CN109795998A - A kind of preparation method and lithium iron phosphate positive material promoting lithium iron phosphate positive material compacted density - Google Patents
A kind of preparation method and lithium iron phosphate positive material promoting lithium iron phosphate positive material compacted density Download PDFInfo
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- CN109795998A CN109795998A CN201811654742.0A CN201811654742A CN109795998A CN 109795998 A CN109795998 A CN 109795998A CN 201811654742 A CN201811654742 A CN 201811654742A CN 109795998 A CN109795998 A CN 109795998A
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- 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 provides a kind of preparation method and lithium iron phosphate positive material for promoting lithium iron phosphate positive material compacted density, including the material liquid mixed by raw material, material liquid is imported in sand mill system in parallel again and is ground, the parallel connection sand mill system is formed in parallel by least two sets sand milling units, and unit, which is sanded, in every set is connected in series by an at least sand mill；It carries out the slurry that the different-grain diameter grain after unit grinding is sanded in every set to be mixed into grinding slurry；It is dried to obtain presoma, calcining, graded crushing obtain lithium iron phosphate positive material powder.The present invention using different setting parameters the sand mill system in parallel that is formed in parallel of sands milling units and meanwhile grind, raising processing efficiency；The slurry of different-grain diameter can be formed simultaneously, so as to improve the compacted density of lithium iron phosphate positive material, so preparation method of the invention is efficiently, fast, improve production efficiency.
Description
Technical field
The present invention relates to field of lithium ion battery anode, particularly provide a kind of promotion lithium iron phosphate positive material pressure
The preparation method and lithium iron phosphate positive material of real density.
Background technique
Under new energy battery is increasingly prevailing, lithium iron phosphate positive material is because of its stable structure, charge and discharge platform is excellent, holds
Measure higher, good cycle, it is safe and nontoxic, low in cost the features such as, absolute market can not be completely replaced by making it have.?
In the consistent situation of each technique, the compacted density of positive electrode is bigger, and battery capacity can be done higher, so compacted density
It is considered as measuring one of the important indicator of positive electrode energy density.Compacted density not only with the real density of material, granularity
Size is related, also related with the particle diameter distribution of material and gradation.
The synthesis of existing LiFePO4 mainly with the synthesis of ferrophosphorus technique carbothermic method, this method first by raw material source of iron,
Lithium source, carbon source carry out wet-mixing and slurry is made in grinding, is then spray-dried, then dry powder high-temperature calcination is synthesized phosphoric acid
Iron lithium.The grinding stage is mainly ground with separate unit sand mill repeatedly, the approximate unimodal normal distribution of grinding gained slurry particle diameter distribution；
Have the shortcomings that compacted density is low by the LiFePO4 that the slurry that this single particle size is distributed finally synthesizes.Patent
201711315675.5 in such a way that the slurry of two kinds of different-grain diameters is mixed, and is formed size grading and is promoted finished product compacting,
But its method needs the synthesis of three steps, i.e., large and small partial size slurry is successively ground, then mixed.The slurry of batch grinding different-grain diameter
Material is unfavorable for large-scale continuous production than relatively time-consuming in production.
Summary of the invention
The drawbacks of slurry of a variety of partial size mixing can be ground by needing multistep just the present invention be directed to existing grinding technique, proposes
A kind of preparation method and lithium iron phosphate positive material promoting lithium iron phosphate positive material compacted density, can be made by one-step method
The mixed slurry of standby partial sizes a variety of out, to promote the compacted density and production efficiency of lithium iron phosphate positive material.
The technical solution adopted by the invention is as follows:
A kind of preparation method promoting lithium iron phosphate positive material compacted density, including the raw material mixed by raw material
Liquid further includes following preparation step:
(1) material liquid is imported in sand mill system in parallel and is ground, the parallel connection sand mill system is by least two
Set is sanded unit and is formed in parallel, and unit, which is sanded, in every set is connected in series by an at least sand mill；
(2) it carries out the slurry that the different-grain diameter after unit grinding is sanded in every set to be mixed into grinding slurry；
(3) grinding slurry is dried to obtain presoma by spray drying tower；
(4) presoma is obtained into LiFePO4 under inert gas protection in 600~800 DEG C of 6~12h of heat preservation；Most pass through afterwards
Crossing graded crushing and obtaining average particle size is 1~3 μm of lithium iron phosphate positive material powder.
Further scheme, the material liquid be by 70~80%wt source of iron, 15~20%wt lithium source, 5~10%wt carbon source,
1~5%wt additive is mixed in solvent, is stirred into the mixed serum that solid content is 30~60%.
Further scheme, the additive are copper oxide, in zinc oxide, indium oxide, tin oxide, lead oxide, bismuth oxide
At least one.
