CN109713197A - A kind of preparation method of composite diaphragm - Google Patents
A kind of preparation method of composite diaphragm Download PDFInfo
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- CN109713197A CN109713197A CN201811609154.5A CN201811609154A CN109713197A CN 109713197 A CN109713197 A CN 109713197A CN 201811609154 A CN201811609154 A CN 201811609154A CN 109713197 A CN109713197 A CN 109713197A
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a kind of preparation methods of composite diaphragm, ceramic slurry, polymethyl methacrylate (PMMA) slurry and Kynoar (PVDF) and its copolymer pulp are first prepared respectively, ceramic slurry is coated on to the upper and lower of basement membrane, PMMA slurry is coated on ceramic coating, PVDF and its copolymer pulp are coated on lower ceramic coating, i.e. a kind of composite diaphragm by PMMA coating/upper ceramic coating/base/lower ceramic coating/PVDF and its it is copolymer coated form, which has preferable imbibition rate, peel strength and thermal stability.
Description
Technical field
The present invention relates to coating membrane technique field, specifically a kind of preparation methods of composite diaphragm.
Background technique
The lithium ion battery separator being commercialized at present has polypropylene screen (PP), polyethylene film (PE) or multilayer complex films.It is poly-
The extensive use of alkene diaphragm, which is shown, has many advantages, such as reasonable cost, chemical stability and the self-closing performance of high temperature, but hot
It shrinks and mechanical strength is poor.When battery local temperature is more than 160 DEG C, diaphragm easily loses mechanical integrity, large area occurs
Contraction causes positive and negative anodes to contact, and battery is made to face the danger burnt and exploded under high temperature.
PP or PE is a kind of non-polar material, it is poor with highly polar electrolyte solution compatibility, and the imbibition of diaphragm with
Liquid-keeping property power has close correlation to the charge and discharge of battery, service life cycle.Polyolefin polymers are to electrolysis
The absorption of liquid and holding capacity are weaker, have a certain impact to the efficiency for charge-discharge of lithium battery；The liquid lithium generally used simultaneously
Existing gap and the battery electrolyte free electrolyte in cyclic process influence electricity between ion battery anode, cathode and diaphragm
The consistency and safety in pond.
Develop a kind of high safety, high intensity, high-temperature resistant diaphragm will become the trend of lithium electric separator development.
Summary of the invention
To overcome existing diaphragm material to the absorption of electrolyte, the disadvantage that holding capacity is weaker and thermal stability is poor, this hair
The bright absorption for being designed to provide a kind of pair of electrolyte and holding capacity are strong, highly-safe, at low cost, the feature of environmental protection is good answers
Close the preparation method of diaphragm.
The present invention provides a kind of preparation method of composite diaphragm, the present invention is by multiple coating process, the two of basement membrane
Side is respectively coated ceramic coating, and PMMA coating and PVDF and its copolymer coated are respectively coated again in ceramic coating, obtains one kind
Tool is of five storeys the composite diaphragm of structure, i.e., a kind of composite diaphragm by PMMA coating/upper ceramic coating/base/lower ceramic coating/
PVDF and its copolymer coated composition.
To achieve the above objectives, the specific technical solution of the present invention is:
A kind of preparation method of composite diaphragm, this method comprises the following steps, and raw material is in terms of mass fraction:
Step 1: preparing ceramic slurry for 40~60 parts of inorganic material, 50~80 parts of deionized waters, 0.1~1 part of carboxymethyl
Sodium cellulosate and 1~6 part of binder, are dispersed with stirring 10~60min, obtain ceramic slurry；
Step 2: preparing PMMA slurry for 40~60 parts of PMMA, 50~80 parts of deionized waters, 0.1~1 part of carboxymethyl cellulose
Plain sodium and 1~6 part of binder, are dispersed with stirring 10~60min, obtain PMMA slurry；
Step 3: preparing PVDF and its copolymer pulp for 40~60 parts of PVDF and its copolymer, 50~80 parts of deionizations
Water, 0.1~1 part of sodium carboxymethylcellulose and 1~6 part of binder, are dispersed with stirring 10~60min, obtain PVDF and its copolymer
Slurry；
Step 4: coating
Ceramic slurry made from step 1 is coated on to the upper and lower of basement membrane as coating method, obtains ceramics painting
Layer and lower ceramic coating, are coated on upper ceramic coating for PMMA slurry made from step 2, obtain PMMA coating, step 3 is made
PVDF and its copolymer pulp be coated on lower ceramic coating, obtain PVDF and its copolymer coated, i.e., a kind of composite diaphragm by
PMMA coating/upper ceramic coating/basement membrane/lower ceramic coating/PVDF and its copolymer coated composition.
