CN107819121A - A kind of LiFePO 4 activity regenerating method - Google Patents
A kind of LiFePO 4 activity regenerating method Download PDFInfo
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- CN107819121A CN107819121A CN201711026166.0A CN201711026166A CN107819121A CN 107819121 A CN107819121 A CN 107819121A CN 201711026166 A CN201711026166 A CN 201711026166A CN 107819121 A CN107819121 A CN 107819121A
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- lithium
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4242—Regeneration of electrolyte or reactants
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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
It is an object of the invention to provide a kind of easy low activity or inactive LiFePO 4 renovation process, this method to comprise the following steps：S1, lithium iron phosphorus content and carbon content detection are carried out to low activity or inactive LiFePO 4, are then 1 according to lithium iron phosphorus mol ratio:1:1 calculates lithium source, source of iron and the phosphorus source for needing to add；The carbon source added is calculated by carbon content 3% 7%；S2, wet ball grinding；It is prepared by S3, presoma：Add active lithium iron phosphate precursor in ball mill, the active lithium iron phosphate precursor of addition is 3% 10% of low activity or inactive LiFePO 4 quality in step S2, continues grinding 36 hours, is then granulated using Centrafugal spray drying tower；S4, presoma sintering；S5, crushing obtain even-grained high activity LiFePO 4.This method can obtain the active LiFePO 4 with excellent chemical property.
Description
Technical field
The present invention relates to the regeneration field of LiFePO 4, more particularly to a kind of LiFePO 4 activity regenerating method.
Background technology
Lithium iron phosphate cathode material is because of its excellent electrical property, reliable security, environmental nonpollution and its original use
Expect many advantages, such as cheap, and be applied to the fields such as automobile, energy storage, communication extensively.
The synthesis of lithium iron phosphate cathode material is according to mol ratio 1 by lithium source, source of iron and phosphorus source three:1:1 mixing, warp
High temperature sintering is crossed to be made.Wherein carbothermic method is that ferric iron element reduction is ferrous iron by a small amount of carbon source of addition, is obtained simultaneously
The carbon-coating cladding of LiFePO 4, it can play a part of improving electronic conductance and suppressing crystal grain growing up.Therefore, in the factory of reality
During preparing LiFePO 4, the air-tightness of control, burner hearth and the purity of inert gas to carbon content have very high
It is required that.But existing technology is difficult complete matching these requirements, there is a little fluctuation, can all occurred underproof in these conditions
LiFePO 4, not only carbon content or lithium iron phosphorus content can be unbalance, and under occurring significantly in terms of the electro-chemical activity
Drop.
Patent CN102064366B discloses a kind of renovation process of LiFePO4, and this method includes（1）By waste phosphoric acid iron
Lithium heat in atmosphere it is fully oxidized, heating-up temperature be 500 DEG C ~ 800 DEG C,（2）Step（1）Carbon source is added in obtained product to fill
Divide mixing,（3）Step（2）Obtained mixture is incubated 3 ~ 5 hours in atmosphere protection, and the temperature of insulation is 600 DEG C ~ 800 DEG C,
It is cooled to 100 DEG C of taking-ups.The patent needs high-temperature process twice, not only increases the energy consumption of manpower electric power, and is easily caused crystal grain
Grow up, the battery capacity of finished product is also only in 120mAh/g or so.
It can be seen that the renovation process of existing LiFePO4 needs high-temperature process twice, the battery of finished product big there is energy consumption
The problem of capacity is relatively low.
The content of the invention
Big in order to solve energy consumption existing for the renovation process of existing LiFePO4, the battery capacity of finished product is relatively low to ask
Topic, the present invention proposes a kind of low activity or inactive LiFePO 4 renovation process, and can obtain higher battery capacity.