Further scheme, the source of iron are anhydrous iron phosphate or water-bearing phosphate iron；
The lithium source is lithium carbonate, lithium hydroxide or lithium acetate；
The carbon source is glucose, in sucrose, starch, citric acid, polyethylene glycol, polyacrylic acid, polyvinylpyrrolidone
At least one；
The solvent is pure water or ethyl alcohol.
Further scheme, material liquid described in step (1) import in different sand milling units individually ground simultaneously.
Further scheme, the sand mill are stick pin type, turbine type or disc type.
Preferably, in the sand mill fill zirconium sphere volume accounting be 30-90%, filling 0.2~1.2mm of zirconium ball size,
Revolving speed is in 400rpm~800rpm.
Further scheme, the average grain diameter for the grinding slurry being mixed into step (2) are 0.5~1.0 μm.
Further scheme, the inlet air temperature of spray drying tower described in step (3) is 230~250 DEG C, leaving air temp 80
~110 DEG C.
Another goal of the invention of the invention is to provide through lithium iron phosphate positive material prepared by above-mentioned preparation method, institute
The compacted density for stating lithium iron phosphate positive material is 2.55-2.65g/cm3。
The present invention grinds mixed slurry using sand mill system in parallel, wherein all sand millings in unit are sanded in every set
The abrasive parameters of machine are consistent, and the abrasive parameters that unit is sanded in difference are different, to make after unit grinding is sanded in every set
Slurry partial size it is different, that is, reach different grinding effects.
It is to work at the same time since unit is sanded in set every in sand mill system in parallel, the slurry of different-grain diameter can be formed simultaneously
Material；Then it is mixed again after discharging, reaches one-step method grinding different-grain diameter mixed slurry；Finally by mixed sand slurry
Carry out spray drying prepare presoma, high temperature sintering obtains iron phosphate powder.Due to LiFePO4 during the sintering process
Powder has reunion, therefore to be crushed to it, be classified to obtain high-compaction lithium iron phosphate anode powder.
After pole piece is made in lithium iron phosphate positive material prepared by the present invention, compacted density reaches 2.55-2.65g/cm3、
Soft Roll 1C specific discharge capacity 145mAh/g or more.
The present invention is ground using the sand mill system in parallel that the sand milling unit of different setting parameters is formed in parallel, that is, is starched
Material is ground respectively by different sand milling units, forms the slurry of different-grain diameter, and when discharging is mixed again can reach one
Different-grain diameter mixed slurry is ground in footwork, and the parameter of each sand mill can be arranged according to the needs of different-grain diameter, i.e., suitable
Ying Xingqiang.Grinding method of the invention efficiently, fast, can be improved production efficiency.
The additive being added in the present invention is copper oxide, zinc oxide, indium oxide, tin oxide, lead oxide, bismuth oxide, is had
Help promote LiFePO4 electric conductivity, is conducive to LiFePO4 electrical property and plays.
Specific embodiment
Embodiment 1
A kind of preparation method promoting lithium iron phosphate positive material compacted density comprising following preparation step:
(1) 74%wt source of iron anhydrous iron phosphate, 18%wt lithium source lithium carbonate, 7%wt carbon source glucose, 1~5%wt are added
Add agent copper oxide to be mixed in solvent pure water, is stirred into the mixed serum that solid content is 45%；
(2) sand mill system in parallel is formed in parallel by two sets of sand milling units, and unit, which is sanded, in every set a sand mill；It will
Mixed serum imports in two sets of sand milling units individually ground respectively simultaneously；Wherein zirconium sphere volume is filled in two sand mills to account for
Than being respectively 400rpm, 800rpm for 60%, filling zirconium ball size 0.6mm, revolving speed.
(3) it carries out the slurry that the different-grain diameter grain after unit grinding is sanded in every set to be mixed into grinding slurry, be averaged grain
Diameter is 0.85 μm；
(4) be 245 DEG C by inlet air temperature by grinding slurry, the spray drying tower that leaving air temp is 95 DEG C is dried
To presoma；
(5) presoma is obtained into LiFePO4 under inert gas protection in 780 DEG C of heat preservation 8h；It is finally broken by classification
The broken lithium iron phosphate positive material powder for obtaining average particle size and being 1.86 μm.
Embodiment 2
A kind of preparation method promoting lithium iron phosphate positive material compacted density comprising following preparation step:
(1) by 70%wt source of iron anhydrous iron phosphate, 20%wt lithium source lithium acetate, 5%wt carbon source polyvinylpyrrolidone,
2%wt additive zinc oxide is mixed in solvent pure water, is stirred into the mixed serum that solid content is 30%；
(2) mixed serum is imported in sand mill system in parallel and is ground, sand mill system in parallel is sanded by two sets
Unit is formed in parallel, and unit, which is sanded, in every set is connected in series by two sand mills；Mixed serum is imported into two sets of sand mills simultaneously
It is individually ground respectively in group, every set is sanded to be introduced into First sand mill in unit and be ground, and then enters back into the
It carries out grinding to obtain slurry in two sand mills.Wherein filling zirconium sphere volume accounting is in a set of sand mill being sanded in unit
30%, zirconium ball size 0.4mm, revolving speed 600rpm are filled；Zirconium sphere volume is filled in sand mill in another set of sand milling unit to account for
Than for 50%, filling zirconium ball size 0.8mm, revolving speed 600rpm.
