CN108493387A - Battery diaphragm coating bonding agent and preparation method thereof - Google Patents
Battery diaphragm coating bonding agent and preparation method thereof Download PDFInfo
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- CN108493387A CN108493387A CN201810368741.3A CN201810368741A CN108493387A CN 108493387 A CN108493387 A CN 108493387A CN 201810368741 A CN201810368741 A CN 201810368741A CN 108493387 A CN108493387 A CN 108493387A
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
-
- 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
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- Chemical Kinetics & Catalysis (AREA)
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- Engineering & Computer Science (AREA)
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- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention relates to a kind of battery diaphragm coating bonding agent and preparation method thereof, the bonding agent includes using vinyl POSS as core, and hydrophilic polymer is the nucleocapsid high molecular polymer of shell；Preparation method is by making the emulsion polymerization of vinyl POSS and hydrophilic polymer monomer, it is grown on vinyl POSS with hydrophilic polymer segment, it is formed using vinyl POSS as core, hydrophilic polymer is the hydrophily battery diaphragm coating bonding agent with bonding effect of shell.The bonding agent is used for lithium battery ceramic diaphragm, diaphragm imbibition/liquid-keeping property can be effectively improved, and effectively inhibit falling off for ceramic powder；After diaphragm is assembled into battery, battery has many advantages, such as that cycle performance is superior, ionic conductivity is high, high rate performance is excellent.
Description
Technical field
The invention belongs to technical field of lithium ion more particularly to a kind of battery diaphragm coating bonding agent and its preparations
Method.
Background technology
Diaphragm is the important composition component of lithium ion battery, and the performance of diaphragm determines the interfacial structure of battery, internal resistance etc.,
And the capacity, cycle performance and safety etc. for directly affecting battery.Ceramic diaphragm is developed on traditional polyalkene diaphragm
The modern high security diaphragm material come, the main preparation method of ceramic diaphragm is by inorganic particle (such as Al2O3、SiO2、TiO2
Deng), bonding agent etc. is dispersed in solvent, then forms ceramic painting in polyalkene diaphragm substrate surface by the tape casting or infusion process
Layer.The thermal contraction performance of ceramic diaphragm, to the imbibition rate of electrolyte, wellability and apply ceramic diaphragm lithium battery from
Electron conductivity, capacity is kept and high rate performance is influenced by inorganic particle, bonding agent and manufacture craft.
Include at present inorganic particle and its manufacture craft and bonding agent to the main direction of studying of ceramic diaphragm coating
Modified and synthesis, such as a kind of lithium battery diaphragm coating boehmites announced of patent CN106186008A and its hydro-thermal preparation side
Method, patent CN103560219A disclose a kind of using poly-dopamine as the preparation method of the ceramic diaphragm of bonding agent.
Wherein, traditional bonding agent, such as Kynoar, Kynoar-hexafluoropropene, although possessing good machine
Tool performance, chemical resistance, cementability, but due to the hydrophobicity of itself, in diaphragm wellability, the chemical property side of battery
There is the space of promotion in face；Such as poly- polymethacrylic acid methyl ester bonding agent, though having certain absorbency, adhesive property is bad, holds
Falling off for diaphragm ceramic powders is easily led to, safety problem occurs so as to cause battery.Therefore, it certainly will need to existing bonding agent
It is modified processing.
Invention content
It is an object of the invention to：For existing cell ceramic diaphragm bonding agent hydrophily is poor, cementability is weak and causes
Ceramic diaphragm wellability is poor, the problems such as ceramic powders are easy to fall off, providing a kind of having high-hydrophilic, high adhesiveness, high electrification
Learn stable battery diaphragm coating bonding agent and its preparation process.
To achieve the goals above, the present invention uses following technical scheme：
A kind of battery diaphragm coating bonding agent, the bonding agent include using vinyl-POSS as core, and hydrophilic polymer is
The nucleocapsid high molecular polymer of shell.
