CN108807794A - A kind of preparation method of high mechanical properties fiber base lithium battery diaphragm material - Google Patents
A kind of preparation method of high mechanical properties fiber base lithium battery diaphragm material Download PDFInfo
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- CN108807794A CN108807794A CN201810626527.3A CN201810626527A CN108807794A CN 108807794 A CN108807794 A CN 108807794A CN 201810626527 A CN201810626527 A CN 201810626527A CN 108807794 A CN108807794 A CN 108807794A
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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
-
- 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
-
- 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
-
- 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 & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Materials Engineering (AREA)
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Abstract
The present invention relates to a kind of preparation methods of high mechanical properties fiber base lithium battery diaphragm material, belong to technical field of electronic materials.Technical solution of the present invention uses microcrystalline cellulose for modified material, after ultrasonic disperse is handled, microcrystalline cellulose disperses evenly, very lack adhesion, pass through homogenization simultaneously, the effective crimp of carry out and destruction to the cell wall of cellulosic material, the contact area of fiber and lye has been significantly greatly increased, more lye are made to infiltrate into inside cellulose to a certain extent, make to have the cellulose of multilevel hierarchy to generate swollen, to be more conducive to fibrillation processing, this unique tridimensional network is as reinforcement, the intensity of basis material can be effectively improved, to be effectively improved the mechanical strength of cellulose pulp material.
Description
Technical field
The present invention relates to a kind of preparation methods of high mechanical properties fiber base lithium battery diaphragm material, belong to electronic material skill
Art field.
Background technology
Most basic for lithium ion battery separator requires to include the following aspects：
（1）Mechanical strength, thermal stability：Battery diaphragm must have certain mechanical strength, just can guarantee that battery is assembling in this way
With during charge and discharge will not short circuit.Thermal stability is one of the important indicator for weighing battery safety, once in battery
Diaphragm is heated to be occurred rupture or is heat-shrinked, it will is caused positive and negative anodes to be in direct contact, is directly resulted in the generation of cell safety accident.
Therefore diaphragm needs to have certain mechanical strength and thermal stability, ensures battery in compression, ion shuttle work and high temperature
In the case of can work normally.
Electronic isolation：Diaphragm must have excellent insulating properties, could play the effect of insulating electron between electrodes.
Its principle acted on is so that the transmission path of electronics can only be by conducting wire, and ion can only be transmitted by electrolyte.
Thickness：The thickness of diaphragm will make very much that ion transmits greatly interface is larger, transmission process is obstructed, it will lead to electricity
Pond internal resistance increases, and battery working efficiency reduces, but diaphragm is excessively thin and mechanical strength properties variation, aperture can be caused larger, holds
Easily cause safety problem, therefore suitable membrane thicknesses are to improving battery performance important role.
Pore structure：Gap appropriate is needed inside diaphragm allows lithium ion to pass through, while can store electrolyte, makes lithium
Ion can quickly pass through diaphragm, while the size in hole and quantity determine the gas permeability and porosity of diaphragm, usually ventilative
Property it is smaller, porosity is higher, and internal resistance is smaller, ion transmission the electrochemistry bigger, therefore that battery can be made to show of rate
Performance is better, but if aperture is excessive, this makes diaphragm not have the purpose that barrier positive and negative polarities are in direct contact, and can make electricity
Short circuit occurs for pond, so as to cause cell safety problem.
Wellability, imbibition rate：Diaphragm, which has excellent wellability, so that electrolyte is quickly infiltrated diaphragm, be conducive to subtract
The time stood after few cell assembling processes and battery assembling, moreover it is possible to avoid because wellability is bad between electrolyte and battery diaphragm
And make there is the phenomenon that excessive bubble or battery leakage between diaphragm and pole piece.The high imbibition rate of diaphragm is conducive to lithium ion
Transmission increases the ionic conductivity of diaphragm, and then improves the chemical property of battery and extend the service life of battery.
Nowadays commercialized diaphragm is mainly polyolefins, can occur to heat phenomenon at a certain temperature, can not
It recurs and obstructs the effect of battery plus-negative plate, and positive and negative anodes are in direct contact and short circuit phenomenon occur, and then cause
A series of safety problems such as batteries caught fire or explosion, therefore the cell safety energy assembled with polyolefins battery diaphragm
The problem of worrying the most can be become.Meanwhile polyolefins diaphragm leads to diaphragm and electrolysis due to the lower surface energy of material itself
Liquid wellability is poor, although having had the method that some improve polyolefins diaphragm for this disadvantage：Surface grafting, polymerization
Object, which coats, and nano inoganic particle coats etc. improves its wellability with electrolyte, but such method results in entire system
The technical process for making battery diaphragm is more complicated so that lithium battery cost is high, seriously constrains the hair of dynamic lithium battery
Exhibition, therefore development technology is relatively easy and the relatively high battery diaphragm of performance becomes one of the main targets of future studies.Seaweed
Sour calcium fibre resources are abundant, environmental-friendly, cheap, have biodegradability, and the paper substrate prepared as raw material using it
Alginic acid fibre
Plain diaphragm high temperature resistant reaches 200 DEG C or more, has good wellability, high imbibition rate and porosity with organic solvent.