A kind of low activity of the invention or inactive LiFePO 4 activity regenerating method, comprise the following steps：
S1, Element detection：Lithium iron phosphorus content and carbon content detection are carried out to low activity or inactive LiFePO 4, then according to
Lithium iron phosphorus mol ratio is 1:1:1 calculates lithium source, source of iron and the phosphorus source for needing to add；Being calculated by carbon content 3%-7% to add
Carbon source；
S2, wet ball grinding：By low activity or inactive LiFePO 4 input ball mill in, then add deionized water, go from
Sub- water is 1.5 with the mass ratio of low activity or inactive LiFePO 4:1, add the need that step S1 is calculated and add lithium iron
Phosphorus source and carbon source, mix 4-12 hours, and stir speed (S.S.) is 60-120 revs/min；
It is prepared by S3, spraying presoma：Active lithium iron phosphate precursor, the active LiFePO 4 of addition are added in ball mill
Presoma is low activity or the 3%-10% of inactive LiFePO 4 quality in step S2, continues to grind 3-6 hours, then uses
Centrafugal spray drying tower is granulated, and obtains presoma of spraying；
S4, spraying presoma sintering：By spraying presoma obtained by step S3, in an inert atmosphere, one-step method high temperature sintering, i.e., with
5 DEG C/min is warming up to 700 ~ 800 DEG C of insulation 4-12 hours, subsequent Temperature fall；
S5, crushing：By the material obtained by step S4, crushed using airslide disintegrating mill, it is sub- to obtain even-grained high activity phosphoric acid
Iron lithium.
Further, source of iron is iron oxide, ferrous oxalate, ferrous oxide, ferroso-ferric oxide, chlorination in the step S1
One or more in iron, frerrous chloride, iron hydroxide, ferric nitrate, ferrous nitrate, phosphate dihydrate iron and anhydrous iron phosphate.
Further, phosphorus source is the one or more in the hydrogen ammonia of phosphoric acid one and ammonium dihydrogen phosphate in the step S1.
Further, lithium source is lithium carbonate, lithium phosphate, lithium dihydrogen phosphate, lithium chloride, a water hydroxide in the step S1
One or more in lithium.
Further, carbon source is the one or more in sucrose or glucose in the step S1.
Further, lithium iron phosphorus content examination criteria is YS/T1028.1-2015, YS/T1028.2- in the step S1
2015、YS/T1028.3-2015；The examination criteria of carbon source is YS/T1028.4-2015.
Further, the abrasive media of ball mill is zirconia ball in the step S2, and ball grinder liner is polyurethane bag
Cover, material is 1 with polyurethane ball weight ratio:3-1:5.
Further, the active lithium iron phosphate precursor of the step S3 is that lithium iron phosphorus mol ratio is 1:1:1 raw material
Mixture, wherein lithium source, source of iron and phosphorus source are identical with step S1 lithium source, source of iron and phosphorus source.
Further, the spray drying out temperature of the step S3 is respectively 160 ~ 250 DEG C and 80 ~ 110 DEG C, is atomized
Disk rotating speed is 16000 ~ 24000 revs/min.
Further, the broken air pressure using 0.8MPa of air-flow, meso-position radius Task-size Controlling to 1-2 in the step S5
Micron.
The present invention is with a small amount of active lithium iron phosphate precursor cladding low activity or inactive LiFePO 4, using simple
Lithium iron P elements supplement and a step high temperature sintering, the active LiFePO 4 with excellent chemical property can be obtained.Utilize
A small amount of active lithium iron phosphate precursor is used as " dopant ", not only acts as the work of cladding low activity or inactive LiFePO 4
With, and also have certain catalytic effect to LiFePO 4 active regeneration, by simple lithium iron P elements supplement and a step
High temperature sintering, you can obtain active LiFePO 4 of the capacity in 135mAh/g.
Brief description of the drawings
Fig. 1 is the LiFePO 4 sample LFP-A and prior art of the present invention plus the preparation of active lithium iron phosphate precursor
It is not added with LiFePO 4 LFP-B prepared by active lithium iron phosphate precursor full battery 1C charge and discharge electrographs.
Embodiment
The present invention is described further with specific embodiment below in conjunction with the accompanying drawings：
Embodiment 1
The grey low activity LiFePO 4 for weighing 10kg is added in ball mill, adds 15L deionized waters.Test low activity phosphorus
The lithium of ferrous silicate lithium, iron, phosphorus mol ratio are 0.81：0.87：1, according to lithium, iron, phosphorus mol ratio 1:1:1 dispensing, add a hydration
Lithium hydroxide 495g, iron oxide 645g；It is 1.3% to test its carbon content, adds sucrose 1.45kg, is ground 8 hours.Weigh a water
Lithium hydroxide 79.7g is closed, ammonium dihydrogen phosphate 218.8g, iron oxide 151.8g, is added in ball mill, is ground 4 hours.Make afterwards
With Centrafugal spray drying tower mist projection granulating, out temperature is 180 and 80 DEG C, and atomizing disk turns 18000 revs/min of kettle.Forerunner
Body is in nitrogen atmosphere, a step high temperature sintering, and being warming up to 780 DEG C with 5 DEG C/min is incubated 4 hours, subsequent Temperature fall；Use gas
Flow disintegrating machine to crush, the broken air pressure using 0.8MPa of air-flow, obtained LiFePO 4 finished product.