The inorganic material is in silica, aluminum oxide, magnesia, calcium oxide, boehmite and titanium dioxide
At least one.
The binder is styrene-acrylic emulsion, pure-acrylic emulsion, styrene-butadiene emulsion, ethylene-vinyl acetate copolymer emulsion and gathers
At least one of vinyl alcohol.
The PVDF and its copolymer is Kynoar, Kynoar-trifluoro-ethylene, Kynoar-tetrafluoro
At least one of ethylene, Kynoar-hexafluoroethylene and Kynoar-hexafluoropropene.
The basement membrane is one in polyethylene monolayer film, polypropylene monofilm and polyethylene and polypropylene multi-layer composite membrane
Kind.
The basement membrane with a thickness of 5~20 μm, upper ceramic coating with a thickness of 0.5~4 μm, the thickness of lower ceramic coating
Be 0.5~4 μm, PMMA coating with a thickness of 0.2~2 μm, PVDF and its copolymer coated with a thickness of 0.2~2 μm.Described
Coating method is one of gravure roll coating, narrow slit type coating, anilox roll coating, Slot-die coating and spraying.
Compared with prior art, the invention has the following advantages:
The PMMA coating of top layer have good electrolyte adsorptivity, higher proof voltage, lower softening point and
Melting temperature, therefore, obtained lithium ion battery separator have good suction electrolyte property, chemical property and in high temperature
Under good closed pore performance；
Undermost PVDF and its copolymer coated can improve the heat-shrinkable and lithium battery diaphragm of diaphragm
Liquid absorption amount improves diaphragm lithium ion conduction ability, to improve the multiplying power and cycle performance of lithium ion battery.
The ceramic coating of basement membrane two sides, can significantly improve the thermal stability of diaphragm, the ceramic coating of porous structure,
Be conducive to the abjection and insertion of lithium ion.
Ceramic slurry, PMMA slurry and the PVDF and its copolymer pulp of preparation are water-based system, aqueous slurry coating
Process is smooth, reduces the requirement to coating apparatus, more environmentally-friendly.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of composite diaphragm prepared by the present invention.
Specific embodiment
Embodiment 1
A kind of preparation method of composite diaphragm, this method comprises the following steps, and raw material is in terms of mass fraction:
Step 1: preparing ceramic slurry for 40 parts of boehmites, 50 parts of deionized waters, 0.1 part of sodium carboxymethylcellulose and 1 part
Styrene-acrylic emulsion is dispersed with stirring 30min, obtains ceramic slurry；
Step 2: preparing PMMA slurry for 40 parts of PMMA, 50 parts of deionized water, 0.1 part of sodium carboxymethylcellulose and 1 part
Styrene-acrylic emulsion is dispersed with stirring 30min, obtains PMMA slurry；
Step 3: preparation PVDF and its copolymer pulp by 40 parts of Kynoar-hexafluoropropenes, 50 parts of deionized waters,
0.1 part of sodium carboxymethylcellulose and 1 part of styrene-acrylic emulsion, are dispersed with stirring 30min, obtain PVDF and its copolymer pulp；
Step 4: coating
Ceramic slurry made from step 1 is coated on to the upper and lower of polyethylene monolayer film as spraying method, is obtained
Upper ceramic coating and lower ceramic coating, are coated on upper ceramic coating for PMMA slurry made from step 2, obtain PMMA coating, will
PVDF made from step 3 and its copolymer pulp are coated on lower ceramic coating, obtain PVDF and its copolymer coated, i.e., a kind of multiple
Diaphragm is closed by PMMA coating/upper ceramic coating/polyethylene monolayer film/lower ceramic coating/PVDF and its copolymer coated is formed.
