CN109273645A - High-temperature-reslithium lithium battery diaphragm and preparation method thereof - Google Patents
High-temperature-reslithium lithium battery diaphragm and preparation method thereof Download PDFInfo
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- CN109273645A CN109273645A CN201811120005.2A CN201811120005A CN109273645A CN 109273645 A CN109273645 A CN 109273645A CN 201811120005 A CN201811120005 A CN 201811120005A CN 109273645 A CN109273645 A CN 109273645A
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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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
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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
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- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
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Abstract
The invention proposes a kind of high-temperature-reslithium lithium battery diaphragms and preparation method thereof, including following components: 10~20 parts of polyester polyol, 25~35 parts of polyether polyol, 1~3 part of nano zircite, 0.6~2.4 part of graphene oxide, 2~6 parts of citric acid, 0.5~1 part of foaming agent, 0.5~1 part of catalyst, 0.5~1 part of stabilizer and 30~36 parts of isocyanates.Preparation method: 1) weighing the component in addition to isocyanates according to the weight ratio and pour into mixing plant, is uniformly mixed, obtains mixture A；2) isocyanates is weighed according to the weight ratio, mixture A and isocyanates are put into respectively in the A material cylinder and B material cylinder of polyurethane foams, after polyurethane foaming machine stirs, is poured into rectangle or square mold, foaming；3) bulk product of step 2) foaming is cut into punch forming.The battery diaphragm has the advantages that high porosity and low thickness, and there are also preferable low-temperature ion conductivity.
Description
Technical field
The invention belongs to technical field of lithium batteries, and in particular to a kind of high-temperature-reslithium lithium battery diaphragm and preparation method thereof.
Background technique
Lithium ion battery is high with its energy density, has extended cycle life the electrical property excellent with voltage height etc. and obtains rapidly
Development, have been widely used for the fields such as mobile phone, portable computer, camera, video camera, electric car, Er Qieying at present
With field still among continuous extension.Lithium ion battery is composed of positive and negative electrodes, electrolyte and separator.Diaphragm is lithium ion battery
One of layer assembly in key, major function is isolation positive and negative anodes and electronics is prevented to pass through, while ion can allow for pass through, thus
Complete the quick transmission in lithium ion in charge and discharge process between positive and negative anodes.
Make since the superiority and inferiority of membrane properties directly affects the internal resistance of cell, discharge capacity, service life cycle and battery
Security performance, thus lithium battery manufacture it is high to diaphragm material product requirement, such as thickness, superficial density, mechanical property this
There is very high requirement a bit.
Existing, lithium ion battery separator material is mainly polyalkene diaphragm such as single-layer polypropylene (PP) microporous barrier, single layer
Polyethylene (PE) microporous barrier and three layers of PP/PE/PP composite membrane, such diaphragm preparation method be mainly dry method tension pore method and
Wet process phase separation method.Polyalkene diaphragm drawback is: one, easily shrinking when polyalkene diaphragm is heated, will cause diaphragm size shakiness
Fixed, positive and negative anodes directly contact and short-circuit；Two, closed pore temperature and broken film temperature are lower, when the situations such as battery puncture occur, battery
It is internal highly exothermic, cause diaphragm to melt contraction completely, battery short circuit generates high temperature until battery disintegrates or explodes.These drawbacks
It is to be determined by polyolefine material self-characteristic, PE fusing point is 128~135 DEG C, and PP fusing point is 150~166 DEG C.Three, it makes
Complex process, at high cost, the disadvantages such as compressive property is low.In addition, diaphragm currently on the market it is all simple play simple isolation
Effect, under identical aperture, not any help of the raising to lithium ion conductivity.
Summary of the invention
The present invention proposes that a kind of high-temperature-reslithium lithium battery diaphragm, the battery diaphragm have the advantages that high porosity and low thickness,
There are also preferable low-temperature ion conductivity.
