CN109841781A - A kind of preparation method of battery diaphragm and its battery diaphragm of preparation - Google Patents
A kind of preparation method of battery diaphragm and its battery diaphragm of preparation Download PDFInfo
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- CN109841781A CN109841781A CN201711211025.6A CN201711211025A CN109841781A CN 109841781 A CN109841781 A CN 109841781A CN 201711211025 A CN201711211025 A CN 201711211025A CN 109841781 A CN109841781 A CN 109841781A
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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 provides a kind of preparation methods of battery diaphragm, including polyphenylene sulfide, polyphenylsulfone, sulfate are blended uniformly at 290~350 DEG C;It is prepared into flaky material;It is immersed in leachate, dissolution removal polyphenylsulfone;It is immersed in aqueous liquid, removes removing sulfate.Method of the invention uses polyphenylene sulfide, polyphenylsulfone, sulfuric acid salt blend, be conducive to that polyphenylene sulfide and polyphenylene sulfone blends is made to form co-cable transmission using sulfate, and the lesser feature of phase size, removal polyphenylsulfone is etched by leachate again, water etching removes removing sulfate, prepares the excellent battery diaphragm of void content, ventilative resistance, puncture intensity, tensile strength, anti-flammability properties.
Description
Technical field
The present invention relates to the preparation methods of plastic film technical field more particularly to a kind of battery diaphragm and prepared therefrom
Battery diaphragm.
Background technique
Currently, lithium ion battery generally uses micropore polyolefin barrier diaphragm, reason is micropore polyolefin barrier diaphragm reasonable
Good mechanical performance and chemical stability can be provided in cost-range, the conventional use of requirement of lithium ion battery can be met.
But polyalkene diaphragm fusing point is low, poor fire, is easily deformed fusing under the high temperature conditions and burns, and influences the peace of lithium ion battery
Full property and service life.
Chinese patent application CN201410445356.6 discloses the lithium electricity of a kind of ceramics and gelatin polymer MULTILAYER COMPOSITE
Pond diaphragm and preparation method thereof, it is compound by polypropylene (PP) and polyethylene (PE), water distribution is successively applied on composite base material surface
Property ceramic coating and aqueous PVDF slurry method four layers of composite diaphragm obtaining thermal safety height and keep electrolyte ability strong.
Chinese patent application CN201310497095.8 be successively coated outside PP or PE diaphragm oxide coating, aramid fiber resinous coat and
PVDF-HEP copolymer layer improves the mechanical property and heat resistance of diaphragm.Chinese patent application CN201380016862.2
It is one layer of microcellular structure being made of aromatic polyamide, gelatin polymer, metal oxide of coating on MIcroporous polyolefin film.
Chinese patent application CN201380016862.7 is laminated on the perforated membrane comprising polyolefin resin comprising polyamide acyl
Imines resinoid and battery separator containing inorganic particulate or cross-linked polymer particle perforated membrane.The above-mentioned prior art be all
Polyethylene is modified on basis, can not change the disadvantage of polyethylene anti-flaming difference, and complex process higher cost, batch
Stability is poor.
Summary of the invention
The purpose of the present invention is to solve the above-mentioned problems of the prior art, and provide a kind of preparation of battery diaphragm
Method and the battery diaphragm of preparation.
The preparation method of battery diaphragm provided by the invention, comprising the following steps:
Polyphenylene sulfide, polyphenylsulfone, sulfate are blended uniformly step A at 290~350 DEG C;
Obtained blend is prepared into flaky material by step B;
Obtained flaky material is immersed in leachate by step C, dissolution removal polyphenylsulfone;
Flaky material after removal polyphenylsulfone is immersed in aqueous liquid, removes removing sulfate by step D.
Wherein, polyphenylene sulfide (PPS) is the thermoplastic resin that thiophenyl is had in polymer molecule backbone, and chemical property is steady
Fixed, solvent resistance is strong, can guarantee battery diaphragm insoluble, insoluble bulging deformation in the electrolytic solution.And polyphenylene sulfide fusing point reaches
281 DEG C, heat distortion temperature is generally higher than 260 DEG C, can use in 180~220 DEG C of temperature ranges, has very high anti-flammability, resistance to
It is hot and rigid.
