CN109888260A - A kind of modification method for preparing and modified material of lithium iron phosphate positive material - Google Patents
A kind of modification method for preparing and modified material of lithium iron phosphate positive material Download PDFInfo
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- CN109888260A CN109888260A CN201910281727.4A CN201910281727A CN109888260A CN 109888260 A CN109888260 A CN 109888260A CN 201910281727 A CN201910281727 A CN 201910281727A CN 109888260 A CN109888260 A CN 109888260A
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- iron phosphate
- lithium iron
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- phosphate positive
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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 invention discloses a kind of modification method for preparing of lithium iron phosphate positive material and modified material, firstly, by lithium iron phosphate positive material to be modified, carbon source and additive are added to the water uniformly mixed this programme；Then, mixing gained slurry is ground, and mist projection granulating is carried out to the slurry after grinding in such a way that air-stream spraying is dry；Finally, mist projection granulating resulting material is sintered, modified spherical lithium iron phosphate anode material is obtained after the completion of sintering.This preparation method simple process, low energy consumption；And it can guarantee material processing performance, promote chemical property.
Description
Technical field
The present invention relates to anode material of lithium battery preparation fields, specifically relate to the modified system of lithium iron phosphate positive material processing performance
Standby technology.
Background technique
Lithium iron phosphate positive material due to having many advantages, such as that nontoxic, environmentally friendly, specific capacity is high, the service life is long, at low cost,
It is widely used in the power supply of the equipment such as electric tool, electric bicycle, electric car, hybrid electric vehicle.
Currently, the production process route of the lithium iron phosphate positive material of mainstream is: water is added in lithium source, carbon source, ferric phosphate
In be uniformly mixed to nano particle, grain sintering, then the particle by being ground into specified particle diameter range are then reproduced, to obtain phosphorus
Sour iron lithium anode material.
However, the LiFePO4 finished-product material produced in this way has the disadvantage that:
(1) material granule is generally smaller, and D50 is in 1um or so.
(2) specific surface area of smashed material increases, and influences the dispersibility in material processing.
(3) crushing LiFePO4 may make LiFePO4 clad fall off, and cause it that cannot play electric action well,
To reduce the performance of the gram volume and high rate performance of material.
Summary of the invention
For the problems of existing production technology lithium iron phosphate positive material produced, need one kind that can improve
The scheme of lithium iron phosphate positive material processing performance.
For this purpose, the purpose of the present invention is to provide a kind of modification method for preparing of lithium iron phosphate positive material, it can be effective
Improve the gram volume and processing performance of lithium iron phosphate positive material；And a kind of modified phosphate iron lithium anode material is formed on this basis
Material.
In order to achieve the above object, the modification method for preparing of lithium iron phosphate positive material provided by the invention, comprising:
Firstly, lithium iron phosphate positive material to be modified, source and additive are added to the water uniformly mixed；
Then, to mixing gained slurry grind, and using air-stream spraying dry by the way of to the slurry after grinding into
Row mist projection granulating；
Finally, mist projection granulating resulting material is sintered, modified spherical lithium iron phosphate anode material is obtained after the completion of sintering.
Further, in parts by weight by lithium iron phosphate positive material 95~98 to be modified in the modification method for preparing
Part, 1~5 part of carbon source and 1~5 part of additive are added in the dispersing apparatus equipped with pure water 100-300 parts, are sufficiently mixed 2~8h, make
Carbon source and additive are coated on around lithium iron phosphate positive material particle to be modified.
It further, first will be after grinding when the modification method for preparing carries out mist projection granulating to the slurry after grinding
Slurry is atomized into droplet by nozzle and compressed air collision, drop using hot dry air it is dry after become micron order
Grain completes mist projection granulating.
Further, the slurry is sprayed with the total mass flow rate of 100-900kg/h from nozzle, the pressure of compressed air used
Power is 0.2-0.7MPa, and the temperature of hot dry air used is 200-300 DEG C.
Further, the granularity of the mist projection granulating resulting material reaches 5-10 μm.
Further, when the modification method for preparing is sintered mist projection granulating resulting material, sintering temperature 600-900
DEG C, the time is 6-24 hours.
Further, carbon source used is glucose, in polyvinyl alcohol, sucrose, soluble starch, cellulose, phenolic resin
It is one or more.