But directly go out calcium alginate fibre with Wet-spinning and be used to prepare diaphragm to will appear that mechanical strength is relatively low, aperture is larger and diaphragm
The problems such as thicker.Therefore the preparation process of entire diaphragm is optimized, becomes the calcium alginate fibre base lithium for obtaining high intensity
The key of ion battery diaphragm.
The invention content technical problems to be solved by the invention：The artificial blood vessel's mechanical property prepared for existing collagen-based materials
The poor problem of energy, provides a kind of preparation method of artificial blood vessel's high mechanical properties fiber type membrane material.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
（1）Take microcrystalline cellulose and in mass ratio 1:10, it is dispersed in 1mol/L sodium hydroxide solutions, is stirred and surpasses
Sound disperses, and collects dispersion liquid and is placed in homogenizer, homogenization 25~30 times after being stirred 2~3h, then uses mass fraction
5% sodium hydroxide solution adjusts pH to 8.5, and filtering collects filter cake and 3~5h of vacuum freeze drying, obtains dried object；
（2）Count in parts by weight, weigh respectively 45~50 parts of 5% acetic acid solutions of mass fraction, 10~15 parts of tannic acid and 10~
15 parts of collagen powder are placed in beaker, are stirred and ultrasonic disperse, collection are modified dispersion liquid and in mass ratio 1:5, it will
Dried object is added in modified dispersion liquid, and standing/filtering simultaneously collects filter cake, dry modified cellulosic materials；
（3）In mass ratio 1:5, modified cellulosic materials are added in papermaking pulp, are impregnated at room temperature, mashing processing obtains
Modified fibre pulp；
（4）Count in parts by weight, weigh 45~50 parts of 5% poly-vinyl alcohol solutions of mass fraction respectively, 10~15 parts of length be 3~
5mm calcium alginate fibres and 10~15 parts of modified cellulose pulps are placed in fiber dissociation device, dissociation processing, copy paper, after dry,
The diaphragm of corresponding size is cut into sheet-punching machine, you can be prepared into the high mechanical properties fiber base lithium battery diaphragm material.
Step（1）The homogenization pressure is 1000~1200bar.
Step（3）It is 30 ° of SR that the mashing processing, which is mashing to beating degree,.
Step（4）The dissociation processing is the dissociation processing at 1000~1100r/min.
Step（4）Quantification of 45~the 50g/m of the copy paper2。
Compared with other methods, advantageous effects are the present invention：
（1）Technical solution of the present invention uses microcrystalline cellulose for modified material, after ultrasonic disperse is handled, microcrystalline cellulose dispersion
Evenly, very adhesion less, while by homogenization, the effective crimp of carry out to the cell wall of cellulosic material and broken
It is bad, the contact area of fiber and lye has been significantly greatly increased, so that more lye is infiltrated into inside cellulose to a certain extent, makes tool
There is the cellulose of multilevel hierarchy to generate swollen, to be more conducive to fibrillation processing, this unique tridimensional network is made
For reinforcement, the intensity of basis material can be effectively improved, to be effectively improved the mechanical strength of cellulose pulp material；
（2）Technical solution of the present invention is by collagen covered fiber cellulosic material and forms it into organic combination, by collagen to fibre
It is organically compound to tie up cellulosic material, improves material surface structure, improves the mechanical strength of material, while technical solution of the present invention passes through
Fiber pulp is effectively combined with calcium alginate, forms effective three-dimensional netted intertexture inside fibrous material by pulp material
Structure, to be effectively improved the mechanical performance of material.