Polyphenylsulfone is to contain phenylene-SO in molecular backbone2The thermoplastic resin of phenylene chain link can provide excellent
Different impact resistance and high intensity.
Sulfate is by sulfate ion (SO4 2-) with other metals, nonmetallic ion form compound.Apply for human hair
The addition of existing sulfate, makes polyphenylene sulfide and polyphenylsulfone co-cable transmission easy to form (Co-continuous Phases),
And phase size is smaller;The characteristics of recycling sulfate to be dissolved in water can prepare emptying aperture after the sulfate of addition is dissolved in elutriation out
Rate is greater than 20%, ventilative resist and is less than 700s/20 μm, and puncture intensity is greater than 1500mN/20 μm, and tensile strength is greater than 125MPa
The battery diaphragm based on polyphenylene sulfide.
Wherein, sulfate is selected from one of sodium sulphate, potassium sulfate, magnesium sulfate, aluminum sulfate or a variety of.
In the present invention, when the blending temperature of polyphenylene sulfide, polyphenylsulfone, sulfate in step A is less than 290 DEG C, body
Not exclusively, co-mixing system is uneven, and material property is bad for system's melting.When blending temperature is greater than 350 DEG C, energy needed for heating systems
Source increases, but can not improve the blending effect of system and the performance of material, increases cost of manufacture.
Wherein, in step A in terms of 100 parts by weight of polyphenylene sulfide, 200~400 parts by weight of polyphenylsulfone work as polyphenylene
When sulfone is less than 200 parts by weight, polyphenylene sulfide and polyphenylsulfone are difficult to form co-cable transmission, are difficult to dissolve removal using leachate
The polyphenylsulfone phase mutually wrapped up by polyphenylene sulfide, obtained product void content is small, and air permeability is low;When polyphenylsulfone is greater than
When 400 parts by weight, polyphenylene sulfide easily becomes dispersed phase, is mutually wrapped up by polyphenylsulfone, obtained product puncture intensity, stretch it is strong
It spends low or even shapeless.Polyphenylsulfone preferably 250~350 parts by weight.
Wherein, in step A in terms of 100 parts by weight of polyphenylene sulfide, otherwise sulfate 50-150 parts by weight are unfavorable for polyphenylene sulfide
Ether and polyphenylsulfone form co-cable transmission.The preferred 80-120 parts by weight of sulfate.
Further, leachate described in step C is selected from one or both of sulfolane, n,N-dimethylacetamide.
Wherein, leachate is for dissolving the removal not polyphenylsulfone compatible with polyphenylene sulfide system.Sulfolane, N, N-
The removal rate for the polyphenylsulfone dissociated in system can be improved in dimethyl acetamide.Preferably comprise sulfolane, N, N- dimethyl
The mixture of acetamide, the two weight ratio are 1: 5~5: 1, preferably 1: 2~2: 1.
Further, dipping temperature is the freezing point of leachate or more, 180 DEG C or less in step C.When dipping temperature is greater than
When equal to 180 DEG C, system will appear void collapse, polyphenylsulfone dissolves the problems such as incomplete, to influence the mechanics of diaphragm
Performance and using effect.Dipping temperature is preferably the freezing point of leachate or more, 150 DEG C or less.
Further, step C further includes applying uniaxial or biaxial stretching to the flaky material after removal polyphenylsulfone, is drawn
Stretching temperature is 100~200 DEG C, and the stretching ratio on single direction is 1~10 times.Simple tension refers to film in one direction
It is stretched, draw direction is generally the longitudinal direction (MD) or lateral (TD) of film.Biaxial tension, which refers to, is mutually perpendicular to film edge
Both direction stretched, draw direction be generally film longitudinal direction (MD) and laterally (TD).Biaxial tension is suitable according to stretching
Sequence, and can be divided into and simultaneously bi-directionally stretch and gradually biaxial tension, the former refers to film in both directions while stretching,
The latter refers to film is first stretched along direction after, then stretch along another direction.