Embodiment 2
The grey low activity LiFePO 4 for weighing 10kg is added in ball mill, adds 15L deionized waters.Test low activity phosphorus
The lithium of ferrous silicate lithium, iron, phosphorus mol ratio are 1：0.97：0.85, according to lithium, iron, phosphorus mol ratio 1:1:1 dispensing, add phosphoric acid one
Hydrogen ammonium 1230.4g, ferrous oxide 133.9g；It is 0.97% to test its carbon content, adds sucrose 1.60kg, is ground 7 hours.Weigh
Lithium carbonate 234g, monoammonium phosphate 837g, ferrous oxide 455g, it is added in ball mill, grinds 5 hours.Afterwards using centrifugation
Formula spray drying tower mist projection granulating, out temperature are 210 and 90 DEG C, and atomizing disk turns 20000 revs/min of kettle.Presoma is in nitrogen
In gas atmosphere, a step high temperature sintering, it is warming up to 770 DEG C with 5 DEG C/min and is incubated 5 hours, subsequent Temperature fall；Crushed using air-flow
Machine crushes, the broken air pressure using 0.8MPa of air-flow, obtained LiFePO 4 finished product.
Embodiment 3
The white inactive LiFePO 4 for weighing 10kg is added in ball mill, adds 15L deionized waters.Test inactive phosphorus
The lithium of ferrous silicate lithium, iron, phosphorus mol ratio are 1：0.97：0.97, according to lithium, iron, phosphorus mol ratio 1:1:1 dispensing, adds ferric phosphate
281g；It is 0.3% to test its carbon content, adds sucrose 1.86kg, is ground 12 hours.Lithium carbonate 117g, ferric phosphate 478g are weighed,
It is added in ball mill, grinds 5 hours.Centrafugal spray drying tower mist projection granulating is used afterwards, and out temperature is 220 Hes
100 DEG C, atomizing disk turns 21000 revs/min of kettle.Presoma a step high temperature sintering, is warming up in nitrogen atmosphere with 5 DEG C/min
760 DEG C are incubated 6 hours, subsequent Temperature fall；Crushed using air-flow disintegrating machine, the broken air pressure using 0.8MPa of air-flow,
Obtained LiFePO 4 finished product.
Embodiment 4
The white inactive LiFePO 4 for weighing 10kg is added in ball mill, adds 15L deionized waters.Test inactive phosphorus
The lithium of ferrous silicate lithium, iron, phosphorus mol ratio are 0.96：1：0.97, according to lithium, iron, phosphorus mol ratio 1:1:1 dispensing, adds lithium chloride
104g, the hydrogen ammonia 246g of phosphoric acid one；It is 0.2% to test its carbon content, adds glucose 3.11kg, is ground 10 hours.Weigh lithium chloride
186g, ferroso-ferric oxide 343g, the hydrogen ammonia 586g of phosphoric acid one, are added in ball mill, grind 6 hours.Centrifugal spray is used afterwards
Mist drying tower mist projection granulating, out temperature are 240 and 110 DEG C, and atomizing disk turns 24000 revs/min of kettle.Presoma is in nitrogen gas
In atmosphere, a step high temperature sintering, it is warming up to 790 DEG C with 5 DEG C/min and is incubated 4 hours, subsequent Temperature fall；Use air-flow disintegrating machine powder
It is broken, the broken air pressure using 0.8MPa of air-flow, obtained LiFePO 4 finished product.
Now detected with embodiment 1, the LiFePO 4 of synthesis is represented with LFP-A, its discharge curve such as Fig. 1 institutes
Show.
Test as a comparison, under above-mentioned the same terms, be added without active lithium iron phosphate precursor, the phosphoric acid of synthesis is sub-
Iron lithium is represented with LFP-B.
By positive electrode, SP, PVDF in mass ratio 8:1:1 is well mixed, is then coated on 0.018mm aluminium foil,
Coating thickness is 100-120 microns, and anode pole piece is obtained after fully drying, through rolling-winding-dress shell, laser welding sealing,
Fluid injection in glove box full of argon gas, finally carries out charge-discharge performance test on LAND cell testers, and charging/discharging voltage is
4.2~2.5V.