Specific implementation mode
Take microcrystalline cellulose and in mass ratio 1:10, it is dispersed in 1mol/L sodium hydroxide solutions, is stirred simultaneously
10~15min of ultrasonic disperse, collect dispersion liquid be placed in homogenizer, under 1000~1200bar pressure homogenization 25~
30 times, after being stirred 2~3h, then with 5% sodium hydroxide solution of mass fraction adjust pH to 8.5, filtering, collect filter cake simultaneously it is true
3~5h of vacuum freecing-dry, obtains dried object；It counts in parts by weight, weighs 45~50 parts of 5% acetic acid solutions of mass fraction, 10 respectively
~15 parts of tannic acid and 10~15 parts of collagen powder are placed in beaker, are stirred and are placed in ultrasound point under 200~300W
10~15min is dissipated, modified dispersion liquid and in mass ratio 1 is collected:5, dried object is added in modified dispersion liquid, 6~8h is stood
Afterwards, filter cake is filtered and collected, at 45~50 DEG C after dry 6~8h, obtains modified cellulosic materials；In mass ratio 1:5, it will be modified
Cellulosic material is added in papermaking pulp, at room temperature impregnate 20~for 24 hours after, then be beaten to beating degree be 30 ° of SR, obtain modification
Fiber pulp is counted in parts by weight, weighs 45~50 parts of 5% poly-vinyl alcohol solutions of mass fraction respectively, 10~15 parts of length are 3
~5mm calcium alginate fibres and 10~15 parts of modified cellulose pulps are placed in fiber dissociation device, at 1000~1100r/min
Dissociation is handled, and the fiber after dissociation is being placed in copy paper in sheet forming apparatus, the quantification of 45~50g/m of control copy paper2, 45~
At 50 DEG C after dry 3~5h, the diaphragm of corresponding size is cut into sheet-punching machine, you can be prepared into the high mechanical properties fiber
Base lithium battery diaphragm material.
Take microcrystalline cellulose and in mass ratio 1:10, it is dispersed in 1mol/L sodium hydroxide solutions, is stirred simultaneously
Ultrasonic disperse 10min collects dispersion liquid and is placed in homogenizer, and homogenization 25 times, are stirred 2h under 1000bar pressure
Afterwards, then with 5% sodium hydroxide solution of mass fraction pH to 8.5 is adjusted, filtering is collected filter cake and vacuum freeze drying 3h, obtained dry
Dry object；It counts in parts by weight, weighs 45 parts of 5% acetic acid solutions of mass fraction, 10 parts of tannic acid and 10 parts of collagen protein powders respectively
End is placed in beaker, is stirred and is placed in ultrasonic disperse 10min under 200W, and modified dispersion liquid and in mass ratio 1 is collected:5, it will
Dried object is added in modified dispersion liquid, after standing 6h, filters and collect filter cake, at 45 DEG C after dry 6h, obtains modified fibre
Cellulosic material；In mass ratio 1:5, modified cellulosic materials are added in papermaking pulp, after impregnating 20h at room temperature, then are beaten
It is 30 ° of SR to beating degree, obtains modified fibre pulp, count in parts by weight, it is molten weighs 45 parts of 5% polyvinyl alcohol of mass fraction respectively
Liquid, 10 parts of length are that 3mm calcium alginate fibres and 10 parts of modified cellulose pulps are placed in fiber dissociation device, in 1000r/min
Fiber after dissociation is being placed in copy paper in sheet forming apparatus, the quantification of 45g/m of control copy paper by lower dissociation processing2, at 45 DEG C
After dry 3h, the diaphragm of corresponding size is cut into sheet-punching machine, you can be prepared into the high mechanical properties fiber base lithium battery
Diaphragm material.
Take microcrystalline cellulose and in mass ratio 1:10, it is dispersed in 1mol/L sodium hydroxide solutions, is stirred simultaneously
Ultrasonic disperse 12min collects dispersion liquid and is placed in homogenizer, and homogenization 27 times, are stirred 2h under 1100bar pressure
Afterwards, then with 5% sodium hydroxide solution of mass fraction pH to 8.5 is adjusted, filtering is collected filter cake and vacuum freeze drying 4h, obtained dry
Dry object；It counts in parts by weight, weighs 47 parts of 5% acetic acid solutions of mass fraction, 12 parts of tannic acid and 12 parts of collagen protein powders respectively
End is placed in beaker, is stirred and is placed in ultrasonic disperse 12min under 250W, and modified dispersion liquid and in mass ratio 1 is collected:5, it will
Dried object is added in modified dispersion liquid, after standing 7h, filters and collect filter cake, at 47 DEG C after dry 7h, obtains modified fibre
Cellulosic material；In mass ratio 1:5, modified cellulosic materials are added in papermaking pulp, after impregnating 22h at room temperature, then are beaten
It is 30 ° of SR to beating degree, obtains modified fibre pulp, count in parts by weight, it is molten weighs 47 parts of 5% polyvinyl alcohol of mass fraction respectively
Liquid, 12 parts of length are that 4mm calcium alginate fibres and 12 parts of modified cellulose pulps are placed in fiber dissociation device, in 1050r/min
Fiber after dissociation is being placed in copy paper in sheet forming apparatus, the quantification of 47g/m of control copy paper by lower dissociation processing2, at 47 DEG C
After dry 4h, the diaphragm of corresponding size is cut into sheet-punching machine, you can be prepared into the high mechanical properties fiber base lithium battery
Diaphragm material.