Further, additive therefor is one or more of carbon nanotube, graphene, SP.
In order to achieve the above object, modified phosphate iron lithium anode material provided by the invention, just by above-mentioned LiFePO4
The modification method for preparing of pole material prepares to be formed.
Further, it is coated with carbon-coating on the particle of the modified phosphate iron lithium anode material, and forms conductive network.
Preparation method provided by the present invention improves the granular size of lithium iron phosphate positive material, increases carbon again
Layer coats and forms conductive network, reduces specific surface area, keeps the spherical morphology of second particle, so that material be made to have more
Good electric conductivity and smaller specific surface area still have good processing performance even if making LiFePO4 under wet blending process,
With excellent multiplying power and cycle performance.
Furthermore this preparation method has the advantages that simple process, low energy consumption, and can improve the chemical property of material
(gram volume as improved material) and processing performance, can be good at overcoming the problems of prior art.
Detailed description of the invention
The present invention is further illustrated below in conjunction with the drawings and specific embodiments.
Fig. 1 is the LiFePO4 SEM figure that mist projection granulating sintering is modified in the present invention.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Conjunction is specifically illustrating, and the present invention is further explained.
It is formed by defect existing for lithium iron phosphate positive material for existing lithium iron phosphate positive material production technology, this
Scheme is directed to the finished product lithium iron phosphate positive electrode of these existing defects, gives a kind of for finished product lithium iron phosphate positive electrode
The processing modified preparation method of further progress can improve the chemical property of lithium iron phosphate positive material (as improved material
Gram volume) and processing performance.
It is sufficiently mixed to be added to the water progress by this preparation method for lithium iron phosphate positive material to be modified, carbon source and additive
It closes uniform；Then, to mixing gained slurry grind, then using air-stream spraying dry by the way of to the slurry after grinding into
Row mist projection granulating；Finally, being again sintered mist projection granulating resulting material, improved spherical lithium iron phosphate anode is obtained after the completion of sintering
Material.
Mixing equipment is used as using mulser, high speed disperser and sand mill etc. in this programme, to guarantee LiFePO4, carbon
Source and additive are sufficiently mixed uniformly, are coated on carbon source and additive around lithium iron phosphate positive material particle.
Furthermore lithium iron phosphate positive material to be modified is producer's finished product lithium iron phosphate positive electrode, especially function here
Rate type positive electrode.In addition, the lithium iron phosphate positive material particle before mixing is 0.2~2um.
The preferred glucose of the carbon source used in this programme, polyvinyl alcohol, sucrose, soluble starch, cellulose, phenolic aldehyde tree
One of rouge is a variety of.
The preferred carbon nanotube of the additive used in this programme, graphene, SP it is one or more.
Traditional mist projection granulating tower is replaced to carry out mist projection granulating, air-flow spray using air-stream spraying drying equipment in this programme
Mist drying equipment be the oxide-based air-stream spraying drying equipment of water system, the drying equipment by lithium iron phosphate positive material, carbon source and
Additive is dried by fog-spray nozzle, guarantees that the particle of uniformly mixed aqueous slurry is dried rapidly and the homogeneity of partial size, guarantee
The uniformity of material, so that the modified phosphate iron lithium anode material of partial size qualification can be obtained.
Accordingly, this programme completes LiFePO4, carbon source and additive after evenly mixing with mixing equipment, will be uniformly mixed
Slurry, with air-stream spraying drying equipment be granulated.When mist projection granulating, slurry is atomized into small liquid by nozzle and compressed air collision
Drop, drop complete mist projection granulating using micron particles are become after hot dry air drying.
In order to guarantee that particle is dried rapidly and the homogeneity of partial size, the slurry mixed in this programme is with 100-
The total mass flow rate of 900kg/h is sprayed from nozzle, while matched, and the pressure of compressed air used is 0.2-0.7MPa and institute
It is 200-300 DEG C with the temperature of hot dry air, thus the granularity of mist projection granulating resulting material reaches 5-10 μm.