When draft temperature is less than 100 DEG C, tensile strength of material is larger, it is difficult to be stretched, when draft temperature is greater than 200 DEG C
When, it is unfavorable for Uniform Tension;When the stretching ratio on single direction is greater than 10, it is unfavorable for the raising of void content and air permeability.
It is preferred that draft temperature is 130~160 DEG C, the stretching ratio on single direction is 2~6 times.
Further, step C further includes applying uniaxial or biaxial stretching to the flaky material being immersed in leachate to stretch,
Draft temperature (i.e. dipping temperature) is 100~180 DEG C, and the stretching ratio on single direction is 1~10 times.
Dipping carries out simultaneously with stretching, and one side saving prepares room and time, and energy saving, reduces cost;It is another
Aspect, it has been found that the product stretched in leachate is than first stretching is produced in leachate immersion, then in air
Object has bigger void content, more preferably air permeability, while puncture intensity and tensile strength are also higher.It is preferred that draft temperature is
130~160 DEG C, the stretching ratio on single direction is 2~6 times.
Further, in the aqueous liquid in the preparation method step D of the battery diaphragm, also contain ethyl alcohol.Ethyl alcohol
Solution can be improved to the wetability of co-mixing system and can sufficiently infiltrate film, the removal rate of sulfate and gone in raising system
Except rate.The volume of preferred alcohol is the 20%~100% of the volume of water.
Further, the preparation method of the battery diaphragm also includes step E, and it is fixed to carry out heat to the sample that step D is obtained
Type, heat setting temperature are 1~20 DEG C higher than draft temperature.
Wherein, thermal finalization refers to is heat-treated the flaky material after stretching at least once, makes its crystallization-stable, allows
The more uniform stable process of the structure and performance of material.Maximum temperature when being heat-treated to material that heat setting temperature refers to.
It is preferred that heat setting temperature is 10~20 DEG C higher than draft temperature.
The present invention provides a kind of battery diaphragm according to made of above-mentioned preparation method.
Further, the void content of the battery diaphragm is greater than 20%, ventilative resist and is less than 700s/20 μm, puncture intensity
Greater than 1500mN/20 μm, tensile strength is greater than 125MPa.
Wherein, void content is the volume percentage of the total volume of perforated membrane hollow hole.Ventilative resistance is the table of air permeability
Sign refers to the gas of certain volume through the time required for sample, and breathing freely, it is bigger to resist, and air permeability is lower.Puncture intensity refers to
Required power when with Special test needle-penetration unit thickness film, reactive film resist the ability that blunt penetrates.Tensile strength is
The maximum nominal tensile stress that sample is born before breaking, characterizes the fracture resistance of material.Preferably, the void content of the battery diaphragm
It is less than 500s/20 μm greater than 40%, ventilative resist, puncture intensity is greater than 2500mN/20 μm, and tensile strength is greater than 150MPa.
The preparation method of battery diaphragm of the invention uses polyphenylene sulfide, polyphenylsulfone, sulfuric acid salt blend, and utilization is specific
Sulfate be conducive to make polyphenylene sulfide and polyphenylene sulfone blends to form co-cable transmission, and the lesser feature of phase size, then
Removal polyphenylsulfone is etched by leachate, water etching removes removing sulfate, and further combined with stretching technique, prepares emptying aperture
Rate, ventilative resistances, puncture intensity, tensile strength, anti-flammability properties it is excellent based on polyphenylene sulfide with fire-retardant
Property battery diaphragm (void content is greater than 20%, it is ventilative resist be less than 700s/20 μm, puncture intensity is greater than 1500mN/20 μm, draws
Intensity is stretched greater than 125MPa).
Battery diaphragm of the invention can be used for lithium battery, especially automobile lithium battery and mobile phone lithium battery.