Take microcrystalline cellulose and in mass ratio 1:10, it is dispersed in 1mol/L sodium hydroxide solutions, is stirred simultaneously
Ultrasonic disperse 15min collects dispersion liquid and is placed in homogenizer, and homogenization 30 times, are stirred 3h under 1200bar pressure
Afterwards, then with 5% sodium hydroxide solution of mass fraction pH to 8.5 is adjusted, filtering is collected filter cake and vacuum freeze drying 5h, obtained dry
Dry object；It counts in parts by weight, weighs 50 parts of 5% acetic acid solutions of mass fraction, 15 parts of tannic acid and 15 parts of collagen protein powders respectively
End is placed in beaker, is stirred and is placed in ultrasonic disperse 15min under 300W, and modified dispersion liquid and in mass ratio 1 is collected:5, it will
Dried object is added in modified dispersion liquid, after standing 8h, filters and collect filter cake, at 50 DEG C after dry 8h, obtains modified fibre
Cellulosic material；In mass ratio 1:5, modified cellulosic materials are added in papermaking pulp, after impregnating for 24 hours at room temperature, then are beaten
It is 30 ° of SR to beating degree, obtains modified fibre pulp, count in parts by weight, it is molten weighs 50 parts of 5% polyvinyl alcohol of mass fraction respectively
Liquid, 15 parts of length are that 5mm calcium alginate fibres and 15 parts of modified cellulose pulps are placed in fiber dissociation device, in 1100r/min
Fiber after dissociation is being placed in copy paper in sheet forming apparatus, the quantification of 50g/m of control copy paper by lower dissociation processing2, at 50 DEG C
After dry 5h, the diaphragm of corresponding size is cut into sheet-punching machine, you can be prepared into the high mechanical properties fiber base lithium battery
Diaphragm material.
Example 1,2,3 prepared by the present invention is tested for the property, specific test result is as follows shown in table table 1：
1 performance test table of table
As seen from the above table, the lithium battery diaphragm material that prepared by the present invention has excellent mechanical strength.
Claims (5)
1. a kind of preparation method of high mechanical properties fiber base lithium battery diaphragm material, it is characterised in that specifically preparation process is：
（1）Take microcrystalline cellulose and in mass ratio 1:10, it is dispersed in 1mol/L sodium hydroxide solutions, is stirred and surpasses
Sound disperses, and collects dispersion liquid and is placed in homogenizer, homogenization 25~30 times after being stirred 2~3h, then uses mass fraction
5% sodium hydroxide solution adjusts pH to 8.5, and filtering collects filter cake and 3~5h of vacuum freeze drying, obtains dried object；
（2）Count in parts by weight, weigh respectively 45~50 parts of 5% acetic acid solutions of mass fraction, 10~15 parts of tannic acid and 10~
15 parts of collagen powder are placed in beaker, are stirred and ultrasonic disperse, collection are modified dispersion liquid and in mass ratio 1:5, it will
Dried object is added in modified dispersion liquid, and standing/filtering simultaneously collects filter cake, dry modified cellulosic materials；
（3）In mass ratio 1:5, modified cellulosic materials are added in papermaking pulp, are impregnated at room temperature, mashing processing obtains
Modified fibre pulp；
（4）Count in parts by weight, weigh 45~50 parts of 5% poly-vinyl alcohol solutions of mass fraction respectively, 10~15 parts of length be 3~
5mm calcium alginate fibres and 10~15 parts of modified cellulose pulps are placed in fiber dissociation device, dissociation processing, copy paper, after dry,
The diaphragm of corresponding size is cut into sheet-punching machine, you can be prepared into the high mechanical properties fiber base lithium battery diaphragm material.
2. a kind of preparation method of high mechanical properties fiber base lithium battery diaphragm material according to claim 1, feature
It is：Step（1）The homogenization pressure is 1000~1200bar.
3. a kind of preparation method of high mechanical properties fiber base lithium battery diaphragm material according to claim 1, feature
It is：Step（3）It is 30 ° of SR that the mashing processing, which is mashing to beating degree,.
4. a kind of preparation method of high mechanical properties fiber base lithium battery diaphragm material according to claim 1, feature
It is：Step（4）The dissociation processing is the dissociation processing at 1000~1100r/min.
5. a kind of preparation method of high mechanical properties fiber base lithium battery diaphragm material according to claim 1, feature
It is：Step（4）Quantification of 45~the 50g/m of the copy paper2。
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| CN201810626527.3A CN108807794A (en) | 2018-06-19 | 2018-06-19 | A kind of preparation method of high mechanical properties fiber base lithium battery diaphragm material |
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| CN201810626527.3A CN108807794A (en) | 2018-06-19 | 2018-06-19 | A kind of preparation method of high mechanical properties fiber base lithium battery diaphragm material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115726227A (en) * | 2022-11-17 | 2023-03-03 | 航天特种材料及工艺技术研究所 | Preparation method of high-temperature-resistant wave-absorbing film |
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Application publication date: 20181113 |