(3) it carries out the slurry that the different-grain diameter grain after unit grinding is sanded in every set to be mixed into grinding slurry, be averaged grain
Diameter is 0.5 μm；
(4) be 230 DEG C by inlet air temperature by grinding slurry, the spray drying tower that leaving air temp is 80 DEG C is dried
To presoma；
(5) presoma is obtained into LiFePO4 under inert gas protection in 600 DEG C of heat preservation 12h；It is finally broken by classification
The broken average particle size that obtains is 1.93 μm of lithium iron phosphate positive material powder.
Embodiment 3
A kind of preparation method promoting lithium iron phosphate positive material compacted density comprising following preparation step:
(1) by 80%wt source of iron water-bearing phosphate iron, 15%wt lithium source lithium hydroxide, 10%wt carbon source (sucrose+starch),
3%wt additive indium oxide is mixed in etoh solvent, is stirred into the mixed serum that solid content is 50%；
(2) mixed serum is imported in sand mill system in parallel and is ground, sand mill system in parallel is sanded by three sets
Unit is formed in parallel, and unit, which is sanded, in every set is connected in series by a sand mill；Mixed serum imports three sets of sand milling units simultaneously
It is middle individually to be ground respectively.Filled in three sand mills zirconium sphere volume accounting be 90%, filling zirconium ball size is respectively 0.2,
0.7,1.2mm, revolving speed are respectively 400rpm, 500rpm, 600rpm.
(3) it carries out the slurry that the different-grain diameter grain after unit grinding is sanded in every set to be mixed into grinding slurry, be averaged grain
Diameter is 0.78 μm；
(4) be 250 DEG C by inlet air temperature by grinding slurry, the spray drying tower that leaving air temp is 110 DEG C is dried
Obtain presoma；
(5) presoma is obtained into LiFePO4 under inert gas protection in 800 DEG C of heat preservation 6h；It is finally broken by classification
The broken average particle size that obtains is 2 μm of lithium iron phosphate positive material powder.
Embodiment 4
A kind of preparation method promoting lithium iron phosphate positive material compacted density comprising following preparation step:
(1) by 76%wt source of iron anhydrous iron phosphate, 18%wt lithium source lithium acetate, 8%wt carbon source (polyethylene glycol+polypropylene
Acid), 3%wt additive tin oxide be mixed in etoh solvent, be stirred into solid content be 60% mixed serum；
(2) mixed serum is imported in sand mill system in parallel and is ground, sand mill system in parallel is sanded by two sets
Unit is formed in parallel, wherein a set of sand milling unit is made of a sand mill, wherein filling zirconium sphere volume accounting is 50%, fills out
Zirconium ball size 0.5mm, revolving speed are filled in 400rpm, and another set of sand milling unit is made of two sand mills, wherein filling zirconium sphere
Product accounting is 80%, filling zirconium ball size 0.9mm, revolving speed are in 600rpm；Mixed serum simultaneously import two sets of sand milling units in into
Row is individually ground.
(3) it carries out the slurry that the different-grain diameter grain after unit grinding is sanded in every set to be mixed into grinding slurry, be averaged grain
Diameter is 1.0 μm；
(4) be 240 DEG C by inlet air temperature by grinding slurry, the spray drying tower that leaving air temp is 100 DEG C is dried
Obtain presoma；
(5) presoma is obtained into LiFePO4 under inert gas protection in 700 DEG C of heat preservation 10h；It is finally broken by classification
The broken average particle size that obtains is 2.98 μm of lithium iron phosphate positive material powder.
Comparative example
1) raw material mixes: 74%wt ferric phosphate, 18%wt lithium carbonate, 7%wt glucose, 1%wt titanium dioxide are pressed
45% solid content, which is dissolved in pure water, to be uniformly mixed.
2) grind slurrying: the slurry that step 1) is uniformly mixed imports filling zirconium ball accounting 60%, filling zirconium ball size
The separate unit sand mill progress multipass grinding of 0.6mm, revolving speed 500rpm, obtain the slurry that granularity is 0.81 μm.
3) powder synthesizes: step 2) slurry is carried out by the spray drying tower of 245 DEG C of inlet air temperature, 95 DEG C of leaving air temp
It is dried to obtain presoma, then handles to obtain LiFePO4 in 780 DEG C of heat preservation 8h under inert gas protection by presoma, finally
1.92 μm of granularity of iron phosphate powder is obtained by classification.
