/h, while ammonium hydroxide and liquid alkaline being added into reaction kettle, by adjusting ammonium hydroxide in reaction process
Content with the additional amount control ammonium hydroxide of liquid alkaline is 3g/L and the pH value of bottom liquid is 9.4, is reached to the solid content in reaction kettle
200g/L stops that charging is added, obtains reacting slurry；
Step 3, the reacting slurry step 2 obtained carries out ageing 5h, then the centrifuge washing at 50~80 DEG C, most
It is dried at 100~150 DEG C afterwards, obtains stratiform lithium cobaltate cathode material.
The stratiform lithium cobaltate cathode material obtained using above-described embodiment is as anode, and metal lithium sheet is as cathode, assembly
Button cell；Using traditional lithium cobaltate cathode material as anode, metal lithium sheet assembles button cell, as right as cathode
According to group；It will carry out above-described embodiment and control group and carry out charge-discharge test, control group test result is, under 0.5C multiplying power for the first time
Specific discharge capacity reaches 160mAh/g；Capacity retention ratio is reduced to 95.3% after 100 charge-discharge cycles, and under 2C multiplying power, discharge ratio
Capacity is only 138.2mAh/g；The test result of above-described embodiment is that first discharge specific capacity reaches under 0.5C multiplying power
168.5mAh/g；Capacity retention ratio is up to 97.2% after 100 charge-discharge cycles；Under 2C multiplying power, specific discharge capacity reaches
145.3mAh/g。
Embodiment 3
The embodiment of the present invention 3 also provides a kind of preparation method of the preparation method of stratiform lithium cobaltate cathode material, method
Implemented by following steps:
Step 1,3m is weighed3Deionized water is added in reaction kettle, ammonium hydroxide and liquid alkaline is then added into reaction kettle, simultaneously
With 1.5m3The speed of/h is passed through oxygen to reaction kettle, stirs 6h under oxygen atmosphere with 200rpm speed, obtains bottom liquid；
It wherein, is 1.5g/L and bottom by adjusting the content of the additional amount of ammonium hydroxide and liquid alkaline control ammonium hydroxide in reaction process
The pH value of liquid is 9；
Wherein, liquid alkaline is sodium hydroxide solution；
Step 2, by the lithium chloride of the cobalt chloride of prepared 120g/L and 100g/L, the charging rate of 100L/h is pressed respectively
Reaction kettle is added with the charging rate of 80L/h, while ammonium hydroxide and liquid alkaline being added into reaction kettle, by adjusting ammonia in reaction process
The content of the additional amount of water and liquid alkaline control ammonium hydroxide is 1.5g/L and the pH value of bottom liquid is 9, is reached to the solid content in reaction kettle
To 200g/L, stops that charging is added, obtain reacting slurry；
Step 3, the reacting slurry step 2 obtained carries out ageing 5h, then the centrifuge washing at 50~80 DEG C, most
It is dried at 100~150 DEG C afterwards, obtains stratiform lithium cobaltate cathode material.