The technical scheme of the present invention is realized as follows:
A kind of high-temperature-reslithium lithium battery diaphragm, the component including following parts by weight:
10~20 parts of polyester polyol, 25~35 parts of polyether polyol, 1~3 part of nano zircite, graphene oxide 0.6
~2.4 parts, 2~6 parts of citric acid, 0.5~1 part of foaming agent, 0.5~1 part of catalyst, 0.5~1 part of stabilizer and isocyanates 30
~36 parts；The polyether polyol is the polyether polyol that degree of functionality is 2-3, and the isocyanates is that degree of functionality is the different of 2-3
Cyanate.
Preferably, the polyester polyol is polycarbonate glycol.
Preferably, the foaming agent is the mixture that the foaming agent is water, pentane and carbon dioxide.
Preferably, the catalyst is solid ammonia.
Preferably, the stabilizer is silicone oil.
Preferably, the isocyanates is selected from toluene diisocyanate and/or methyl diphenylene diisocyanate.
It is a further object to provide a kind of preparation methods of high-temperature-reslithium lithium battery diaphragm, comprising the following steps:
1) weigh according to the weight ratio polyester polyol, polyether polyol, nano zircite, graphene oxide, citric acid,
Foaming agent, catalyst and stabilizer pour into mixing plant, are uniformly mixed, obtain mixture A；
2) isocyanates is weighed according to the weight ratio, and mixture A and isocyanates are put into polyurethane foams respectively
A material cylinder and B material cylinder in, after polyurethane foaming machine stirs, be poured into rectangle or square mold, foaming；
3) bulk product of step 2) foaming is placed on special foam pingqie machine, is sliced by thickness requirement,
Again by sheet material specification requirement punch forming by size.
Preferably, for the thickness of the high-temperature-reslithium lithium battery diaphragm at 8~40 μm, porosity is 76~81%.
Preferably, the polyurethane foaming machine A expects 460~560 revs/min of revolution speed, and B expects 350~450 turns of revolution speed；
1600~2000 revs/min of speed of agitator；200~3100 Grams Per Second of material feeding；40~50 degree of mold temperature；7~10 points of foamed time
Clock.
Beneficial effects of the present invention:
High-temperature-reslithium lithium battery diaphragm of the invention be on the basis of using for reference former successful experience, using polyester polyol,
Polyether polyol and isocyanates add nano zircite, graphene oxide and citric acid while preparing diaphragm, is added and is used as
Add agent, not only improve high temperature resistance, also improve low-temperature ion conductivity, solve conventional membrane it is all simple play it is simple
Buffer action and promotion conductive effect cannot be played.
Specific embodiment
Embodiment 1
A kind of high-temperature-reslithium lithium battery diaphragm, the component including following parts by weight:
16 parts of polycarbonate glycol, 30 parts of polyether polyol, 2 parts of nano zircite, 1.8 parts of graphene oxide, citric acid 4
Part, 0.8 part of foaming agent, solid 0.7 part of ammonia, 0.7 part of silicone oil and 33 parts of toluene diisocyanate；Polyether polyol is that degree of functionality is 2
Polyether polyol, foaming agent are the mixture of water, pentane and carbon dioxide.
The preparation method of high-temperature-reslithium lithium battery diaphragm, comprising the following steps:
1) polycarbonate glycol, polyether polyol, nano zircite, graphene oxide, lemon are weighed according to the weight ratio
Acid, foaming agent, solid ammonia and stabilizer pour into mixing plant, are uniformly mixed, obtain mixture A；
2) toluene diisocyanate is weighed according to the weight ratio, and mixture A and toluene diisocyanate are put into poly- ammonia respectively
In the A material cylinder and B material cylinder of ester foaming agent, after polyurethane foaming machine stirs, it is poured into rectangle or square mold, foaming
Molding；Polyurethane foaming machine A expects 500 revs/min of revolution speed, and B expects 410 turns of revolution speed；1800 revs/min of speed of agitator；Material feeding
1300 Grams Per Seconds；45 degree of mold temperature；Foamed time 8 minutes.
3) bulk product of step 2) foaming is placed on special foam pingqie machine, is sliced by thickness requirement,
Again by sheet material specification requirement punch forming by size.
