CN108565380A - A kind of preparation method of lithium ion battery separator - Google Patents
A kind of preparation method of lithium ion battery separator Download PDFInfo
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- CN108565380A CN108565380A CN201810258424.6A CN201810258424A CN108565380A CN 108565380 A CN108565380 A CN 108565380A CN 201810258424 A CN201810258424 A CN 201810258424A CN 108565380 A CN108565380 A CN 108565380A
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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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- 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
- 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
- H01M50/411—Organic 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
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
- H01M50/429—Natural polymers
- H01M50/4295—Natural cotton, cellulose or wood
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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
- H01M50/44—Fibrous 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
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
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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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Abstract
The present invention relates to field of lithium ion battery, provide a kind of preparation method of lithium ion battery separator, and step includes:1) chemically stable layers prepare base material, 2) are prepared, 3) refractory layer is prepared, existing lithium battery diaphragm base material is overcome to the disagreeableness defect of environment.
Description
Technical field
The present invention relates to field of lithium ion battery, especially a kind of preparation method of lithium ion battery separator.
Background technology
In the structure of lithium electron ion battery, diaphragm is one of the interior layer assembly of key.The main function of diaphragm is to make electricity
The positive and negative electrode in pond is separated, prevent the two poles of the earth contact and it is short-circuit, additionally have the function of electrolyte ion capable of being made to pass through.Every
Membrane material itself is nonconducting, and physicochemical properties have a great impact to the performance of battery.Currently, well known lithium battery
Diaphragm construction be include polyethylene diagrams, which is easy by thermal explosion, and traditional lithium battery diaphragm drawing
Stretch that intensity is too low, the integrated operation of inconvenient battery production.Accordingly, there exist the needs of battery diaphragm as offer, battery every
Film provides lower air drag and lower pore size, and whole higher tensile strength simultaneously, while showing suitable
When chemical stability, structural intergrity, dimensional stability, and it is easily fabricated.
Patent document CN201110461239 provides a kind of lithium battery diaphragm, including：One polyester nonwoven fabric fid,
In the polyester nonwoven fabric fid include polyethylene terephthalate, polytrimethylene terephthalate, poly terephthalic acid ring
Own dimethyl ester or combinations thereof；One Kynoar or derivatives thereof layer is formed on the polyester nonwoven fabric fid, and wherein this is poly-
Vinylidene or derivatives thereof layer includes Kynoar, Kynoar-hexafluoropropylene copolymer, Kynoar-trifluoro
Vinyl chloride copolymer or derivatives thereof or combination；And one ultraviolet light solidification or thermally curable polymer layer, be formed in this gather inclined fluorine
On ethylene or derivatives thereof layer, the wherein coating weight of ultraviolet light solidification or thermally curable polymer layer is between 19.4~36.4g/
M2, the wherein ultraviolet light cure or thermally curable polymer layer includes dimethyl silicone polymer or epoxides.The lithium battery every
Film solves the problems, such as that diaphragm is heat-resisting and dimensionally stable, but is oil base material there are still used polyester nonwoven fabric fid
Material, the problem unfavorable to environmental protection.
Invention content
Therefore, for the above content, the present invention provides a kind of preparation method of lithium ion battery separator, overcomes existing lithium
Battery diaphragm base material is to the disagreeableness defect of environment.