The stratiform lithium cobaltate cathode material obtained using above-described embodiment is as anode, and metal lithium sheet is as cathode, assembly
Button cell；Using traditional lithium cobaltate cathode material as anode, metal lithium sheet assembles button cell, as right as cathode
According to group；It will carry out above-described embodiment and control group and carry out charge-discharge test, control group test result is, under 0.5C multiplying power for the first time
Specific discharge capacity reaches 160mAh/g；Capacity retention ratio is reduced to 95.3% after 100 charge-discharge cycles, and under 2C multiplying power, discharge ratio
Capacity is only 138.2mAh/g；The test result of above-described embodiment is that first discharge specific capacity reaches under 0.5C multiplying power
167.4mAh/g；Capacity retention ratio is up to 97.1% after 100 charge-discharge cycles；Under 2C multiplying power, specific discharge capacity reaches
144.1mAh/g。
Embodiment 4
The embodiment of the present invention 4 also provides a kind of preparation method of the preparation method of stratiform lithium cobaltate cathode material, method
Implemented by following steps:
Step 1,4m is weighed3Deionized water is added in reaction kettle, ammonium hydroxide and liquid alkaline is then added into reaction kettle, simultaneously
With 1.5m3The speed of/h is passed through oxygen to reaction kettle, stirs 6h under oxygen atmosphere with 200rpm speed, obtains bottom liquid；
It wherein, is 3g/L and bottom liquid by adjusting the content of the additional amount of ammonium hydroxide and liquid alkaline control ammonium hydroxide in reaction process
PH value be 9.6；
Wherein, liquid alkaline is sodium hydroxide solution；
Step 2, by the lithium chloride of the cobalt chloride of prepared 100g/L and 100g/L, the charging rate of 80L/h is pressed respectively
Reaction kettle is added with the charging rate of 80L/h, while ammonium hydroxide and liquid alkaline being added into reaction kettle, by adjusting ammonia in reaction process
The content of the additional amount of water and liquid alkaline control ammonium hydroxide is 3g/L and the pH value of bottom liquid is 9.6, is reached to the solid content in reaction kettle
To 200g/L, stops that charging is added, obtain reacting slurry；
Step 3, the reacting slurry step 2 obtained carries out ageing 5h, then the centrifuge washing at 50~80 DEG C, most
It is dried at 100~150 DEG C afterwards, obtains stratiform lithium cobaltate cathode material.
The stratiform lithium cobaltate cathode material obtained using above-described embodiment is as anode, and metal lithium sheet is as cathode, assembly
Button cell；Using traditional lithium cobaltate cathode material as anode, metal lithium sheet assembles button cell, as right as cathode
According to group；It will carry out above-described embodiment and control group and carry out charge-discharge test, control group test result is, under 0.5C multiplying power for the first time
Specific discharge capacity reaches 160mAh/g；Capacity retention ratio is reduced to 95.3% after 100 charge-discharge cycles, and under 2C multiplying power, discharge ratio
Capacity is only 138.2mAh/g；The test result of above-described embodiment is that first discharge specific capacity reaches under 0.5C multiplying power
170.2mAh/g；Capacity retention ratio is up to 96.9% after 100 charge-discharge cycles；Under 2C multiplying power, specific discharge capacity reaches
146.8mAh/g。
Embodiment 5
The embodiment of the present invention 5 also provides a kind of preparation method of the preparation method of stratiform lithium cobaltate cathode material, method
Implemented by following steps:
Step 1,4m is weighed3Deionized water is added in reaction kettle, ammonium hydroxide and liquid alkaline is then added into reaction kettle, simultaneously
With 1.5m3The speed of/h is passed through oxygen to reaction kettle, stirs 6h under oxygen atmosphere with 200rpm speed, obtains bottom liquid；
It wherein, is 4.5g/L and bottom by adjusting the content of the additional amount of ammonium hydroxide and liquid alkaline control ammonium hydroxide in reaction process
The pH value of liquid is 9.9；
Wherein, liquid alkaline is sodium hydroxide solution；
Step 2, by the lithium chloride of the cobalt chloride of prepared 100g/L and 80g/L, respectively by 80L/h charging rate and
Reaction kettle is added in the charging rate of 20L/h, while ammonium hydroxide and liquid alkaline being added into reaction kettle, by adjusting ammonium hydroxide in reaction process
Content with the additional amount control ammonium hydroxide of liquid alkaline is 4.5g/L and the pH value of bottom liquid is 9.9, is reached to the solid content in reaction kettle
To 200g/L, stops that charging is added, obtain reacting slurry；
Step 3, the reacting slurry step 2 obtained carries out ageing 5h, then the centrifuge washing at 50~80 DEG C, most
It is dried at 100~150 DEG C afterwards, obtains stratiform lithium cobaltate cathode material.