The thickness of high-temperature-reslithium lithium battery diaphragm is at 16 μm, porosity 78%, air permeability 28sec/100cc, resistance to compression
Rebound degree is 1.5 × 10 in 95% or more, -15 DEG C of conductivity-3S/cm。
Embodiment 2
A kind of high-temperature-reslithium lithium battery diaphragm, the component including following parts by weight:
10 parts of polycarbonate glycol, 35 parts of polyether polyol, 1 part of nano zircite, 0.6 part of graphene oxide, citric acid 2
Part, 0.5 part of foaming agent, solid 0.5 part of ammonia, 0.5 part of silicone oil and 30 parts of methyl diphenylene diisocyanate；Polyether polyol is function
The polyether polyol that degree is 3, foaming agent are the mixture of water, pentane and carbon dioxide.
The preparation method of high-temperature-reslithium lithium battery diaphragm, comprising the following steps:
1) polycarbonate glycol, polyether polyol, nano zircite, graphene oxide, lemon are weighed according to the weight ratio
Acid, foaming agent, solid ammonia and stabilizer pour into mixing plant, are uniformly mixed, obtain mixture A；
2) methyl diphenylene diisocyanate is weighed according to the weight ratio, by mixture A and diphenylmethane diisocyanate
Ester put into respectively polyurethane foams A material cylinder and B material cylinder in, after polyurethane foaming machine stirs, be poured into rectangle or
In square mold, foaming；Polyurethane foaming machine A expects 460 revs/min of revolution speed, and B expects 450 turns of revolution speed；Speed of agitator
1600 revs/min；200 Grams Per Second of material feeding；40 degree of mold temperature；Foamed time 10 minutes.
3) bulk product of step 2) foaming is placed on special foam pingqie machine, is sliced by thickness requirement,
Again by sheet material specification requirement punch forming by size.
The thickness of high-temperature-reslithium lithium battery diaphragm is at 8 μm, porosity 76%, air permeability 25sec/100cc, and resistance to compression is returned
Bullet rate is 1.1 × 10 in 95% or more, -15 DEG C of conductivity-3S/cm。
Embodiment 3
A kind of high-temperature-reslithium lithium battery diaphragm, the component including following parts by weight:
20 parts of polycarbonate glycol, 25 parts of polyether polyol, 3 parts of nano zircite, 2.4 parts of graphene oxide, citric acid 6
Part, 1 part of foaming agent, solid 1 part of ammonia, 1 part of silicone oil and 36 parts of isocyanates；Polyether polyol is the polyether polyol that degree of functionality is 2,
Isocyanates is toluene diisocyanate and methyl diphenylene diisocyanate, and foaming agent is the mixed of water, pentane and carbon dioxide
Close object.
The preparation method of high-temperature-reslithium lithium battery diaphragm, comprising the following steps:
1) polycarbonate glycol, polyether polyol, nano zircite, graphene oxide, lemon are weighed according to the weight ratio
Acid, foaming agent, solid ammonia and silicone oil pour into mixing plant, are uniformly mixed, obtain mixture A；
2) isocyanates is weighed according to the weight ratio, and mixture A and isocyanates are put into polyurethane foams respectively
A material cylinder and B material cylinder in, after polyurethane foaming machine stirs, be poured into rectangle or square mold, foaming；It is poly-
Urethane foaming machine A expects 560 revs/min of revolution speed, and B expects 350 turns of revolution speed；2000 revs/min of speed of agitator；3100 grams of material feeding/
Second；50 degree of mold temperature；Foamed time 7 minutes.