Wherein, the inorganic core (SiO that polyhedral oligomeric silsesquioxane (POSS) is made of silicon (Si), oxygen (O)3/2)nWith
There is the organic/inorganic hybridization material that horn collectively forms, there is nanometer size effect, inorganic core to assign the good thermostabilization of material
Property and mechanicalness, as CN105670004A announce a kind of POSS bases nano hybridization micella preparation method.For acrylic acid, third
For the vinyl hydrophilic polymer monomer such as alkene nitrile, it can be grown on vinyl silsesquioxane by emulsion polymerization hydrophilic
Macromolecular chain, to realize the compounding design of spherical nucleocapsid high molecular weight hydrophilic polymer, if vinyl-POSS is core,
Shell is the nucleocapsid high molecular polymer of polyacrylonitrile, and periphery possesses many polar groups, can form multiple spot bonding, still
Such as the tentacle of octopus, well by diaphragm coating ceramic particle and basement membrane bond together.
Wherein, the preparation method of the battery diaphragm coating bonding agent, includes the following steps：
Step (1)：Prepare the mixed solution of initiator, emulsifier, vinyl-POSS：By weight by initiator, emulsifier
Compare 0.02-0.05:2-4 is added in the deionized water of 100-150ml, and it is water-soluble to add the sodium hydroxide that mass fraction is 5%
Vinyl-POSS monomers are added to alkalescent in liquid tune PH after being completely dissolved, wherein vinyl-POSS is with initiator weight ratio
0.02-0.03:0.04-0.09；
Step (2)：The preparation of vinyl-POSS/ hydrophilic polymer nucleocapsids：Under suitable mixing speed, Xiang Bu
Suddenly hydrophilic polymer monomer is added in (1) mixed solution, wherein vinyl-POSS is 2- with hydrophilic polymer monomer weight ratio
4:200-600；Then at 85~90 DEG C, isothermal reaction 4~8 hours；
Step (3)：After the completion of step (2) reaction, 30~40 DEG C are cooled to, is demulsified, be filtered, washed, dried with concentrated hydrochloric acid
Obtain the vinyl-POSS/ hydrophilic polymer nucleocapsid high molecular polymers of white powder.
Preferably, in step (1), the initiator is azodiisobutyronitrile, sodium peroxydisulfate, in ammonium persulfate at least
It is a kind of.
Preferably, in step (1), the emulsifier is odium stearate, lauryl sodium sulfate, dodecyl benzene sulfonic acid
At least one of sodium.
Preferably, in step (1), the vinyl-POSS is pentahedron vinyl-POSS, hexahedron vinyl-
At least one of POSS, octahedra vinyl-POSS.
Preferably, in step (2), the hydrophilic polymer monomer is at least one of acrylic acid, acrylonitrile.
Preferably, in step (3), the weight of the vinyl-POSS/ hydrophilic polymer nucleocapsid high molecular polymers
Average molecular weight is 100000~150000.
Compared with the prior art, by the present invention in that the emulsion polymerization of vinyl-POSS and hydrophilic polymer monomer,
It is grown on vinyl-POSS with hydrophilic polymer segment, is formed using vinyl-POSS as core, hydrophilic polymer
For the hydrophily battery diaphragm coating bonding agent with bonding effect of shell, which is used for lithium battery ceramic diaphragm,
Diaphragm imbibition/liquid-keeping property can be effectively improved, and effectively inhibits falling off for ceramic powder；After diaphragm is assembled into battery, battery
Have many advantages, such as that cycle performance is superior, ionic conductivity is high, high rate performance is excellent.
Specific implementation mode
To keep technical scheme of the present invention and advantage clearer, below in conjunction with specific embodiment, to the skill of the present invention
Art scheme is clearly and completely described, it is clear that and described embodiments are some of the embodiments of the present invention, rather than all
Embodiment.Based on the embodiments of the present invention, those of ordinary skill in the art institute without creative efforts
The every other embodiment obtained, shall fall within the protection scope of the present invention.