With reference to shown in full battery 1C discharge curves Fig. 1 of lithium iron phosphate cathode material, room temperature measures LFP-A electric discharge specific volumes
Measure as 135 mAh/g, 110 mAh/g far above LFP-B.
Summary, the present invention are adopted with a small amount of active lithium iron phosphate precursor cladding low activity or inactive LiFePO 4
With simple lithium iron P elements supplement and a step high temperature sintering, the active ferrous phosphate with excellent chemical property can be obtained
Lithium.
The specific embodiment of the present invention is described in detail above, but it is intended only as example, it is of the invention and unlimited
It is formed on particular embodiments described above.To those skilled in the art, it is any to the equivalent modifications that carry out of the present invention and
Substitute also all among scope of the invention.Therefore, waiting for being made without departing from the spirit and scope of the invention is exchanged and repaiied
Change, all should be contained within the scope of the invention.
Claims (10)
1. a kind of LiFePO 4 activity regenerating method, comprises the following steps：
S1, Element detection：Lithium iron phosphorus content and carbon content detection are carried out to low activity or inactive LiFePO 4, then according to
Lithium iron phosphorus mol ratio is 1:1:1 calculates lithium source, source of iron and the phosphorus source for needing to add；Being calculated by carbon content 3%-7% to add
Carbon source；
S2, wet ball grinding：By low activity or inactive LiFePO 4 input ball mill in, then add deionized water, go from
Sub- water is 1.5 with the mass ratio of low activity or inactive LiFePO 4:1, add the need that step S1 is calculated and add lithium iron
Phosphorus source and carbon source, mix 4-12 hours, and stir speed (S.S.) is 60-120 revs/min；
It is prepared by S3, spraying presoma：Active lithium iron phosphate precursor, the active LiFePO 4 of addition are added in ball mill
Presoma is low activity or the 3%-10% of inactive LiFePO 4 quality in step S2, continues to grind 3-6 hours, then uses
Centrafugal spray drying tower is granulated, and obtains presoma of spraying；
S4, spraying presoma sintering：By presoma obtained by step S3, in an inert atmosphere, one-step method high temperature sintering, i.e., with 5 DEG C/
Min is warming up to 700 ~ 800 DEG C of insulation 4-12 hours, subsequent Temperature fall；
S5, crushing：By the material obtained by step S4, crushed using airslide disintegrating mill, it is sub- to obtain even-grained high activity phosphoric acid
Iron lithium.
2. renovation process according to claim 1, it is characterised in that source of iron is iron oxide, oxalic acid Asia in the step S1
Iron, ferrous oxide, ferroso-ferric oxide, iron chloride, frerrous chloride, iron hydroxide, ferric nitrate, ferrous nitrate, phosphate dihydrate iron and
One or more in anhydrous iron phosphate.
3. renovation process according to claim 1, it is characterised in that phosphorus source is the hydrogen ammonia of phosphoric acid one and phosphorus in the step S1
One or more in acid dihydride ammonium.
4. renovation process according to claim 1, it is characterised in that in the step S1 lithium source be lithium carbonate, lithium phosphate,
One or more in lithium dihydrogen phosphate, lithium chloride, Lithium hydroxide monohydrate.
5. renovation process according to claim 1, it is characterised in that carbon source is in sucrose or glucose in the step S1
One or more.
6. renovation process according to claim 1, it is characterised in that lithium iron phosphorus content examination criteria is in the step S1
YS/T1028.1-2015、YS/T1028.2-2015、YS/T1028.3-2015；The examination criteria of carbon source is YS/T1028.4-
2015。
7. according to the renovation process any one of claim 1-6, it is characterised in that ball mill grinds in the step S2
Grinding media is zirconia ball, and ball grinder liner coats for polyurethane, and material is 1 with polyurethane ball weight ratio:3-1:5.
8. renovation process according to claim 7, it is characterised in that the active lithium iron phosphate precursor of the step S3
It is 1 for lithium iron phosphorus mol ratio:1:1 raw mixture, wherein lithium source, source of iron and phosphorus source and step S1 lithium source, source of iron and phosphorus
Source is identical.
9. renovation process according to claim 8, it is characterised in that the spray drying out temperature point of the step S3
Wei not be 160 ~ 250 DEG C and 80 ~ 110 DEG C, atomizing disk rotating speed is 16000 ~ 24000 revs/min.
10. renovation process according to claim 9, it is characterised in that air-flow is broken in the step S5 uses 0.8MPa
Air pressure, meso-position radius Task-size Controlling to 1-2 microns.
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