3) bulk product of step 2) foaming is placed on special foam pingqie machine, is sliced by thickness requirement,
Again by sheet material specification requirement punch forming by size.
The thickness of high-temperature-reslithium lithium battery diaphragm is at 40 μm, porosity 81%, air permeability 33sec/100cc, resistance to compression
Rebound degree is 2.1 × 10 in 95% or more, -15 DEG C of conductivity-3S/cm。
Comparative example 1
A kind of lithium battery diaphragm, the component including following parts by weight:
46 parts of polyether polyol, 1.8 parts of graphene oxide, 4 parts of citric acid, 0.8 part of foaming agent, solid 0.7 part of ammonia, silicone oil
0.7 part and 35 parts of toluene diisocyanate；Polyether polyol is the polyether polyol that degree of functionality is 2, foaming agent be water, pentane and
The mixture of carbon dioxide.
Preparation method is substantially the same manner as Example 1, the difference is that the content of each component.
The thickness of the lithium battery diaphragm is at 20 μm, porosity 67%, air permeability 21sec/100cc, resistance to compression rebound
Rate is 1.2 × 10 in 90% or more, -15 DEG C of conductivity-3S/cm。
Comparative example 2
A kind of lithium battery diaphragm, the component including following parts by weight:
10 parts of polycarbonate glycol, 35 parts of polyether polyol, 1.6 parts of nano zircite, 0.5 part of foaming agent, solid ammonia 0.5
Part, 0.5 part of silicone oil and 32 parts of methyl diphenylene diisocyanate；Polyether polyol is the polyether polyol that degree of functionality is 3, foaming
Agent is the mixture of water, pentane and carbon dioxide.
Preparation method is substantially the same manner as Example 2, the difference is that the content of each component.
The thickness of lithium battery diaphragm is at 10 μm, porosity 73%, air permeability 23sec/100cc, resistance to compression rebound degree
It is 2.6 × 10 in 93% or more, -15 DEG C of conductivity-4S/cm。
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of high-temperature-reslithium lithium battery diaphragm, which is characterized in that the component including following parts by weight:
10~20 parts of polyester polyol, 25~35 parts of polyether polyol, 1~3 part of nano zircite, graphene oxide 0.6~2.4
Part, 2~6 parts of citric acid, 0.5~1 part of foaming agent, 0.5~1 part of catalyst, 0.5~1 part of stabilizer and isocyanates 30~36
Part；The polyether polyol is the polyether polyol that degree of functionality is 2-3, and the isocyanates is the isocyanic acid that degree of functionality is 2-3
Ester.
2. high-temperature-reslithium lithium battery diaphragm according to claim 1, which is characterized in that the polyester polyol is polycarbonate
Glycol.
3. high-temperature-reslithium lithium battery diaphragm according to claim 1, which is characterized in that the foaming agent is that the foaming agent is
The mixture of water, pentane and carbon dioxide.
4. high-temperature-reslithium lithium battery diaphragm according to claim 1, which is characterized in that the catalyst is solid ammonia.
5. high-temperature-reslithium lithium battery diaphragm according to claim 1, which is characterized in that the stabilizer is silicone oil.
6. according to claim 1 to high-temperature-reslithium lithium battery diaphragm described in 5 any one, which is characterized in that the isocyanates
Selected from toluene diisocyanate and/or methyl diphenylene diisocyanate.
7. the preparation method of high-temperature-reslithium lithium battery diaphragm as described in claim 1, which comprises the following steps:
1) polyester polyol, polyether polyol, nano zircite, graphene oxide, citric acid, foaming are weighed according to the weight ratio
Agent, catalyst and stabilizer pour into mixing plant, are uniformly mixed, obtain mixture A；
2) isocyanates is weighed according to the weight ratio, and mixture A and the isocyanates A for putting into polyurethane foams respectively are expected
In cylinder and B material cylinder, after polyurethane foaming machine stirs, it is poured into rectangle or square mold, foaming；
3) bulk product of step 2) foaming is placed on special foam pingqie machine, is sliced by thickness requirement, then will
Sheet material specification requirement punch forming by size.