In order to achieve the above objectives, the present invention is achieved by the following technical solutions：
A kind of preparation method of lithium ion battery separator, the specific steps are：
1) base material, cellulose powder and the sulfuric acid solution in mass ratio 1 that mass fraction is 50-62% are prepared:10-1：16 ratio
Then it is anti-to be diluted with water stopping by example mixing, magnetic agitation 10-20min is placed under 40-60 DEG C of water bath condition that the reaction was continued 4-6h
It answers, centrifuges 3-5 times, suspension is transferred in bag filter, is placed in deionized water and impregnates, until pH value neutrality is subsequent
Continuous ultrasonic wave processing 1-1.5h, ultrasonic power 15-20KHZ, then centrifuge, suspension is obtained powdered by freeze-drying
Nano micro crystal cellulose (NCC)；Prepare powdered nano micro crystal cellulose, hydroxypropyl cellulose (HPC), silane coupling agent and goes
The mass ratio of ionized water, nano micro crystal cellulose and hydroxypropyl cellulose is 8:2-4:6, silane coupling agent dosage is that nanometer is micro-
The 0.3-2% of crystalline cellulose and hydroxypropyl cellulose gross mass, nano micro crystal cellulose is dissolved in deionized water, is stirred in magnetic force
Heating stirring in device is mixed, keeps its fully dispersed, hydroxypropyl cellulose solution and stirring that mass fraction is 10% is then added, so
After be added silane coupling agent, it is to be dissolved after ultrasonic wave disperse 1-2h, ultrasonic power 15-20KHZ, form latex, the latex warp
Through casting film-forming after vacuum outgas, 17-30 μm of film thickness, dry 4-5h, obtains base material in 70-80 DEG C of vacuum；
2) chemically stable layers are prepared, by octavinyl-POSS 5-8 parts by weight, Kynoar 80-90 parts by weight, diformazan
Yl acetamide solvent (DMAc) 400-500 parts by weight are stirred to react 3-4h at 80-100 DEG C, stop reaction, by prepared base
Material infiltration 10-20min in reaction solution, takes out, the dry 4-5h in 70-80 DEG C of vacuum；
3) refractory layer is prepared, it is silane coupled by DMAc solvent 400-500 parts by weight and inorganic nano material 1-10 parts by weight
5-10 parts of parts by weight of agent are uniformly mixed, and the dissolving of polyimides 80-90 parts by weight is added, and high-speed stirred is uniform, are coated on chemical steady
Given layer surface, 1-10 μm of thickness, dry 4-5h, obtains lithium ion battery separator in 70-80 DEG C of vacuum.
It is further improved to be:The cellulose powder preferably microcrystalline cellulose powder.
It is further improved to be:The sulfuric acid solution mass fraction a concentration of 60%.
It is further improved to be:The mass ratio of the nano micro crystal cellulose and hydroxypropyl cellulose is 6:4
It is further improved to be:The inorganic nano material is nano silicon dioxide, 20-50 nanometers of average grain diameter.
By using preceding solution, the beneficial effects of the invention are as follows：
1, it is that the base material that raw material makes is environmentally friendly by using the cellulose extracted in plant；Have using NCC
Nanometer size effect, high-specific surface area and strong mechanical performance, as reinforcement, mechanical performance, thermostabilization to macromolecule matrix
The tools such as property increase significantly, and prepared lithium ion battery membrane properties are excellent, and electrolyte absorptivity is big, ionic conductivity
Height, good thermal stability.
2, by carrying out POSS hydridization to poly- inclined Buddhist ethylene, its chemical stability is further improved.
3, the polyimides being added in refractory layer is outstanding heat proof material, and the addition of inorganic nano material contributes to resistance to
Hole is formed in thermosphere, has both effect that is heat-resisting and increasing diaphragm hole.
4, diaphragm uses multilayered structure, and tensile strength is high, safe.
Specific implementation mode
Carry out the embodiment that the present invention will be described in detail below with reference to specific embodiment, how skill is applied to the present invention whereby
Art means solve technical problem, and the realization process for reaching technique effect can fully understand and implement.
Unless otherwise specified, the conventional hand that the technological means employed in embodiment is well known to those skilled in the art
Section, used reagent and product are also available commercial.The source of agents useful for same, trade name and it is necessary to list it
Constituent person indicates on the first appearance.
