CN106731927A - A kind of preparation method of lithium metal even particulate dispersion slurry - Google Patents
A kind of preparation method of lithium metal even particulate dispersion slurry Download PDFInfo
- Publication number
- CN106731927A CN106731927A CN201611168980.1A CN201611168980A CN106731927A CN 106731927 A CN106731927 A CN 106731927A CN 201611168980 A CN201611168980 A CN 201611168980A CN 106731927 A CN106731927 A CN 106731927A
- Authority
- CN
- China
- Prior art keywords
- lithium metal
- butadiene
- styrene rubber
- polar solven
- particulate dispersion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/50—Mixing liquids with solids
- B01F23/51—Methods thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F21/00—Dissolving
- B01F21/02—Methods
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F21/00—Dissolving
- B01F21/10—Dissolving using driven stirrers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/50—Mixing liquids with solids
- B01F23/55—Mixing liquids with solids the mixture being submitted to electrical, sonic or similar energy
- B01F23/551—Mixing liquids with solids the mixture being submitted to electrical, sonic or similar energy using vibrations
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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
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0404—Methods of deposition of the material by coating on electrode collectors
-
- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention provides a kind of preparation method of lithium metal even particulate dispersion slurry, comprises the following steps：Under magneton stirring, butadiene-styrene rubber is dissolved in non-polar solven, magneton mixing speed is 800 turns per minute, mixing time is 2 hours；The mixed solution of butadiene-styrene rubber/non-polar solven has been transferred in lid narrow-mouthed bottle；Lithium metal particle is added to the mixed solution of butadiene-styrene rubber/non-polar solven, narrow-mouthed bottle is sealed on bottle stopper, and sealed with sealing film；Will be equipped with lithium metal particle, the narrow-mouthed bottle of the mixed solution of butadiene-styrene rubber/non-polar solven and be placed in Ultrasound Instrument ultrasonic half an hour, obtain final product lithium metal even particulate dispersion slurry, and shift and saved backup in the glove box of argon gas protection.The present invention can form the suspension of lithium metal even particulate dispersion, and side reaction will not occur cause lithium to lose, and method is simple, is easy to large-scale industrialized production.
Description
Technical field
The present invention relates to electrochemical material manufacturing technology field, and in particular to a kind of lithium metal even particulate dispersion slurry
Preparation method.
Background technology
Be commercialized for lithium ion battery first by Sony within 1991, and lithium-ion electric in global range is opened from this
The research boom of pond material.Have energy density high, lightweight and the features such as long lifespan due to lithium ion battery, set as movement
Standby power supply is very popular.But, for lithium ion battery energy density in itself, size and the electrode material kind of its capacity
Class is closely related.Develop high power capacity electrode material be always lithium ion battery worker in global range core work it
One.Graphite is the negative material for being currently widely used in lithium ion battery, only has the theoretical capacity of 372mAh/g due to it, so that
Constrain the energy density of battery.Lithium anode material has very tempting application prospect, because its theoretical capacity density
3650mAh/g is reached, is 10 times of conventional graphite electrodes theoretical capacity, be to set up the lithium-ion battery systems of high-energy-density most
One of good candidate materials.
During li-ion electrode materials are applied to collector, traditional method be using Kynoar (PVDF) with
It is higher that 1-METHYLPYRROLIDONE/oiliness (NMP) or sodium carboxymethylcellulose (CMC) are mixed to get viscosity with water (water solubility)
Solution, and active material evenly spread into above-mentioned solution, then it is carried out into even spread on a current collector.And in body series
In, because lithium metal particle has very big chemical reactivity, can be with the oxygen in surrounding environment, vapor, nitrogen etc.
Generation side reaction causes lithium to lose, and is easily reacted with polar solvent.Therefore, used in lithium metal particle and traditional slurry
Binding agent PVDF, CMC etc. can not be compatible, it is necessary to the solvent for finding replacement carrys out dispersed metal lithium particle, to overcome existing skill
The deficiency of art.
The content of the invention
It is an object of the invention to provide a kind of preparation method of lithium metal even particulate dispersion slurry, with stable in properties non-
Polar solvent constitutes dispersion soln as medium is separated with a small amount of binding agent, and dispersed metal lithium particle can form uniformity preferable
Suspension, and side reaction will not occur cause lithium to lose, method is simple, is easy to large-scale industrialized production.