Specific embodiment
The present invention is further illustrated below by the mode of embodiment, does not therefore limit the present invention to the embodiment
Among range.
It is of the present invention " more than ", " following " include this number, " being greater than ", " being less than " are not comprising this number.
Parameter involved in the embodiment of the present invention and comparative example and its measuring method are as follows:
Void content: by mercury injection method measurement in GB/T 21650.1-2008.
Ventilative to resist: standardization air permeability is measured according to JIS P8117, using formula A=20 μ m (X)/T1 by its result
It is standardized as the air permeability values of the same film with 20 μ m thicks.In formula, X is the reality of the air permeability of the film with actual (real) thickness T1
Measured value, A are the standardization air permeability of the same film with 20 μ m thicks.
Puncture intensity: it is carried out according to described in GB/T10004-2008, it may be assumed that be mounted on the test piece that diameter is 100mm
On sample film clamping ring, diameter 1.0mm is then used, diameter tip radius is the steel needle of 0.5mm, with the speed of (50 ± 5) mm/min
Degree goes to top to pierce, and reads the peak load that steel needle penetrates test piece.Test the piece number 5 or more, takes its arithmetic mean of instantaneous value.
Tensile strength: it is carried out according to GB/T 1040.3-2006, speed of experiment 10mm/min.Specimen types are 2 types, size
Long 150mm × wide 10mm.For unidirectional and biaxial tension sample, the tensile strength on the direction MD is tested.
Anti-flammability: it is tested according to UL94 (vertical checkout) standard.
Embodiment 1~11
According to the composition of raw materials in Tables 1 and 2, battery diaphragm sample is produced in accordance with the following steps:
Polyphenylene sulfide, polyphenylsulfone, sulfate are blended uniformly step A at 290~350 DEG C;
Blend is prepared into flaky material by moulding press by step B;
Flaky material is immersed in 10min in leachate, dissolution removal polyphenylsulfone by step C;Wherein, embodiment 10
In 11, the weight ratio of sulfolane and n,N-dimethylacetamide is 1: 1;
Flaky material after removal polyphenylsulfone is immersed in aqueous liquid, removes removing sulfate by step D, is made
Thickness is about 40 microns of sample;Wherein, in embodiment 11, the volume of ethyl alcohol is the 50% of water.
1 Examples 1 to 5 formula of table (by polyphenylene sulfide be 100 parts by weight in terms of.: expression does not contain;Zero: expression contains)
2 embodiment 6~11 of table formula (by polyphenylene sulfide be 100 parts by weight in terms of.: expression does not contain;Zero: expression contains)
Embodiment 12~16
On the basis of using the same materials and preparation method of embodiment 11, obtained after removing polyphenylsulfone to step C
To flaky material apply uniaxial or biaxial stretching in hot-air.The draft temperature and stretching ratio of embodiment 12~16 are as follows
Shown in table 3.Wherein, stretching ratio 2 × 1 indicates that the stretching ratio that the stretching ratio in the direction MD is the direction 2, TD is 1.
3 embodiment of table, 12~16 draft temperature and stretching ratio
Classification | Embodiment 12 | Embodiment 13 | Embodiment 14 | Embodiment 15 | Embodiment 16 |
Draft temperature (DEG C) | 100 | 200 | 130 | 160 | 145 |
Drawing process | Simple tension | Simple tension | Simultaneously bi-directionally stretch | Simultaneously bi-directionally stretch | Simultaneously bi-directionally stretch |
Stretching ratio | 2×1 | 10×1 | 3×3 | 6×2 | 5×3 |
Remarks: unidirectional and biaxial tension direction is MD × TD.
Embodiment 17~22
On the basis of using the same materials and preparation method of embodiment 11, leached in step C while to being immersed in
Flaky material in liquid applies uniaxial or biaxial stretching, and adds step E, carries out thermal finalization to obtained sample.Embodiment 17
~22 stretching ratio and heat setting temperature is as shown in table 4 below.