Basement membrane with a thickness of 12 μm, upper ceramic coating with a thickness of 1 μm, lower ceramic coating with a thickness of 1 μm, PMMA coating
With a thickness of 1 μm, PVDF and its copolymer coated with a thickness of 1 μm.
Embodiment 2
A kind of preparation method of composite diaphragm, this method comprises the following steps, and raw material is in terms of mass fraction:
Step 1: preparing ceramic slurry for 45 parts of titanium dioxide, 70 parts of deionized waters, 0.4 part of sodium carboxymethylcellulose and 5
Part pure-acrylic emulsion, is dispersed with stirring 30min, obtains ceramic slurry；
Step 2: preparing PMMA slurry for 45 parts of PMMA, 70 parts of deionized water, 0.4 part of sodium carboxymethylcellulose and 5 parts
Pure-acrylic emulsion is dispersed with stirring 30min, obtains PMMA slurry；
Step 3: preparation PVDF and its copolymer pulp by 45 parts of Kynoar-hexafluoroethylenes, 70 parts of deionized waters,
0.4 part of sodium carboxymethylcellulose and 5 parts of pure-acrylic emulsions, are dispersed with stirring 30min, obtain PVDF and its copolymer pulp；
Step 4: coating
Ceramic slurry made from step 1 is coated on the upper layer of polyethylene monolayer film under as anilox roll coating method
Layer, obtains ceramic coating and lower ceramic coating, PMMA slurry made from step 2 is coated on upper ceramic coating, obtains PMMA
PVDF made from step 3 and its copolymer pulp are coated on lower ceramic coating by coating, obtain PVDF and its copolymer coated,
I.e. a kind of composite diaphragm is applied by PMMA coating/upper ceramic coating/polyethylene monolayer film/lower ceramic coating/PVDF and its copolymer
Layer composition.
Basement membrane with a thickness of 12 μm, upper ceramic coating with a thickness of 1.5 μm, lower ceramic coating with a thickness of 1.5 μm, PMMA
Coating with a thickness of 0.5 μm, PVDF and its copolymer coated with a thickness of 0.5 μm.
Embodiment 3
A kind of preparation method of composite diaphragm, this method comprises the following steps, and raw material is in terms of mass fraction:
Step 1: preparing ceramic slurry for 55 parts of calcium oxide, 80 parts of deionized waters, 0.7 part of sodium carboxymethylcellulose and 4 parts
Ethylene-vinyl acetate copolymer emulsion is dispersed with stirring 40min, obtains ceramic slurry；
Step 2: preparing PMMA slurry for 55 parts of PMMA, 80 parts of deionized water, 0.7 part of sodium carboxymethylcellulose and 4 parts
Ethylene-vinyl acetate copolymer emulsion is dispersed with stirring 40min, obtains PMMA slurry；
Step 3: preparation PVDF and its copolymer pulp by 55 parts of Kynoar-hexafluoroethylenes, 80 parts of deionized waters,
0.7 part of sodium carboxymethylcellulose and 4 parts of ethylene-vinyl acetate copolymer emulsions, are dispersed with stirring 40min, obtain PVDF and its are total to
Polymers slurry；
Step 4: coating
Ceramic slurry made from step 1 is coated on the upper layer of polypropylene monofilm under as narrow slit type coating method
Layer, obtains ceramic coating and lower ceramic coating, PMMA slurry made from step 2 is coated on upper ceramic coating, obtains PMMA
PVDF made from step 3 and its copolymer pulp are coated on lower ceramic coating by coating, obtain PVDF and its copolymer coated,
I.e. a kind of composite diaphragm is applied by PMMA coating/upper ceramic coating/polypropylene monofilm/lower ceramic coating/PVDF and its copolymer
Layer composition.
Basement membrane with a thickness of 12 μm, upper ceramic coating with a thickness of 2 μm, lower ceramic coating with a thickness of 2 μm, PMMA coating
With a thickness of 1 μm, PVDF and its copolymer coated with a thickness of 1 μm.