Embodiment 1
By sodium peroxydisulfate, lauryl sodium sulfate by weight 0.04：3 are added in 150ml deionized waters, add matter
It is that 5% sodium hydrate aqueous solution adjusts pH to 8 to measure score；Then hexahedron vinyl-POSS is added, wherein hexahedron ethylene
Base-POSS is 0.02 with sodium peroxydisulfate weight ratio:0.04；Under stirring appropriate, addition is with vinyl-POSS weight ratios
250:1 acrylic acid；Then isothermal reaction 4 hours at 90 DEG C after the completion of reaction, are cooled to 40 DEG C, with concentrated hydrochloric acid demulsification, mistake
Filter, wash, being dried to obtain the hexahedron vinyl-POSS/ polyacrylic acid nucleocapsid polymer bonding agent of white powder.
By bonding agent powder, alundum (Al2O3) nano-particle, carboxymethyl cellulose by weight 5:1:90 be added to it is water-soluble
In liquid, the mixed solution that solid content is 50% is made, mixes 1h under 20000 rotating speeds, obtains coating slurry.Using blade coating side
Slurry is applied to polypropylene diaphragm surface by formula, and the lithium battery ceramic diaphragm coating of 5 μ m-thicks is obtained after 80 DEG C of dryings, is fully infiltrated
LiPF6Electrolyte uses electrochemical workstation to test its surface lithium ion conductivity as 3.9 × 10-3Scm-1, coating adhesion is
41Nm-1；It is assembled into LiFePO4/ C lithium batteries.Its cycle performance is tested using electrochemical workstation, after 400 circle of cycle, still
Keep 92% initial discharge capacity；Sample as a comparison, by Kynoar, carboxymethyl cellulose, alundum (Al2O3) nano-particle
Slurry and coating are prepared according to same ratio, it is 5.7 × 10 to measure its surface lithium ion conductivity-4Scm-1, coating adhesion is
21Nm-1, after 400 circle of cycle, capacity retention ratio is only 79%.
Embodiment 2
By azodiisobutyronitrile, neopelex by weight 0.02：3 are added in 120ml deionized waters, then
It is that 5% sodium hydrate aqueous solution adjusts pH to 8 that mass fraction, which is added,；Then pentahedron vinyl-POSS, wherein pentahedron is added
Vinyl-POSS is 0.03 with azodiisobutyronitrile weight ratio:0.05；Under stirring appropriate, it is added and vinyl-POSS weights
Amount is than being 300:1 acrylonitrile；Then isothermal reaction 6 hours at 70 DEG C after the completion of reaction, are cooled to 35 DEG C, use concentrated hydrochloric acid
Be demulsified, be filtered, washed, being dried to obtain white powder pentahedron vinyl-POSS/ polyacrylonitrile nucleocapsid structural polymers it is viscous
Connect agent.
By bonding agent powder, alundum (Al2O3) nano-particle, hydroxypropyl methyl cellulose by weight 5:2:90 are added to
In aqueous solution, the mixed solution that solid content is 45% is made, mixes 1h under 15000 rotating speeds, obtains coating slurry.Using scraping
Slurry is applied to polypropylene diaphragm surface by painting mode, the lithium battery ceramic diaphragm coating of 5 μ m-thicks is obtained after 60 DEG C of dryings, fully
Infiltrate LiPF6Electrolyte uses electrochemical workstation to test its surface lithium ion conductivity as 3.6 × 10-3Scm-1, coating attachment
Power is 43Nm-1；It is assembled into LiFePO4/ C lithium batteries.Its cycle performance is tested using electrochemical workstation, after 400 circle of cycle,
Still keep 93% initial discharge capacity；Sample as a comparison, by polymethyl methacrylate, hydroxypropyl methyl cellulose, three
Al 2 O nano-particle prepares slurry and coating according to same ratio, and it is 5.7 × 10 to measure its surface lithium ion conductivity- 4Scm-1, coating adhesion 15Nm-1, after 400 circle of cycle, capacity retention ratio is only 80%.
Embodiment 3
By ammonium persulfate, odium stearate by weight 0.03：2.5 are added in 130ml deionized waters, add quality point
Number is that 5% sodium hydrate aqueous solution adjusts pH to 7.5；Then octahedra vinyl-POSS is added, wherein octahedra vinyl-
POSS is 0.03 with ammonium persulfate weight ratio:0.08；Under stirring appropriate, it is 300 to be added with vinyl POSS weight ratios:1
Acrylic acid；Isothermal reaction 5 hours at 80 DEG C after the completion of reaction, are cooled to 30 DEG C, be demulsified, be filtered, washed with concentrated hydrochloric acid,
It is dried to obtain the octahedra vinyl-POSS/ polyacrylic acid nucleocapsid polymer bonding agent of white powder.