4 embodiment of table, 17~22 draft temperature, stretching ratio and heat setting temperature
Comparative example 1~5
On the basis of using 5 identical preparation method of embodiment, composition of raw materials and component are as shown in table 5.Wherein, comparative example
Step C is not included in 3 preparation process;Sulfate is not used in the preparation process of comparative example 4, does not include step D yet;Comparative example
Polyphenylsulfone, sulfate are not used in 5 preparation process, do not include step C, D yet.
5 comparative example 1~5 of table formula (by polyphenylene sulfide be 100 parts by weight in terms of)
Diaphragm prepared by embodiment 1~17 and comparative example 1~5 is tested for the property, test result is as shown in table 6.
Each embodiment and comparative example membrane properties test result of table 6
As described in Table 6, the battery diaphragm of preparation method preparation provided by the invention has excellent air permeability, anti-flammability, resists
Puncture intensity and tensile strength.And the battery diaphragm void content of the production of comparative example 1,3,4,5 is low, permeability is bad, is unfavorable for
Substance shifts in battery, and battery efficiency is not high;Though the various aspects of performance of the battery diaphragm of comparative example 2 is met the requirements, it is made
Blending temperature is higher during standby, but performance does not correspondingly increase but, waste of resource, uneconomical practical.
Claims (10)
1. a kind of preparation method of battery diaphragm, which comprises the following steps:
Polyphenylene sulfide, polyphenylsulfone, sulfate are blended uniformly step A at 290~350 DEG C;
Obtained blend is prepared into flaky material by step B;
Obtained flaky material is immersed in leachate by step C, dissolution removal polyphenylsulfone;
Flaky material after removal polyphenylsulfone is immersed in aqueous liquid, removes removing sulfate by step D.
2. the preparation method of battery diaphragm according to claim 1, it is characterised in that: with 100 weight of polyphenylene sulfide in step A
Measure part meter, 200~400 parts by weight of polyphenylsulfone, sulfate 50-150 parts by weight.
3. the preparation method of battery diaphragm according to claim 2, it is characterised in that: with 100 weight of polyphenylene sulfide in step A
Measure part meter, 250~350 parts by weight of polyphenylsulfone, sulfate 80-120 parts by weight.
4. the preparation method of battery diaphragm according to claim 1, it is characterised in that: the sulfate be selected from sodium sulphate,
One of potassium sulfate, magnesium sulfate, aluminum sulfate are a variety of.
5. the preparation method of battery diaphragm according to claim 1, it is characterised in that: leachate described in step C is selected from
One or both of sulfolane, n,N-dimethylacetamide, dipping temperature are the freezing point of leachate or more, 180 DEG C or less.
6. the preparation method of battery diaphragm according to claim 5, it is characterised in that: leachate described in step C is ring
The mixture of fourth sulfone, n,N-dimethylacetamide, the two weight ratio are 1: 5~5: 1, dipping temperature be the freezing point of leachate with
Above, 150 DEG C or less.
7. the preparation method of battery diaphragm according to claim 1, it is characterised in that: step C further includes to the poly- Asia of removal
The flaky material obtained after phenylsulfone applies uniaxial or biaxial stretching, and draft temperature is 100~200 DEG C, the drawing on single direction
Stretching multiplying power is 1~10 times.
8. the preparation method of battery diaphragm according to claim 1, it is characterised in that: step C further includes to being immersed in
The flaky material in liquid applies uniaxial or biaxial stretching out, and draft temperature is 100~180 DEG C, the stretching ratio on single direction
It is 1~10 times.
9. the preparation method of battery diaphragm according to claim 7 or 8, it is characterised in that: the preparation of the battery diaphragm
Method also includes step E, carries out thermal finalization to obtained sample, heat setting temperature is 1~20 DEG C higher than draft temperature.
10. a kind of according to claim 1 to battery diaphragm made from any one of 9 preparation methods.
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Cited By (1)
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CN113948818A (en) * | 2021-11-17 | 2022-01-18 | 北京胜能能源科技有限公司 | Polyphenylene sulfide composite diaphragm and preparation method and application thereof |
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