The stratiform lithium cobaltate cathode material obtained using above-described embodiment is as anode, and metal lithium sheet is as cathode, assembly
Button cell；Using traditional lithium cobaltate cathode material as anode, metal lithium sheet assembles button cell, as right as cathode
According to group；It will carry out above-described embodiment and control group and carry out charge-discharge test, control group test result is, under 0.5C multiplying power for the first time
Specific discharge capacity reaches 160mAh/g；Capacity retention ratio is reduced to 95.3% after 100 charge-discharge cycles, and under 2C multiplying power, discharge ratio
Capacity is only 138.2mAh/g；The test result of above-described embodiment is that first discharge specific capacity reaches under 0.5C multiplying power
169.7mAh/g；Capacity retention ratio is up to 97.4% after 100 charge-discharge cycles；Under 2C multiplying power, specific discharge capacity reaches
146.2mAh/g。
Embodiment 6
The embodiment of the present invention 6 also provides a kind of preparation method of the preparation method of stratiform lithium cobaltate cathode material, method
Implemented by following steps:
Step 1,4m is weighed3Deionized water is added in reaction kettle, ammonium hydroxide and liquid alkaline is then added into reaction kettle, simultaneously
With 1.5m3The speed of/h is passed through oxygen to reaction kettle, stirs 6h under oxygen atmosphere with 200rpm speed, obtains bottom liquid；
It wherein, is 1.5g/L and bottom by adjusting the content of the additional amount of ammonium hydroxide and liquid alkaline control ammonium hydroxide in reaction process
The pH value of liquid is 9.2；
Wherein, liquid alkaline is sodium hydroxide solution；
Step 2, by the lithium chloride of the cobalt chloride of prepared 100g/L and 120g/L, the charging rate of 80L/h is pressed respectively
Reaction kettle is added with the charging rate of 100L/h, while ammonium hydroxide and liquid alkaline being added into reaction kettle, in reaction process by adjusting
The content of the additional amount of ammonium hydroxide and liquid alkaline control ammonium hydroxide is 1.5g/L and the pH value of bottom liquid is 9.2, is contained to consolidating in reaction kettle
Amount reaches 200g/L, stops that charging is added, obtains reacting slurry；
Step 3, the reacting slurry step 2 obtained carries out ageing 5h, then the centrifuge washing at 50~80 DEG C, most
It is dried at 100~150 DEG C afterwards, obtains stratiform lithium cobaltate cathode material.
The stratiform lithium cobaltate cathode material obtained using above-described embodiment is as anode, and metal lithium sheet is as cathode, assembly
Button cell；Using traditional lithium cobaltate cathode material as anode, metal lithium sheet assembles button cell, as right as cathode
According to group；It will carry out above-described embodiment and control group and carry out charge-discharge test, control group test result is, under 0.5C multiplying power for the first time
Specific discharge capacity reaches 160mAh/g；Capacity retention ratio is reduced to 95.3% after 100 charge-discharge cycles, and under 2C multiplying power, discharge ratio
Capacity is only 138.2mAh/g；The test result of above-described embodiment is that first discharge specific capacity reaches under 0.5C multiplying power
167.8mAh/g；Capacity retention ratio is up to 97.2% after 100 charge-discharge cycles；Under 2C multiplying power, specific discharge capacity reaches
144.7mAh/g。
Embodiment 7
The embodiment of the present invention 7 also provides a kind of preparation method of the preparation method of stratiform lithium cobaltate cathode material, method
Implemented by following steps:
Step 1,3.5m is weighed3Deionized water is added in reaction kettle, ammonium hydroxide and liquid alkaline is then added into reaction kettle, together
When with 1m3The speed of/h is passed through oxygen to reaction kettle, stirs 2h under oxygen atmosphere with 150rpm speed, obtains bottom liquid；
It wherein, is 3.2g/L and bottom by adjusting the content of the additional amount of ammonium hydroxide and liquid alkaline control ammonium hydroxide in reaction process
The pH value of liquid is 8.5；
Wherein, liquid alkaline is sodium hydroxide solution；
Step 2, by the lithium chloride of the cobalt chloride of prepared 100g/L and 100g/L, the charging rate of 80L/h is pressed respectively
Reaction kettle is added with the charging rate of 80L/h, while ammonium hydroxide and liquid alkaline being added into reaction kettle, by adjusting ammonia in reaction process
The content of the additional amount of water and liquid alkaline control ammonium hydroxide is 3.2g/L and the pH value of bottom liquid is 8.5, to the solid content in reaction kettle
Reach 200g/L, stops that charging is added, obtain reacting slurry；
Step 3, the reacting slurry step 2 obtained carries out ageing 5h, then the centrifuge washing at 50~80 DEG C, most
It is dried at 100~150 DEG C afterwards, obtains stratiform lithium cobaltate cathode material.