Embodiment 1
A kind of preparation method of lithium ion battery separator, the specific steps are：
1) base material is prepared, cellulose powder 10kg will be prepared and mixed with the sulfuric acid 100kg of mass fraction 50%, magnetic agitation
15min is placed under 60 DEG C of water bath conditions that the reaction was continued 6h, is then diluted with water stopping reaction, centrifuges 3 times, by suspension
It is transferred in bag filter, is placed in deionized water and impregnates, until continuing ultrasonic wave processing 1h, ultrasonic power after pH value neutrality
15KHZ, then centrifuge, suspension obtains NCC by freeze-drying；Take NCC 2kg, HPC 0.5kg, silane coupling agent 75g
With 10kg deionized waters, NCC is dissolved in deionized water, the heating stirring in magnetic stirring apparatus keeps its fully dispersed, then adds
Enter hydroxypropyl cellulose solution and the stirring that mass fraction is 10%, silane coupling agent is then added, ultrasonic wavelength-division after to be dissolved
1h, ultrasonic power 15KHZ are dissipated, forms latex, for the latex through casting film-forming after vacuum outgas, 17 μm of film thickness is true at 70 DEG C
Aerial dry 4h, obtains base material；Contain microcrystalline cellulose and non-microcrystalline cellulose in cellulose powder, the present invention is washed away non-with sulfuric acid
Microcrystalline cellulose is carried out nanosizing by ultrasonic resonance, utilizes the nano-scale of nano micro crystal cellulose by microcrystalline cellulose
Effect can enhance hydroxypropyl cellulose film strength up to 200%, and the effect of coupling agent is the coupling of reinforcing fiber element, increase
By force at film strength；
2) chemically stable layers are prepared, by octavinyl-POSS 50g, Kynoar 800g, dimethylacetamide solvent
(DMAc) 3200g is stirred to react 3h at 80 DEG C, stops reaction, and prepared base material infiltration 10min in reaction solution takes out,
The dry 4h in 70 DEG C of vacuum；Silsesquioxane (POSS) is a kind of compound with special molecular structure, internal nothing
Machine skeleton Si-O-Si structures can provide good heat resistance for material, and the organic group of outer layer can enhance itself and polymer matrix again
Compatibility between body, and already existing organic side group on POSS can be chemically modified by side group conversion method, to
Obtain another new POSS with reactivity side group.By being blended with PVDF, it can effectively improve inorganic particulate and polymerize
The compatibility of object, tensile strength enhancing, thermal stability improve；
3) refractory layer is prepared, by DMAc solvents 5000g and nanometer silicon dioxide material 100g, silane coupling agent 100g mixing
Uniformly, polyimides 800g dissolvings are added, high-speed stirred is uniform, is coated on chemical stabilization layer surface, and 1 μm of thickness is true at 70 DEG C
Aerial dry 5h, obtains lithium ion battery separator, the nano silicon dioxide, 20 nanometers of average grain diameter；Polyimides is outstanding
Heat proof material, heat resisting temperature reach 200-300 DEG C, the addition of inorganic nano material helps to form hole in refractory layer, simultaneous
Has effect that is heat-resisting and increasing diaphragm hole.
Prepared lithium ion battery separator, septum body electrical isolation, porosity 51%, electrolyte absorptivity are 420%,
Ionic conductivity is 1.31Ms/cm, and thermostabilization is good, and 4h size changing rates are less than 0.1% under the conditions of 200 DEG C, film break temperature
210℃。
Embodiment 2
A kind of preparation method of lithium ion battery separator, the specific steps are：
1) base material is prepared, microcrystal cellulose powder 10kg will be prepared and mixed with the sulfuric acid 160kg of mass fraction 62%, magnetic force stirs
The 10min 4h that are placed under 40 DEG C of water bath conditions that the reaction was continued are mixed, stopping reaction being then diluted with water, centrifuges 5 times, will suspend
Liquid is transferred in bag filter, is placed in deionized water and is impregnated, until continuing ultrasonic wave processing 1.5h, ultrasonic work(after pH value neutrality
Rate 20KHZ, then centrifuge, suspension obtains NCC by freeze-drying；Take NCC 2kg, HPC 3kg, silane coupling agent
100g and 15kg deionized waters, NCC is dissolved in deionized water, and the heating stirring in magnetic stirring apparatus keeps its fully dispersed, so
Hydroxypropyl cellulose solution and the stirring that mass fraction is 10% are added afterwards, silane coupling agent is then added, it is ultrasonic after to be dissolved
Wavelength-division dissipates 2h, ultrasonic power 20KHZ, forms latex, the latex is after vacuum outgas through casting film-forming, 30 μm of film thickness, 80
Dry 5h, obtains base material in DEG C vacuum；
2) chemically stable layers are prepared, by octavinyl-POSS 80g, Kynoar 900g, DMAc 4500g, in 80 DEG C
Under be stirred to react 4h, stop reaction, prepared base material infiltration 20min in reaction solution take out, it is dry in 80 DEG C of vacuum
5h；
3) refractory layer is prepared, by DMAc solvents 4000g and nanometer silicon dioxide material 10g, silane coupling agent 50g mixing is equal
It is even, polyimides 900g dissolvings are added, high-speed stirred is uniform, is coated on chemical stabilization layer surface, 10 μm of thickness, in 80 DEG C of vacuum
Middle dry 4h obtains lithium ion battery separator, the nano silicon dioxide, 50 nanometers of average grain diameter.