In addition, this programme is sintered when being sintered to mist projection granulating resulting material using nitrogen atmosphere stove, and burn
The temperature of knot is 600-900 DEG C, and the time is 4-24 hours, after finally sintering gained powder sieving, obtains modified spherical phosphoric acid
Iron lithium anode material.In specific sintering, preferably 600 DEG C of sintering temperature, 700 DEG C or 800 DEG C, the preferred 4-18 of sintering time is small
When.
Processing improves preparation method by improving second of packet to LiFePO 4 material with carbon source and additive accordingly
Effect is covered, and improves electric conductivity.It is formed by modified spherical lithium iron phosphate positive material, improves granular size, reduces ratio
Surface area, keeps the spherical morphology of second particle, so that material be made to have better electric conductivity and smaller specific surface area (ginseng
See Fig. 1).Even if making the modified spherical lithium iron phosphate positive material under wet blending process, still there is good processing performance and excellent
Different multiplying power and cycle performance.
This is because carbon source and additive are uniformly coated on lithium iron phosphate particles surface, and are burning after spray drying
After knot, residual carbon can also be uniformly coated on lithium iron phosphate particles surface, form good conductive network；And the process coated
In, to the modification that coarse particle carries out, so that particle surface is more smooth.
Based on above-mentioned preparation method, the process of modified spherical lithium iron phosphate anode material is illustratively prepared below, it should
Preparation process is as follows:
1) in parts by weight by 95~98 parts of lithium iron phosphate positive material to be modified, 1~5 part of carbon source and additive 1~5
Part is added in the dispersing apparatus equipped with pure water 100-300 parts, is sufficiently mixed 2~8h, is coated on carbon source and additive to be modified
Lithium iron phosphate positive material particle around；
2) slurry being mixed to get is ground 2~6 hours with sand mill, guarantees that slurry is uniformly mixed；
3) with air-stream spraying drying equipment to ground slurry mist projection granulating, slurry is with the gross mass of 100-900kg/h
Flow velocity is sprayed from nozzle and the pressure of compressed air used is 0.2-0.7MPa, and the temperature of hot dry air used is 250 ± 50 DEG C,
So that the granularity of mist projection granulating resulting material reaches 5-10 μm；
4) mist projection granulating resulting material is sent into nitrogen atmosphere stove and is sintered, be first warming up to 700 ± 50 DEG C, then keep the temperature 3-
10 hours, then natually cooled to room temperature, the time of entire sintering process are 4~18 hours, after sintering gained powder sieving, are obtained
To modified phosphate iron lithium anode material.
In order to better understand and implement, this programme is described in detail below with reference to case study on implementation.
In the specific implementation, used mixing equipment is high speed disperser or sand mill uniformly to be divided to this programme
It dissipates.
Carbon source used is one of glucose, polyvinyl alcohol, sucrose, soluble starch, cellulose, phenolic resin or more
Kind.Additive therefor is one or more of carbon nanotube, graphene, SP.
Meanwhile used drying equipment is air-stream spraying pelletizer.
Embodiment 1
1) 96 parts of finished product lithium iron phosphate positive electrode, 3 parts of carbon source and 1 part of additive are added in parts by weight and pure water is housed
In 300 parts of high-speed dispersion equipment, it is sufficiently mixed 4h；
2) mixing gained slurry is ground, with air-stream spraying drying equipment to the slurry mist projection granulating after grinding, slurry
Material is sprayed with the total mass flow rate of 100-900kg/h from nozzle, and the pressure of compressed air used is 0.5MPa, hot dry air used
Temperature be 230 ± 10 DEG C, the granularity of mist projection granulating resulting material reaches D50 up to 8 μm；
3) mist projection granulating resulting material is sent into nitrogen atmosphere stove and is sintered, first pass through 4h temperature-rise period, it is warming up to 720 ±
10 DEG C, 6 hours then are kept the temperature, then natually cooled to room temperature, the time of entire sintering process is 10 hours, sintering gained powder
After sieving, the improved spherical lithium iron phosphate anode material of processing performance is obtained.