By bonding agent powder, titanium dioxide nano-particle, hydroxypropyl methyl cellulose by weight 6:2:90 are added to water
In solution, the mixed solution that solid content is 45% is made, mixes 2h under 20000 rotating speeds, obtains coating slurry.Using blade coating
Slurry is applied to polypropylene diaphragm surface by mode, and the lithium battery ceramic diaphragm coating of 5 μ m-thicks is obtained after 80 DEG C of dryings, is fully soaked
Moisten LiPF6Electrolyte uses electrochemical workstation to test its surface lithium ion conductivity as 3.7 × 10-3Scm-1, coating adhesion
For 42Nm-1；It is assembled into LiFePO4/ C lithium batteries.Its cycle performance is tested using electrochemical workstation, after 400 circle of cycle, according to
The initial discharge capacity of old holding 91%；Sample as a comparison, Kynoar-hexafluoropropylene copolymer, hydroxypropyl methyl is fine
Dimension element, titanium dioxide nano-particle prepare slurry and coating according to same ratio, measure its surface lithium ion conductivity be 4.1 ×
10-4Scm-1, coating adhesion 22Nm-1, after 400 circle of cycle, capacity retention ratio is only 78%.
Embodiment 4
By sodium peroxydisulfate, odium stearate by weight 0.05：4 are added in 150ml deionized waters, add mass fraction
PH to 7.5 is adjusted for 5% sodium hydrate aqueous solution；Then hexahedron vinyl-POSS is added, wherein hexahedron vinyl-
POSS is 0.03 with sodium peroxydisulfate weight ratio:0.09；Under stirring appropriate, it is added and octahedra vinyl-POSS weight ratios
It is 250:1 acrylic acid；Isothermal reaction 5 hours at 75 DEG C after the completion of reaction, are cooled to 35 DEG C, with concentrated hydrochloric acid demulsification, mistake
Filter, wash, being dried to obtain the octahedra vinyl-POSS/ polyacrylic acid nucleocapsid polymer bonding agent of white powder.
By bonding agent powder, titanium dioxide nano-particle, hydroxypropyl methyl cellulose by weight 5:3:90 are added to water
In solution, the mixed solution that solid content is 46% is made, mixes 2.5h under 15000 rotating speeds, obtains coating slurry.Using scraping
Slurry is applied to polypropylene diaphragm surface by painting mode, the lithium battery ceramic diaphragm coating of 5 μ m-thicks is obtained after 70 DEG C of dryings, fully
Infiltrate LiPF6Electrolyte uses electrochemical workstation to test its surface lithium ion conductivity as 3.8 × 10-3Scm-1, coating attachment
Power is 47Nm-1；It is assembled into LiFePO4/ C lithium batteries.Its cycle performance is tested using electrochemical workstation, after 400 circle of cycle,
Still keep 92% initial discharge capacity；Sample as a comparison, by polymethyl methacrylate, hydroxypropyl methyl cellulose, two
Titanium oxide nanoparticles prepare slurry and coating according to same ratio, and it is 5.1 × 10 to measure its surface lithium ion conductivity-4Scm-1, coating adhesion 16Nm-1, after 400 circle of cycle, capacity retention ratio is only 78%.
According to the disclosure and teachings of the above specification, those skilled in the art in the invention can also be to above-mentioned embodiment party
Formula is changed and is changed.Therefore, the invention is not limited in above-mentioned specific implementation mode, every those skilled in the art exist
Made any conspicuously improved, replacement or modification all belongs to the scope of protection of the present invention on the basis of the present invention.This
Outside, although having used some specific terms in this specification, these terms are merely for convenience of description, not to the present invention
Constitute any restrictions.
Claims (7)
1. a kind of battery diaphragm coating bonding agent, it is characterised in that：The bonding agent includes the parent using vinyl-POSS as core
Aqueous polymer is the nucleocapsid high molecular polymer of shell.