The stratiform lithium cobaltate cathode material obtained using above-described embodiment is as anode, and metal lithium sheet is as cathode, assembly
Button cell；Using traditional lithium cobaltate cathode material as anode, metal lithium sheet assembles button cell, as right as cathode
According to group；It will carry out above-described embodiment and control group and carry out charge-discharge test, control group test result is, under 0.5C multiplying power for the first time
Specific discharge capacity reaches 160mAh/g；Capacity retention ratio is reduced to 95.3% after 100 charge-discharge cycles, and under 2C multiplying power, discharge ratio
Capacity is only 138.2mAh/g；The test result of above-described embodiment is that first discharge specific capacity reaches under 0.5C multiplying power
169.4mAh/g；Capacity retention ratio is up to 96.8% after 100 charge-discharge cycles；Under 2C multiplying power, specific discharge capacity reaches
144.7mAh/g。
Embodiment 8
The embodiment of the present invention 8 also provides a kind of preparation method of the preparation method of stratiform lithium cobaltate cathode material, method
Implemented by following steps:
Step 1,3.5m is weighed3Deionized water is added in reaction kettle, ammonium hydroxide and liquid alkaline is then added into reaction kettle, together
When with 2m3The speed of/h is passed through oxygen to reaction kettle, stirs 6h under oxygen atmosphere with 250rpm speed, obtains bottom liquid；
It wherein, is 2.8g/L and bottom by adjusting the content of the additional amount of ammonium hydroxide and liquid alkaline control ammonium hydroxide in reaction process
The pH value of liquid is 9.2；
Wherein, liquid alkaline is sodium hydroxide solution；
Step 2, by the lithium chloride of the cobalt chloride of prepared 100g/L and 100g/L, the charging rate of 80L/h is pressed respectively
Reaction kettle is added with the charging rate of 80L/h, while ammonium hydroxide and liquid alkaline being added into reaction kettle, by adjusting ammonia in reaction process
The content of the additional amount of water and liquid alkaline control ammonium hydroxide is 2.8g/L and the pH value of bottom liquid is 9.2, to the solid content in reaction kettle
Reach 200g/L, stops that charging is added, obtain reacting slurry；
Step 3, the reacting slurry step 2 obtained carries out ageing 5h, then the centrifuge washing at 50~80 DEG C, most
It is dried at 100~150 DEG C afterwards, obtains stratiform lithium cobaltate cathode material.