Embodiment 4
A kind of preparation method of composite diaphragm, this method comprises the following steps, and raw material is in terms of mass fraction:
Step 1: preparing ceramic slurry for 60 parts of silica, 60 parts of deionized waters, 0.5 part of sodium carboxymethylcellulose and 3
Part polyvinyl alcohol, is dispersed with stirring 20min, obtains ceramic slurry；
Step 2: preparing PMMA slurry for 60 parts of PMMA, 60 parts of deionized water, 0.5 part of sodium carboxymethylcellulose and 3 parts
Polyvinyl alcohol is dispersed with stirring 20min, obtains PMMA slurry；
Step 3: preparation PVDF and its copolymer pulp by 60 parts of Kynoar-tetrafluoroethene, 60 parts of deionized waters,
0.5 part of sodium carboxymethylcellulose and 3 parts of polyvinyl alcohol, are dispersed with stirring 20min, obtain PVDF and its copolymer pulp；
Step 4: coating
Ceramic slurry made from step 1 is coated on the upper layer of polypropylene monofilm under as narrow slit type coating method
Layer, obtains ceramic coating and lower ceramic coating, PMMA slurry made from step 2 is coated on upper ceramic coating, obtains PMMA
PVDF made from step 3 and its copolymer pulp are coated on lower ceramic coating by coating, obtain PVDF and its copolymer coated,
I.e. a kind of composite diaphragm is applied by PMMA coating/upper ceramic coating/polypropylene monofilm/lower ceramic coating/PVDF and its copolymer
Layer composition.
Basement membrane with a thickness of 16 μm, upper ceramic coating with a thickness of 4 μm, lower ceramic coating with a thickness of 4 μm, PMMA coating
With a thickness of 2 μm, PVDF and its copolymer coated with a thickness of 2 μm.
Embodiment 5
A kind of preparation method of composite diaphragm, this method comprises the following steps, and raw material is in terms of mass fraction:
Step 1: preparing ceramic slurry for 55 parts of aluminum oxides, 70 parts of deionized waters, 1 part of sodium carboxymethylcellulose and 6
Part styrene-butadiene emulsion, is dispersed with stirring 50min, obtains ceramic slurry；
Step 2: preparing PMMA slurry for 55 parts of PMMA, 70 parts of deionized water, 1 part of sodium carboxymethylcellulose and 6 parts of fourths
Benzene lotion, is dispersed with stirring 50min, obtains PMMA slurry；
Step 3: preparing PVDF and its copolymer pulp for 55 parts of Kynoar-trifluoro-ethylenes, 70 parts of deionized waters, 1
Part sodium carboxymethylcellulose and 6 parts of styrene-butadiene emulsions, are dispersed with stirring 50min, obtain PVDF and its copolymer pulp；
Step 4: coating
Ceramic slurry made from step 1 is coated on polyethylene and polypropylene multi-layer composite membrane as gravure roll coating method
The upper and lower, obtain ceramic coating and lower ceramic coating, by PMMA slurry made from step 2 be coated on it is upper ceramics apply
Layer, obtain PMMA coating, PVDF made from step 3 and its copolymer pulp be coated on lower ceramic coating, obtain PVDF and its
Copolymer coated, i.e., a kind of composite diaphragm is by PMMA coating/upper ceramic coating/polyethylene and polypropylene multi-layer composite membrane/lower pottery
Porcelain coating/PVDF and its copolymer coated composition.
Basement membrane with a thickness of 18 μm, upper ceramic coating with a thickness of 2 μm, lower ceramic coating with a thickness of 2 μm, PMMA coating
With a thickness of 0.2 μm, PVDF and its copolymer coated with a thickness of 0.2 μm.