Prepared lithium ion battery separator, septum body electrical isolation, porosity 47%, electrolyte absorptivity are 432%,
Ionic conductivity is 1.45Ms/cm, and thermostabilization is good, and 4h size changing rates are less than 0.1% under the conditions of 200 DEG C, film break temperature
205℃。
Embodiment 3
A kind of preparation method of lithium ion battery separator, the specific steps are：
1) base material is prepared, microcrystal cellulose powder 10kg will be prepared and mixed with the sulfuric acid 120kg of mass fraction 60%, magnetic force stirs
The 12min 5h that are placed under 50 DEG C of water bath conditions that the reaction was continued are mixed, stopping reaction being then diluted with water, centrifuges 4 times, will suspend
Liquid is transferred in bag filter, is placed in deionized water and is impregnated, until continuing ultrasonic wave processing 1.5h, ultrasonic work(after pH value neutrality
Rate 20KHZ, then centrifuge, suspension obtains NCC by freeze-drying；Take NCC 3kg, HPC 2kg, silane coupling agent 50g
With 10kg deionized waters, NCC is dissolved in deionized water, the heating stirring in magnetic stirring apparatus keeps its fully dispersed, then adds
Enter hydroxypropyl cellulose solution and the stirring that mass fraction is 10%, silane coupling agent is then added, ultrasonic wavelength-division after to be dissolved
1.5h, ultrasonic power 20KHZ are dissipated, forms latex, the latex is after vacuum outgas through casting film-forming, 20 μm of film thickness, at 75 DEG C
Dry 5h, obtains base material in vacuum；
2) chemically stable layers are prepared, by octavinyl-POSS 60g, Kynoar 850g, DMAc 3800g, in 80 DEG C
Under be stirred to react 4h, stop reaction, prepared base material infiltration 20min in reaction solution take out, it is dry in 80 DEG C of vacuum
5h；
3) refractory layer is prepared, by DMAc solvents 4500g and nanometer silicon dioxide material 50g, silane coupling agent 80g mixing is equal
It is even, polyimides 850g dissolvings are added, high-speed stirred is uniform, is coated on chemical stabilization layer surface, 5 μm of thickness, in 80 DEG C of vacuum
Middle dry 4h obtains lithium ion battery separator, the nano silicon dioxide, 30 nanometers of average grain diameter.
Prepared lithium ion battery separator, septum body electrical isolation, porosity 49%, electrolyte absorptivity are 412%,
Ionic conductivity is 1.31Ms/cm, and thermostabilization is good, and 4h size changing rates are less than 0.1% under the conditions of 200 DEG C, film break temperature
207℃。
The foregoing descriptions are merely the embodiment using this origination techniques content, any those skilled in the art use this wound
Make done modifications and changes, all belong to the scope of the claims of this creation opinion, and is not limited to those disclosed embodiments.