The stratiform lithium cobaltate cathode material obtained using above-described embodiment is as anode, and metal lithium sheet is as cathode, assembly
Button cell；Using traditional lithium cobaltate cathode material as anode, metal lithium sheet assembles button cell, as right as cathode
According to group；It will carry out above-described embodiment and control group and carry out charge-discharge test, control group test result is, under 0.5C multiplying power for the first time
Specific discharge capacity reaches 160mAh/g；Capacity retention ratio is reduced to 95.3% after 100 charge-discharge cycles, and under 2C multiplying power, discharge ratio
Capacity is only 138.2mAh/g；The test result of above-described embodiment is that first discharge specific capacity reaches under 0.5C multiplying power
169.4mAh/g；Capacity retention ratio is up to 97.0% after 100 charge-discharge cycles；Under 2C multiplying power, specific discharge capacity reaches
145.7mAh/g。
Embodiment 9
The embodiment of the present invention 9 also provides a kind of preparation method of the preparation method of stratiform lithium cobaltate cathode material, method
Implemented by following steps:
Step 1,3.5m is weighed3Deionized water is added in reaction kettle, ammonium hydroxide and liquid alkaline is then added into reaction kettle, together
When with 3m3The speed of/h is passed through oxygen to reaction kettle, stirs 10h under oxygen atmosphere with 350rpm speed, obtains bottom liquid；
It wherein, is 5g/L and bottom liquid by adjusting the content of the additional amount of ammonium hydroxide and liquid alkaline control ammonium hydroxide in reaction process
PH value be 11；
Wherein, liquid alkaline is sodium hydroxide solution；
Step 2, by the lithium chloride of the cobalt chloride of prepared 100g/L and 100g/L, the charging rate of 80L/h is pressed respectively
Reaction kettle is added with the charging rate of 80L/h, while ammonium hydroxide and liquid alkaline being added into reaction kettle, by adjusting ammonia in reaction process
The content of the additional amount of water and liquid alkaline control ammonium hydroxide is 5g/L and the pH value of bottom liquid is 11, is reached to the solid content in reaction kettle
200g/L stops that charging is added, obtains reacting slurry；
Step 3, the reacting slurry step 2 obtained carries out ageing 5h, then the centrifuge washing at 50~80 DEG C, most
It is dried at 100~150 DEG C afterwards, obtains stratiform lithium cobaltate cathode material.
The stratiform lithium cobaltate cathode material obtained using above-described embodiment is as anode, and metal lithium sheet is as cathode, assembly
Button cell；Using traditional lithium cobaltate cathode material as anode, metal lithium sheet assembles button cell, as right as cathode
According to group；It will carry out above-described embodiment and control group and carry out charge-discharge test, control group test result is, under 0.5C multiplying power for the first time
Specific discharge capacity reaches 160mAh/g；Capacity retention ratio is reduced to 95.3% after 100 charge-discharge cycles, and under 2C multiplying power, discharge ratio
Capacity is only 138.2mAh/g；The test result of above-described embodiment is that first discharge specific capacity reaches under 0.5C multiplying power
167.5mAh/g；Capacity retention ratio is up to 97.4% after 100 charge-discharge cycles；Under 2C multiplying power, specific discharge capacity reaches
144.5mAh/g。
Embodiment 10
The embodiment of the present invention 10 also provides a kind of preparation method of the preparation method of stratiform lithium cobaltate cathode material, method
Implemented by following steps:
Step 1,3.5m is weighed3Deionized water is added in reaction kettle, ammonium hydroxide and liquid alkaline is then added into reaction kettle, together
When with 1.5m3The speed of/h is passed through oxygen to reaction kettle, stirs 6h under oxygen atmosphere with 200rpm speed, obtains bottom liquid；
It wherein, is 1.8g/L and bottom by adjusting the content of the additional amount of ammonium hydroxide and liquid alkaline control ammonium hydroxide in reaction process
The pH value of liquid is 8.9；
Wherein, liquid alkaline is sodium hydroxide solution；
Step 2, by the lithium chloride of the cobalt chloride of prepared 100g/L and 100g/L, the charging rate of 80L/h is pressed respectively
Reaction kettle is added with the charging rate of 80L/h, while ammonium hydroxide and liquid alkaline being added into reaction kettle, by adjusting ammonia in reaction process
The content of the additional amount of water and liquid alkaline control ammonium hydroxide is 1.8g/L and the pH value of bottom liquid is 8.9, to the solid content in reaction kettle
Reach 100g/L, stops that charging is added, obtain reacting slurry；
Step 3, the reacting slurry step 2 obtained carries out ageing 1h, then the centrifuge washing at 50~80 DEG C, most
It is dried at 100~150 DEG C afterwards, obtains stratiform lithium cobaltate cathode material.