Embodiment 6
A kind of preparation method of composite diaphragm, this method comprises the following steps, and raw material is in terms of mass fraction:
Step 1: prepare ceramic slurry by 50 parts of aluminum oxides, 65 parts of deionized waters, 0.5 part of sodium carboxymethylcellulose and
2 parts of pure-acrylic emulsions, are dispersed with stirring 40min, obtain ceramic slurry；
Step 2: preparing PMMA slurry for 50 parts of PMMA, 65 parts of deionized water, 0.5 part of sodium carboxymethylcellulose and 2 parts
Pure-acrylic emulsion is dispersed with stirring 40min, obtains PMMA slurry；
Step 3: preparing PVDF and its copolymer pulp for 50 parts of Kynoar, 65 parts of deionized waters, 0.5 part of carboxymethyl
Sodium cellulosate and 2 parts of pure-acrylic emulsions, are dispersed with stirring 40min, obtain PVDF and its copolymer pulp；
Step 4: coating
Ceramic slurry made from step 1 is coated on polyethylene and polypropylene multi-layer composite membrane as gravure roll coating method
The upper and lower, obtain ceramic coating and lower ceramic coating, by PMMA slurry made from step 2 be coated on it is upper ceramics apply
Layer, obtain PMMA coating, PVDF made from step 3 and its copolymer pulp be coated on lower ceramic coating, obtain PVDF and its
Copolymer coated, i.e., a kind of composite diaphragm is by PMMA coating/upper ceramic coating/polyethylene and polypropylene multi-layer composite membrane/lower pottery
Porcelain coating/PVDF and its copolymer coated composition.
Basement membrane with a thickness of 10 μm, upper ceramic coating with a thickness of 3 μm, lower ceramic coating with a thickness of 3 μm, PMMA coating
With a thickness of 1 μm, PVDF and its copolymer coated with a thickness of 1 μm.
Comparative example 1
12 μm of polyethylene monolayer films
Comparative example 2
A kind of preparation method of composite diaphragm, this method comprises the following steps, and raw material is in terms of mass fraction:
Step 1: preparing ceramic slurry for 40 parts of boehmites, 50 parts of deionized waters, 0.1 part of sodium carboxymethylcellulose and 1 part
Styrene-acrylic emulsion is dispersed with stirring 30min, obtains ceramic slurry；
Step 2: coating
Ceramic slurry made from step 1 is coated on to the upper and lower of polyethylene monolayer film as spraying method, is obtained
Upper ceramic coating and lower ceramic coating, i.e., a kind of composite diaphragm is by upper ceramic coating/polyethylene monolayer film/lower ceramic coating group
At.
Basement membrane with a thickness of 12 μm, upper ceramic coating with a thickness of 2 μm, lower ceramic coating with a thickness of 2 μm.
Comparative example 3
A kind of preparation method of composite diaphragm, this method comprises the following steps, and raw material is in terms of mass fraction:
Step 1: preparing PMMA slurry for 40 parts of PMMA, 50 parts of deionized water, 0.1 part of sodium carboxymethylcellulose and 1 part
Styrene-acrylic emulsion is dispersed with stirring 30min, obtains PMMA slurry；
Step 2: preparation PVDF and its copolymer pulp by 40 parts of Kynoar-hexafluoropropenes, 50 parts of deionized waters,
0.1 part of sodium carboxymethylcellulose and 1 part of styrene-acrylic emulsion, are dispersed with stirring 30min, obtain PVDF and its copolymer pulp；
Step 3: coating
PMMA slurry made from step 1 is coated on to the upper layer of polyethylene monolayer film as spraying method, obtains PMMA painting
PVDF made from step 2 and its copolymer pulp, are coated on the lower layer of polyethylene monolayer film, obtain PVDF and its copolymer by layer
Coating, i.e., a kind of composite diaphragm is by PMMA coating/polyethylene monolayer film/PVDF and its copolymer coated forms.
Basement membrane with a thickness of 12 μm, PMMA coating with a thickness of 2 μm, PVDF and its copolymer coated with a thickness of 2 μm.
Performance test:
Imbibition rate: diaphragm is immersed into 2h in electrolyte, imbibition rate is calculated as follows:
In formula: W1, W2For the quality before and after imbibition.
Thermal contraction performance: diaphragm is cut into the square that side length is 10cm × 10cm, is put between two pieces of paper, outer clip two panels
Glass plate is put into 140 DEG C of high-temperature test chamber 1h, calculates laterally (TD), longitudinal (MD) percent thermal shrinkage and is calculated as follows:
In formula: L1, L2To be put into diaphragm size before and after high-temperature test chamber, tests 3 times and be averaged.
Performance test experiment such as table 1.