2. a kind of preparation method of battery diaphragm coating bonding agent according to claim 1, which is characterized in that including with
Lower step：
Step (1)：Prepare the mixed solution of initiator, emulsifier, vinyl-POSS：By weight by initiator, emulsifier
0.02-0.05:2-4 is added in the deionized water of 100~150ml, adds the sodium hydrate aqueous solution that mass fraction is 5%
It adjusts pH to alkalescent, vinyl-POSS is added after being completely dissolved, wherein vinyl-POSS is 0.02- with initiator weight ratio
0.03:0.04-0.09；
Step (2)：The preparation of vinyl-POSS/ hydrophilic polymer nucleocapsids：Under stiring, to the mixed solution of step (1)
Middle addition hydrophilic polymer monomer, wherein vinyl-POSS is 2-4 with hydrophilic polymer monomer weight ratio:200-600；Then
At 85~90 DEG C, isothermal reaction 4~8 hours；
Step (3)：After the completion of step (2) reaction, 30~40 DEG C are cooled to, is demulsified, be filtered, washed, is dried to obtain with concentrated hydrochloric acid
Vinyl-POSS/ hydrophilic polymer nucleocapsid the high molecular polymers of white powder.
3. the preparation method of battery diaphragm coating bonding agent according to claim 2, it is characterised in that：In step (1),
The initiator is at least one of azodiisobutyronitrile, sodium peroxydisulfate, ammonium persulfate.
4. the preparation method of battery diaphragm coating bonding agent according to claim 2, it is characterised in that：In step (1),
The emulsifier is at least one of odium stearate, lauryl sodium sulfate, neopelex.
5. the preparation method of battery diaphragm coating bonding agent according to claim 2, it is characterised in that：In step (1),
Vinyl-the POSS is pentahedron vinyl-POSS, in hexahedron vinyl-POSS, octahedra vinyl-POSS
It is at least one.
6. the preparation method of battery diaphragm coating bonding agent according to claim 2, it is characterised in that：In step (2),
The hydrophilic polymer monomer is at least one of acrylic acid, acrylonitrile.
7. the preparation method of battery diaphragm coating bonding agent according to claim 2, it is characterised in that：In step (3),
The weight average molecular weight of the vinyl-POSS/ hydrophilic polymer nucleocapsid high molecular polymers is 100000~150000.
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| CN201810368741.3A CN108493387B (en) | 2018-04-23 | 2018-04-23 | Adhesive for battery diaphragm coating and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112341961A (en) * | 2020-10-28 | 2021-02-09 | 欣旺达电动汽车电池有限公司 | Adhesive, diaphragm and preparation method thereof |
| WO2021189399A1 (en) * | 2020-03-27 | 2021-09-30 | 宁德新能源科技有限公司 | Separator, electrode assembly, battery, and electronic device |
| CN113795975A (en) * | 2020-03-31 | 2021-12-14 | 宁德新能源科技有限公司 | Separator, electrode assembly, battery, and electronic device |
| CN114520329A (en) * | 2020-11-19 | 2022-05-20 | 比亚迪股份有限公司 | Adhesive, preparation method thereof and slurry |
| JP2022545913A (en) * | 2019-12-03 | 2022-11-01 | 寧徳時代新能源科技股▲分▼有限公司 | SECONDARY BATTERY, DEVICE CONTAINING SECONDARY BATTERY, METHOD FOR MANUFACTURING SECONDARY BATTERY, AND ADHESIVE COMPOSITION |
| WO2024119286A1 (en) * | 2022-12-05 | 2024-06-13 | 宁德时代新能源科技股份有限公司 | Polymer, separator film, and secondary battery and electrical apparatus related thereto |
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| CN114520329A (en) * | 2020-11-19 | 2022-05-20 | 比亚迪股份有限公司 | Adhesive, preparation method thereof and slurry |
| WO2024119286A1 (en) * | 2022-12-05 | 2024-06-13 | 宁德时代新能源科技股份有限公司 | Polymer, separator film, and secondary battery and electrical apparatus related thereto |
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