8. the preparation method of high-temperature-reslithium lithium battery diaphragm according to claim 7, which is characterized in that the high temperature resistant lithium electricity
For the thickness of pond diaphragm at 8~40 μm, porosity is 76~81%.
9. the preparation method of high-temperature-reslithium lithium battery diaphragm according to claim 7, which is characterized in that the polyurethane foam
Machine A expects 460~560 revs/min of revolution speed, and B expects 350~450 turns of revolution speed；1600~2000 revs/min of speed of agitator；Material feeding
200~3100 Grams Per Seconds；40~50 degree of mold temperature；Foamed time 7~10 minutes.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811120005.2A CN109273645A (en) | 2018-09-25 | 2018-09-25 | High-temperature-reslithium lithium battery diaphragm and preparation method thereof |
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| CN201811120005.2A CN109273645A (en) | 2018-09-25 | 2018-09-25 | High-temperature-reslithium lithium battery diaphragm and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111081954A (en) * | 2019-11-22 | 2020-04-28 | 东莞东阳光科研发有限公司 | Diaphragm coating slurry, diaphragm and preparation method thereof |
| EP4369452A1 (en) * | 2022-11-11 | 2024-05-15 | AESC Japan Ltd. | Secondary battery and preparation method thereof |
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| CN104638220A (en) * | 2015-02-11 | 2015-05-20 | 中材科技股份有限公司 | Environment-friendly high-performance ceramic coating lithium ion battery diaphragm and preparation method thereof |
| CN104916803A (en) * | 2015-07-03 | 2015-09-16 | 中国第一汽车股份有限公司 | Laminar inorganic matter-polymer composite membrane capable of improving ion transmission efficiency |
| CN105280866A (en) * | 2015-09-14 | 2016-01-27 | 李振勇 | Heat-resisting lithium battery diaphragm and preparation method thereof |
| CN106887552A (en) * | 2015-09-25 | 2017-06-23 | 三星电子株式会社 | Electrode composite diaphragm component for lithium battery and the lithium battery including it |
| CN107611321A (en) * | 2016-07-11 | 2018-01-19 | 宁德新能源科技有限公司 | Barrier film and secondary cell |
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Patent Citations (5)
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|---|---|---|---|---|
| CN104638220A (en) * | 2015-02-11 | 2015-05-20 | 中材科技股份有限公司 | Environment-friendly high-performance ceramic coating lithium ion battery diaphragm and preparation method thereof |
| CN104916803A (en) * | 2015-07-03 | 2015-09-16 | 中国第一汽车股份有限公司 | Laminar inorganic matter-polymer composite membrane capable of improving ion transmission efficiency |
| CN105280866A (en) * | 2015-09-14 | 2016-01-27 | 李振勇 | Heat-resisting lithium battery diaphragm and preparation method thereof |
| CN106887552A (en) * | 2015-09-25 | 2017-06-23 | 三星电子株式会社 | Electrode composite diaphragm component for lithium battery and the lithium battery including it |
| CN107611321A (en) * | 2016-07-11 | 2018-01-19 | 宁德新能源科技有限公司 | Barrier film and secondary cell |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111081954A (en) * | 2019-11-22 | 2020-04-28 | 东莞东阳光科研发有限公司 | Diaphragm coating slurry, diaphragm and preparation method thereof |
| CN111081954B (en) * | 2019-11-22 | 2020-12-22 | 东莞东阳光科研发有限公司 | Diaphragm coating slurry, diaphragm and preparation method thereof |
| EP4369452A1 (en) * | 2022-11-11 | 2024-05-15 | AESC Japan Ltd. | Secondary battery and preparation method thereof |
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