Embodiment 2
1) 97 parts of lithium iron phosphate positive material, 2 parts of carbon source and 1 part of additive are added in parts by weight and pure water 300 is housed
In the nanometer sand mill of part, it is fully ground 4h；
2) mixing gained slurry is ground, with air-stream spraying drying equipment to the slurry mist projection granulating after grinding, slurry
Material is sprayed with the total mass flow rate of 100-900kg/h from nozzle, and the pressure of compressed air used is 0.4MPa, hot dry air used
Temperature be 240 ± 10 DEG C, the granularity of mist projection granulating resulting material reaches D50 up to 9 μm；
3) mist projection granulating resulting material is sent into nitrogen atmosphere stove and is sintered, first pass through 2h temperature-rise period, it is warming up to 740 ±
10 DEG C, 4 hours then are kept the temperature, then natually cooled to room temperature, the time of entire sintering process is 6 hours, sintering gained powder
After sieving, the improved spherical lithium iron phosphate anode material of processing performance is obtained.
By example 1, example 2 the improved spherical lithium iron phosphate anode material of processing performance and original sample compare
Analysis, specific as shown in Table 1 and Table 2:
Table 1
As shown in Table 1, embodiment 1, the average particle size of 2 samples, tap density are significantly greater than comparative example, specific surface area
It is significantly less than comparative example.
Table 2
As shown in Table 2, modified LiFePO 4 material 1,2 and primary sample are made into slurry, in similar initial viscosity
Under, embodiment 1,2 samples solid content be higher than the solid content of primary sample；And Stability of Slurry is also above primary sample；
The discharge capacity for being made into Sample Cell simultaneously is substantially better than primary sample.
Thus example can be good at it is found that can be improved the chemical property and processing performance of material based on this programme
Overcome the problems of prior art.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (10)
1. a kind of modification method for preparing of lithium iron phosphate positive material characterized by comprising
Firstly, by lithium iron phosphate positive material to be modified, carbon source and additive are added to the water uniformly mixed；
Then, mixing gained slurry is ground, and slurry after grinding is sprayed in such a way that air-stream spraying is dry
Mist is granulated；
Finally, mist projection granulating resulting material is sintered, modified spherical lithium iron phosphate anode material is obtained after the completion of sintering.
2. the modification method for preparing of lithium iron phosphate positive material according to claim 1, which is characterized in that the modified system
95~98 parts of lithium iron phosphate positive material to be modified, 1~5 part of carbon source and 1~5 part of additive are added in parts by weight in Preparation Method
Enter in the dispersing apparatus equipped with pure water 100-300 parts, is sufficiently mixed 2~8h, carbon source and additive is made to be coated on phosphoric acid to be modified
Around iron lithium anode material particle.
3. the modification method for preparing of lithium iron phosphate positive material according to claim 1, which is characterized in that the modified system
When Preparation Method carries out mist projection granulating to the slurry after grinding, the slurry after grinding is collided into mist by nozzle and compressed air first
It is melted into droplet, drop completes mist projection granulating using micron particles are become after hot dry air drying.
4. the modification method for preparing of lithium iron phosphate positive material according to claim 3, which is characterized in that the slurry with
The total mass flow rate of 100-900kg/h is sprayed from nozzle, and the pressure of compressed air used is 0.2-0.7MPa, hot dry air used
Temperature be 200-300 DEG C.
5. the modification method for preparing of lithium iron phosphate positive material according to claim 3 or 4, which is characterized in that the spray
The granularity that mist is granulated resulting material reaches 5-10 μm.
6. the modification method for preparing of lithium iron phosphate positive material according to claim 1, which is characterized in that the modified system
When Preparation Method is sintered mist projection granulating resulting material, sintering temperature is 600-900 DEG C, and the time is 6-24 hours.
7. the modification method for preparing of lithium iron phosphate positive material according to claim 1, which is characterized in that carbon source used is
One of glucose, polyvinyl alcohol, sucrose, soluble starch, cellulose, phenolic resin are a variety of.
8. the modification method for preparing of lithium iron phosphate positive material according to claim 1, which is characterized in that additive therefor
For one or more of carbon nanotube, graphene, SP.
9. a kind of modified phosphate iron lithium anode material, which is characterized in that the modified phosphate iron lithium anode material is wanted by right
The modification method for preparing of lithium iron phosphate positive material described in any one of 1-8 is asked to prepare to be formed.
10. modified phosphate iron lithium anode material according to claim 9, which is characterized in that the modified phosphate iron lithium is just
It is coated with carbon-coating on the particle of pole material, and forms conductive network.
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Application publication date: 20190614 |