The test of 1 membrane properties of table
Show that composite diaphragm prepared by the present invention has preferable imbibition rate to electrolyte from 1 the performance test results of table,
The thermal contraction of 140 DEG C of lower diaphragm plates is significantly less than comparative example 1, comparative example 2 and comparative example 3.
Claims (7)
1. a kind of preparation method of composite diaphragm, which is characterized in that the preparation method includes the following steps that raw material is with quality
Number meter:
Step 1: preparing ceramic slurry
By 40 ~ 60 parts of inorganic material, 50 ~ 80 parts of deionized waters, 0.1 ~ 1 part of sodium carboxymethylcellulose and 1 ~ 6 part of binder, stirring
Disperse 10 ~ 60min, obtains ceramic slurry；
Step 2: preparation PMMA slurry
By 40 ~ 60 parts of PMMA, 50 ~ 80 parts of deionized waters, 0.1 ~ 1 part of sodium carboxymethylcellulose and 1 ~ 6 part of binder, it is dispersed with stirring
10 ~ 60min obtains PMMA slurry；
Step 3: preparation PVDF and its copolymer pulp
By 40 ~ 60 parts of PVDF and its copolymer, 50 ~ 80 parts of deionized waters, 0.1 ~ 1 part of sodium carboxymethylcellulose and 1 ~ 6 part of bonding
Agent is dispersed with stirring 10 ~ 60min, obtains PVDF and its copolymer pulp；
Step 4: coating
Ceramic slurry made from step 1 is coated on to the upper and lower of basement membrane as coating method, obtain ceramic coating and
PMMA slurry made from step 2 is coated on upper ceramic coating, obtains PMMA coating by lower ceramic coating, will be made from step 3
PVDF and its copolymer pulp are coated on lower ceramic coating, obtain PVDF and its copolymer coated, i.e., a kind of composite diaphragm by
PMMA coating/upper ceramic coating/basement membrane/lower ceramic coating/PVDF and its copolymer coated composition.
2. a kind of preparation method of composite diaphragm according to claim 1, which is characterized in that the inorganic material is two
At least one of silica, aluminum oxide, magnesia, calcium oxide, boehmite and titanium dioxide.
3. a kind of preparation method of composite diaphragm according to claim 1, which is characterized in that the binder is phenylpropyl alcohol
At least one of lotion, pure-acrylic emulsion, styrene-butadiene emulsion, ethylene-vinyl acetate copolymer emulsion and polyvinyl alcohol.
4. a kind of preparation method of composite diaphragm according to claim 1, which is characterized in that the PVDF and its copolymerization
Object be Kynoar, Kynoar-trifluoro-ethylene, Kynoar-tetrafluoroethene, Kynoar-hexafluoroethylene and
At least one of Kynoar-hexafluoropropene.
5. a kind of preparation method of composite diaphragm according to claim 1, which is characterized in that the basement membrane is polyethylene
Monofilm, polypropylene monofilm and one of polyethylene and polypropylene multi-layer composite membrane.
6. a kind of preparation method of composite diaphragm according to claim 1, which is characterized in that the basement membrane with a thickness of
5 ~ 20 μm, upper ceramic coating with a thickness of 0.5 ~ 4 μm, lower ceramic coating with a thickness of 0.5 ~ 4 μm, PMMA coating with a thickness of
0.2 ~ 2 μm, PVDF and its copolymer coated with a thickness of 0.2 ~ 2 μm.
7. a kind of preparation method of composite diaphragm according to claim 1, which is characterized in that the coating method is recessed
One of roller coating, narrow slit type coating, anilox roll coating, Slot-die coating and spraying.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113193303A (en) * | 2021-04-16 | 2021-07-30 | 江西京九动力能源有限公司 | Composite diaphragm for lithium battery and preparation method thereof |
| WO2024008055A1 (en) * | 2022-07-04 | 2024-01-11 | 中材锂膜有限公司 | Porous separator and preparation method therefor, and electrochemical device |
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| WO2024008055A1 (en) * | 2022-07-04 | 2024-01-11 | 中材锂膜有限公司 | Porous separator and preparation method therefor, and electrochemical device |
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Application publication date: 20190503 |