Its compacted density is detected and through it to above-described embodiment 1-4 and comparative example the lithium iron phosphate positive material powder prepared
Manufactured soft-package battery (other than positive electrode is respectively selected from the material of above-described embodiment 1-4 and comparative example preparation, tie by others
Structure, composition are the same) performance test 1C specific discharge capacity, shown in table specific as follows:
| Compacted density/gcm-3 | 1C specific discharge capacity/mAhg-1 | |
| Embodiment 1 | 2.60 | 145.6 |
| Embodiment 2 | 2.64 | 145.1 |
| Embodiment 3 | 2.61 | 145.8 |
| Embodiment 4 | 2.58 | 146.2 |
| Comparative example | 2.35 | 145.2 |
It can be seen that from upper table, the present invention is ground using the sand mill system in parallel that different sand milling units are formed in parallel,
It can achieve the slurry that different-grain diameter mixing is made in one-step method, to improve the compacted density of lithium iron phosphate positive material, together
When ensure that specific discharge capacity.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of preparation method for promoting lithium iron phosphate positive material compacted density, including the material liquid mixed by raw material,
It is characterized by also including following preparation steps:
(1) material liquid is imported in sand mill system in parallel and is ground, the parallel connection sand mill system is by least two sets of sand
Grinding machine group is formed in parallel, and unit, which is sanded, in every set is connected in series by an at least sand mill；
(2) it carries out the slurry that the different-grain diameter after unit grinding is sanded in every set to be mixed into grinding slurry；
(3) grinding slurry is dried to obtain presoma by spray drying tower；
(4) presoma is obtained into LiFePO4 under inert gas protection in 600~800 DEG C of 6~12h of heat preservation；Finally through excessive
The broken average particle size that obtains of grade is 1~3 μm of lithium iron phosphate positive material powder.
2. preparation method according to claim 1, it is characterised in that: the material liquid be by 70~80%wt source of iron, 15~
20%wt lithium source, 5~10%wt carbon source, 1~5%wt additive are mixed in solvent, and being stirred into solid content is 30~60%
Mixed serum.
3. preparation method according to claim 2, it is characterised in that: the additive is copper oxide, zinc oxide, oxidation
At least one of indium, tin oxide, lead oxide, bismuth oxide.
4. preparation method according to claim 2, it is characterised in that: the source of iron is anhydrous iron phosphate or water-bearing phosphate
Iron；
The lithium source is lithium carbonate, lithium hydroxide or lithium acetate；
The carbon source be glucose, sucrose, starch, citric acid, polyethylene glycol, polyacrylic acid, in polyvinylpyrrolidone extremely
Few one kind；
The solvent is pure water or ethyl alcohol.
5. preparation method according to claim 1, it is characterised in that: material liquid described in step (1) imports difference simultaneously
Sand milling unit in individually ground.
6. preparation method according to claim 5, it is characterised in that: the sand mill is stick pin type, turbine type or disc type.
7. preparation method according to claim 5, it is characterised in that: filling zirconium sphere volume accounting in the sand mill is
30-90%, filling 0.2~1.2mm of zirconium ball size, revolving speed are in 400rpm~800rpm.
8. preparation method according to claim 1, it is characterised in that: the grinding slurry being mixed into step (2) is averaged
Partial size is 0.5~1.0 μm.
9. preparation method according to claim 1, it is characterised in that: the air inlet temperature of spray drying tower described in step (3)
Degree is 230~250 DEG C, leaving air temp is 80~110 DEG C.
10. the lithium iron phosphate positive material as prepared by claim 1-9 described in any item preparation methods, it is characterised in that:
The compacted density of the lithium iron phosphate positive material is 2.55-2.65g/cm3。
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Cited By (5)
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| CN112310374A (en) * | 2020-10-30 | 2021-02-02 | 合肥融捷能源材料有限公司 | Method for preparing high-compaction low-specific-surface-area lithium iron phosphate by sectional grinding-spray drying |
| CN113582150A (en) * | 2021-07-19 | 2021-11-02 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of high-compaction lithium iron phosphate cathode material |
| CN114162800A (en) * | 2021-11-15 | 2022-03-11 | 广东派勒智能纳米科技股份有限公司 | Production method of lithium ion battery anode material |
| CN116443840A (en) * | 2023-03-28 | 2023-07-18 | 合肥国轩高科动力能源有限公司 | Lithium iron phosphate positive electrode material and preparation method thereof |
| CN116730313A (en) * | 2023-06-25 | 2023-09-12 | 江西智锂科技股份有限公司 | Preparation method of ultralow-temperature lithium iron phosphate positive electrode material |
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Application publication date: 20190524 |