To achieve these goals, the technical solution adopted by the present invention is as follows：
A kind of preparation method of lithium metal even particulate dispersion slurry, comprises the following steps：
1) under magneton stirring, butadiene-styrene rubber (SBR) is dissolved in non-polar solven, magneton mixing speed is per minute
800 turns, mixing time is 2 hours, butadiene-styrene rubber is completely dissolved in toluene, becomes milky white solution；
2) butadiene-styrene rubber/non-polar solven mixed solution has been transferred in lid narrow-mouthed bottle；
3) lithium metal particle is added to butadiene-styrene rubber/non-polar solven mixed solution, narrow-mouthed bottle is sealed on bottle stopper, and
Sealed with sealing film；
4) narrow-mouthed bottle that will be equipped with lithium metal particle, butadiene-styrene rubber/non-polar solven mixing liquid is placed in Ultrasound Instrument, often
Ultrasonic half an hour is carried out under temperature, the slurry of lithium metal even particulate dispersion is obtained final product, is then shifted in the gloves of argon gas protection
Saved backup in case.
According to above scheme, the butadiene-styrene rubber is 1 with the mass ratio of non-polar solven:49 (i.e. butadiene-styrene rubber quality is dense
Spend for 2%), now the viscosity of mixed liquor is 8 centipoises second (cPs), metallic lithium powder can be dispersed into suspension wherein, protects
Hold not stratified in 10 minutes, be advantageous to slurry coats.When butadiene-styrene rubber mass concentration is 4%, its viscosity reaches 17
Centipoise second (cPs), higher when 6%, 8%, system viscosity is unfavorable for greatly very much the carrying out of coating process.
According to above scheme, the non-polar solven be toluene, to toluene or both arbitrary proportion mixture.
According to above scheme, the lithium metal particle is 3 with the mass ratio of butadiene-styrene rubber/non-polar solven mixed solution:
10, the phosphoric acid obtained under a little proportionings can realize most uniform coating.
The Ultrasound Instrument dispersion steps that the present invention is used, lithium powder is highly stable in the dispersion of SBR/ toluene solutions, 10 minutes according to
It is so homogeneously dispersed state, is very beneficial for coating；If being not added with ultrasonic step, lithium powder is 3 minutes or so in SBR/ toluene solutions
Will fast hierarchical, be unfavorable for slurry coats.
Butadiene-styrene rubber that the present invention is used, non-polar solven toluene are all apolar substance, three to toluene, metallic lithium powder
Person together can stable existence without occur side reaction.Using the ORGANIC SOLVENT MIXTURES of stabilization equably by lithium metal particle
Wherein, the slurry of preparation be able to can make as the medium of even spread on lithium metal particle cathode pole piece in the battery for distribution
Lithium metal even particulate dispersion is to negative material surface, there is provided lithium ion battery is rely the lithium source of charge/discharge operation.
The beneficial effects of the invention are as follows：
The present invention, as dispersion, makes lithium metal particle wherein using butadiene-styrene rubber and toluene (or to toluene) solution
Carry out dispersed and keep not stratified in 10 minutes, enable follow-up material by even spread smoothly complete, pair will not occur
Reaction causes lithium to lose；Method is simple, is easy to large-scale industrialized production.
Specific embodiment
Technical scheme is illustrated with reference to embodiment.
Embodiment 1：
The present invention provides a kind of preparation method of lithium metal even particulate dispersion slurry, comprises the following steps：
1) under magneton stirring, 0.2g butadiene-styrene rubber is dissolved in 9.8g toluene, magneton mixing speed is per minute 800
Turn, mixing time is 2 hours；
2) 10.0g butadiene-styrene rubber/toluene mixed solution has been transferred in lid narrow-mouthed bottle；
3) 3g lithium metal particles are added to butadiene-styrene rubber/toluene mixed solution, narrow-mouthed bottle is sealed on bottle stopper, and with sealing
Mouth diaphragm seal；
4) lithium metal particle, the narrow-mouthed bottle of the mixed solution of butadiene-styrene rubber/toluene be will be equipped with and is placed in ultrasound half in Ultrasound Instrument
Hour, obtain final product lithium metal even particulate dispersion slurry, and shift and saved backup in the glove box of argon gas protection.