The stratiform lithium cobaltate cathode material obtained using above-described embodiment is as anode, and metal lithium sheet is as cathode, assembly
Button cell；Using traditional lithium cobaltate cathode material as anode, metal lithium sheet assembles button cell, as right as cathode
According to group；It will carry out above-described embodiment and control group and carry out charge-discharge test, control group test result is, under 0.5C multiplying power for the first time
Specific discharge capacity reaches 160mAh/g；Capacity retention ratio is reduced to 95.3% after 100 charge-discharge cycles, and under 2C multiplying power, discharge ratio
Capacity is only 138.2mAh/g；The test result of above-described embodiment is that first discharge specific capacity reaches under 0.5C multiplying power
168.7mAh/g；Capacity retention ratio is up to 97.3% after 100 charge-discharge cycles；Under 2C multiplying power, specific discharge capacity reaches
145.5mAh/g。
Embodiment 11
The embodiment of the present invention 11 also provides a kind of preparation method of the preparation method of stratiform lithium cobaltate cathode material, method
Implemented by following steps:
Step 1,3.5m is weighed3Deionized water is added in reaction kettle, ammonium hydroxide and liquid alkaline is then added into reaction kettle, together
When with 1.5m3The speed of/h is passed through oxygen to reaction kettle, stirs 6h under oxygen atmosphere with 200rpm speed, obtains bottom liquid；
It wherein, is 2.5g/L and bottom by adjusting the content of the additional amount of ammonium hydroxide and liquid alkaline control ammonium hydroxide in reaction process
The pH value of liquid is 9.4；
Wherein, liquid alkaline is sodium hydroxide solution；
Step 2, by the lithium chloride of the cobalt chloride of prepared 100g/L and 100g/L, the charging rate of 80L/h is pressed respectively
Reaction kettle is added with the charging rate of 80L/h, while ammonium hydroxide and liquid alkaline being added into reaction kettle, by adjusting ammonia in reaction process
The content of the additional amount of water and liquid alkaline control ammonium hydroxide is 2.5g/L and the pH value of bottom liquid is 9.4, to the solid content in reaction kettle
Reach 200g/L, stops that charging is added, obtain reacting slurry；
Step 3, the reacting slurry step 2 obtained carries out ageing 7h, then the centrifuge washing at 50~80 DEG C, most
It is dried at 100~150 DEG C afterwards, obtains stratiform lithium cobaltate cathode material.
The stratiform lithium cobaltate cathode material obtained using above-described embodiment is as anode, and metal lithium sheet is as cathode, assembly
Button cell；Using traditional lithium cobaltate cathode material as anode, metal lithium sheet assembles button cell, as right as cathode
According to group；It will carry out above-described embodiment and control group and carry out charge-discharge test, control group test result is, under 0.5C multiplying power for the first time
Specific discharge capacity reaches 160mAh/g；Capacity retention ratio is reduced to 95.3% after 100 charge-discharge cycles, and under 2C multiplying power, discharge ratio
Capacity is only 138.2mAh/g；The test result of above-described embodiment is that first discharge specific capacity reaches under 0.5C multiplying power
168.5mAh/g；Capacity retention ratio is up to 97.2% after 100 charge-discharge cycles；Under 2C multiplying power, specific discharge capacity reaches
145.6mAh/g。
Embodiment 12
The embodiment of the present invention 12 also provides a kind of preparation method of the preparation method of stratiform lithium cobaltate cathode material, method
Implemented by following steps:
Step 1,3.5m is weighed3Deionized water is added in reaction kettle, ammonium hydroxide and liquid alkaline is then added into reaction kettle, together
When with 1.5m3The speed of/h is passed through oxygen to reaction kettle, stirs 6h under oxygen atmosphere with 200rpm speed, obtains bottom；
It wherein, is 2.5g/L and bottom by adjusting the content of the additional amount of ammonium hydroxide and liquid alkaline control ammonium hydroxide in reaction process
The pH value of liquid is 9.5；
Wherein, liquid alkaline is sodium hydroxide solution；
Step 2, by the lithium chloride of the cobalt chloride of prepared 100g/L and 100g/L, the charging rate of 80L/h is pressed respectively
Reaction kettle is added with the charging rate of 80L/h, while ammonium hydroxide and liquid alkaline being added into reaction kettle, by adjusting ammonia in reaction process
The content of the additional amount of water and liquid alkaline control ammonium hydroxide is 2.5g/L and the pH value of bottom liquid is 9.5, to the solid content in reaction kettle
Reach 300g/L, stops that charging is added, obtain reacting slurry；
Step 3, the reacting slurry step 2 obtained carries out ageing 10h, then the centrifuge washing at 50~80 DEG C,
It is finally dried at 100~150 DEG C, obtains stratiform lithium cobaltate cathode material.