Claims (5)
1. a kind of preparation method of lithium ion battery separator, it is characterised in that：The specific steps are：
1) base material, cellulose powder and the sulfuric acid solution in mass ratio 1 that mass fraction is 50-62% are prepared:10-1：16 ratio is mixed
It closing, then magnetic agitation 10-20min is placed under 40-60 DEG C of water bath condition that the reaction was continued 4-6h is diluted with water stopping reaction,
It centrifuges 3-5 times, suspension is transferred in bag filter, is placed in deionized water and impregnates, until continuing after pH value neutrality
Ultrasonic wave processing 1-1.5h, ultrasonic power 15-20KHZ, then centrifuge, suspension obtains powdered receive by freeze-drying
Rice microcrystalline cellulose；Prepare powdered nano micro crystal cellulose, hydroxypropyl cellulose, silane coupling agent and deionized water, nanometer
The mass ratio of microcrystalline cellulose and hydroxypropyl cellulose is 8:2-4:6, silane coupling agent dosage be nano micro crystal cellulose with
The 0.3-2% of hydroxypropyl cellulose gross mass, nano micro crystal cellulose is dissolved in deionized water, is heated in magnetic stirring apparatus
Stirring, keeps its fully dispersed, and hydroxypropyl cellulose solution and stirring that mass fraction is 10% is then added, silane is then added
Coupling agent, rear ultrasonic wave to be dissolved disperse 1-2h, ultrasonic power 15-20KHZ, form latex, the latex is after vacuum outgas
Through casting film-forming, 17-30 μm of film thickness, dry 4-5h, obtains base material in 70-80 DEG C of vacuum；
2) chemically stable layers are prepared, by octavinyl-POSS 5-8 parts by weight, Kynoar 80-90 parts by weight, dimethyl second
Amide solvent 400-500 parts by weight are stirred to react 3-4h at 80-100 DEG C, stop reaction, and prepared base material is infiltrated anti-
10-20min in liquid is answered, is taken out, the dry 4-5h in 70-80 DEG C of vacuum；
3) refractory layer is prepared, by dimethylacetamide solvent 400-500 parts by weight and inorganic nano material 1-10 parts by weight, silane
5-10 parts of parts by weight of coupling agent are uniformly mixed, and the dissolving of polyimides 80-90 parts by weight are added, high-speed stirred is uniform, being coated on
It learns and stablizes layer surface, 1-10 μm of thickness, dry 4-5h, obtains lithium ion battery separator in 70-80 DEG C of vacuum.
2. a kind of preparation method of lithium ion battery separator according to claim 1, it is characterised in that：The cellulose powder
Preferably microcrystalline cellulose powder.
3. a kind of preparation method of lithium ion battery separator according to claim 1, it is characterised in that：The sulfuric acid solution
Mass fraction a concentration of 60%.
4. a kind of preparation method of lithium ion battery separator according to claim 1, it is characterised in that：The nano microcrystalline
The mass ratio of cellulose and hydroxypropyl cellulose is 6:4.
5. a kind of preparation method of lithium ion battery separator according to claim 1, it is characterised in that：The inorganic nano
Material is nano silicon dioxide, and average grain diameter is 20-50 nanometers.
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| CN201810258424.6A CN108565380B (en) | 2018-03-27 | 2018-03-27 | Preparation method of lithium ion battery diaphragm |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113517517A (en) * | 2021-03-05 | 2021-10-19 | 深圳市新非泽科技有限公司 | Coating slurry for lithium battery diaphragm and coating process |
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| CN105720224A (en) * | 2016-03-28 | 2016-06-29 | 北京理工大学 | Novel nano-crystalline cellulose modified lithium ion battery diaphragm and preparation method thereof |
| CN106220904A (en) * | 2016-08-22 | 2016-12-14 | 王利萍 | A kind of preparation method of NCC modified sodium alginate degradable composite membrane |
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| CN103242658A (en) * | 2013-05-24 | 2013-08-14 | 中国国旅贸易有限责任公司 | Porous membrane and preparation method thereof |
| CN104342850A (en) * | 2013-08-08 | 2015-02-11 | 珠海市红旌发展有限公司 | Polyimide film containing nanocrystal cellulose and preparation method thereof |
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| CN105185940A (en) * | 2015-10-23 | 2015-12-23 | 旭成（福建）科技股份有限公司 | Preparation method and application of polyolefin/nanocrystal cellulose composite diaphragm |
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| CN113517517A (en) * | 2021-03-05 | 2021-10-19 | 深圳市新非泽科技有限公司 | Coating slurry for lithium battery diaphragm and coating process |
| CN113517517B (en) * | 2021-03-05 | 2022-12-30 | 深圳市新非泽科技有限公司 | Coating slurry for lithium battery diaphragm and coating process |
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