Embodiment 2：
The present invention provides a kind of preparation method of lithium metal even particulate dispersion slurry, comprises the following steps：
1) under magneton stirring, 1g butadiene-styrene rubber is dissolved in 49g in toluene, magneton mixing speed is per minute 800
Turn, mixing time is 2 hours；
2) by 50g butadiene-styrene rubber/be transferred in lid narrow-mouthed bottle to the mixed solution of toluene；
3) to butadiene-styrene rubber/add 15g lithium metal particles to the mixed solution of toluene, narrow-mouthed bottle is sealed on bottle stopper,
And sealed with sealing film；
4) lithium metal particle, the narrow-mouthed bottle of the mixed solution of butadiene-styrene rubber/toluene be will be equipped with and is placed in ultrasound half in Ultrasound Instrument
Hour, obtain final product lithium metal even particulate dispersion slurry, and shift and saved backup in the glove box of argon gas protection.
Above example is only used to illustrative and not limiting technical scheme, although above-described embodiment enters to the present invention
Detailed description is gone, the person skilled of this area should be understood：The present invention can be modified or replaced on an equal basis, but
Any modification and local replacement for not departing from spirit and scope of the invention all should be covered in scope of the presently claimed invention.
Claims (4)
1. a kind of preparation method of lithium metal even particulate dispersion slurry, it is characterised in that comprise the following steps：
1) under magneton stirring, butadiene-styrene rubber is dissolved in non-polar solven, magneton mixing speed is 800 turns per minute, is stirred
The time is mixed for 2 hours；
2) butadiene-styrene rubber/non-polar solven mixed solution has been transferred in lid narrow-mouthed bottle；
3) lithium metal particle is added to butadiene-styrene rubber/non-polar solven mixed solution, narrow-mouthed bottle is sealed on bottle stopper, and with sealing
Mouth diaphragm seal；
4) narrow-mouthed bottle that will be equipped with lithium metal particle, butadiene-styrene rubber/non-polar solven mixing liquid is placed in Ultrasound Instrument, under normal temperature
Ultrasonic half an hour is carried out, the slurry of lithium metal even particulate dispersion is obtained final product, is then shifted in the glove box of argon gas protection
Save backup.
2. the preparation method of lithium metal even particulate dispersion slurry according to claim 1, it is characterised in that the butylbenzene
Rubber is 1 with the mass ratio of non-polar solven:49.
3. the preparation method of lithium metal even particulate dispersion slurry according to claim 1, it is characterised in that the non-pole
Property solvent include toluene, to toluene or both arbitrary proportion mixture.
4. the preparation method of lithium metal even particulate dispersion slurry according to claim 1, it is characterised in that the metal
Lithium particle is 3 with the mass ratio of butadiene-styrene rubber/non-polar solven mixed solution:10.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611168980.1A CN106731927A (en) | 2016-12-16 | 2016-12-16 | A kind of preparation method of lithium metal even particulate dispersion slurry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611168980.1A CN106731927A (en) | 2016-12-16 | 2016-12-16 | A kind of preparation method of lithium metal even particulate dispersion slurry |
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| CN106731927A true CN106731927A (en) | 2017-05-31 |
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| CN201611168980.1A Pending CN106731927A (en) | 2016-12-16 | 2016-12-16 | A kind of preparation method of lithium metal even particulate dispersion slurry |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101388453A (en) * | 2007-09-13 | 2009-03-18 | 深圳市比克电池有限公司 | Electrode slurry dispersing method |
| CN103918108A (en) * | 2011-10-05 | 2014-07-09 | 加州大学校务委员会 | Lithium metal doped electrodes for lithium-ion rechargeable chemistry |
| CN105932282A (en) * | 2016-06-08 | 2016-09-07 | 湖南锂顺能源科技有限公司 | Lithium ion battery and preparation method thereof |
-
2016
- 2016-12-16 CN CN201611168980.1A patent/CN106731927A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101388453A (en) * | 2007-09-13 | 2009-03-18 | 深圳市比克电池有限公司 | Electrode slurry dispersing method |
| CN103918108A (en) * | 2011-10-05 | 2014-07-09 | 加州大学校务委员会 | Lithium metal doped electrodes for lithium-ion rechargeable chemistry |
| CN105932282A (en) * | 2016-06-08 | 2016-09-07 | 湖南锂顺能源科技有限公司 | Lithium ion battery and preparation method thereof |
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| PB01 | Publication | ||
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170531 |