The stratiform lithium cobaltate cathode material obtained using above-described embodiment is as anode, and metal lithium sheet is as cathode, assembly
Button cell；Using traditional lithium cobaltate cathode material as anode, metal lithium sheet assembles button cell, as right as cathode
According to group；It will carry out above-described embodiment and control group and carry out charge-discharge test, control group test result is, under 0.5C multiplying power for the first time
Specific discharge capacity reaches 160mAh/g；Capacity retention ratio is reduced to 95.3% after 100 charge-discharge cycles, and under 2C multiplying power, discharge ratio
Capacity is only 138.2mAh/g；The test result of above-described embodiment is that first discharge specific capacity reaches under 0.5C multiplying power
168.8mAh/g；Capacity retention ratio is up to 96.8% after 100 charge-discharge cycles；Under 2C multiplying power, specific discharge capacity reaches
145.9mAh/g。
The foregoing is only a preferred embodiment of the present invention, is not intended to limit the scope of the present invention.
Claims (10)
1. a kind of preparation method of stratiform lithium cobaltate cathode material, which is characterized in that its method is implemented by following steps:
Step 1, reaction kettle is added in deionized water, ammonium hydroxide and liquid alkaline, is then passed through oxygen to reaction kettle and stirs, obtain bottom
Liquid；
Step 2, reaction kettle is added in prepared cobalt chloride and lithium chloride, while ammonium hydroxide and liquid alkaline is added into reaction kettle, adjusted
The charging rate of whole cobalt chloride and lithium chloride with control reaction, reach 100~300g/L to the solid content in reaction kettle, stop into
Material obtains reacting slurry；
Step 3, the reacting slurry that the step 2 obtains is aged, is then centrifuged for washing, finally dries, obtain stratiform cobalt
Sour lithium anode material.
2. a kind of preparation method of stratiform lithium cobaltate cathode material according to claim 1, which is characterized in that the step
The additional amount of deionized water is 3~4m in 13。
3. a kind of preparation method of stratiform lithium cobaltate cathode material according to claim 2, which is characterized in that the step
The flow that oxygen is passed through in 1 is 1~3m3/h。
4. a kind of preparation method of stratiform lithium cobaltate cathode material according to claim 3, which is characterized in that the step
Mixing speed is 150~350rpm in 1, and mixing time is 2~10h.
5. a kind of preparation method of stratiform lithium cobaltate cathode material according to claim 4, which is characterized in that the step
1 and step 2 in deionized water in the content of ammonium hydroxide remain 1~5g/L.
6. a kind of preparation method of stratiform lithium cobaltate cathode material according to claim 5, which is characterized in that the step
1 and step 2 reaction process in pH value remain 8~11.
7. a kind of preparation method of stratiform lithium cobaltate cathode material, feature described in -6 any one exist according to claim 1
In the concentration of cobalt chloride is 80~120g/L in the step 2, and the charging rate of the cobalt chloride is 20~100L/h.
8. a kind of preparation method of stratiform lithium cobaltate cathode material according to claim 7, which is characterized in that the step
The concentration of lithium chloride is 80~120g/L in 2, and the charging rate of the lithium chloride is 20~100L/h.
9. a kind of preparation method of stratiform lithium cobaltate cathode material according to claim 8, which is characterized in that the step
Digestion time is 1~10h in 3.
10. a kind of preparation method of stratiform lithium cobaltate cathode material according to claim 9, which is characterized in that the step
Wash temperature is 50~80 DEG C in rapid 3, and drying temperature is 100~150 DEG C.
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