CN106252564A - A kind of preparation method of high puncture strength lithium ion battery separator - Google Patents
A kind of preparation method of high puncture strength lithium ion battery separator Download PDFInfo
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- CN106252564A CN106252564A CN201610806084.7A CN201610806084A CN106252564A CN 106252564 A CN106252564 A CN 106252564A CN 201610806084 A CN201610806084 A CN 201610806084A CN 106252564 A CN106252564 A CN 106252564A
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- ion battery
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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
- H01M50/446—Composite material consisting of a mixture of organic and inorganic materials
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical Kinetics & Catalysis (AREA)
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- Materials Engineering (AREA)
- Composite Materials (AREA)
- Inorganic Chemistry (AREA)
- Cell Separators (AREA)
Abstract
The invention provides the preparation method of a kind of high puncture strength lithium ion battery separator, including: poly-for high isotactic 1 butylene is mixed with antioxidant, after stirring, obtains the first mixture；Described first mixture is put in extrusion casting apparatus and carry out slab, obtain precursor film；Described precursor film is carried out heat treatment, longitudinal stretching, obtains lithium ion battery separator.Compared with prior art, the present invention utilizes high isotactic resin directly to carry out being cast, stretching, it is to avoid the situations such as uneven thickness occur, and it is uniform, without the brilliant feature put that the lithium ion battery separator of preparation has thickness.Second, there is due to poly-1 butylene of high isotactic the features such as prominent heat-resisting creep properties, environmental stress crack resistance and good toughness, it is ensured that the lithium ion battery separator of preparation has higher high puncture strength.Again, the preparation technology of the present invention is simple, it is adaptable to industrialized production.Test result indicate that, the puncture strength of lithium ion battery separator prepared by the present invention is at more than 430g.
Description
Technical field
The present invention relates to technical field of lithium ion, particularly relate to the system of a kind of high puncture strength lithium ion battery separator
Preparation Method.
Background technology
Along with the development of information technology, the demand of portable power source is the most quickly increased by we, meanwhile, with conventional batteries phase
Ratio, the direction of demand also there occurs transformation: energy is high, volume is little, lightweight, security performance is high, has had become as portable power source
The new direction of development.The advantage such as have that monomer voltage is high, specific energy high due to lithium ion battery and self discharge is little, therefore by extensively
It is applied to the fields such as digital product, electric tool and electric automobile.
The barrier film of business-like lithium ion battery is mostly and uses PP or PE is raw material, passes through uniaxial or biaxial stretching
It is prepared from.In the assembling process of lithium ion battery, needing both positive and negative polarity and barrier film are wrapped up folding repeatedly, this process can
Can make diaphragm tears, cause battery short circuit, the safety to lithium ion battery affects, and therefore improves lithium ion
The puncture strength of battery diaphragm, can reduce the tear ratio of barrier film, and reduce the fraction defective of assembled battery.
At present, the main method improving lithium ion battery separator puncture strength is to select high molecular weight polypropylene resin, example
As, the Chinese patent literature of Application No. 201210472283.0 reports the polypropylene power lithium battery that a kind of mechanical strength strengthens
Pond barrier film and preparation method thereof, modifying agent is inorganic nano-particle and nucleator, and wherein the percentage by weight of acrylic resin is
85%-95%, the percentage by weight of inorganic nano-particle is 5%-10%, and the percentage by weight of nucleator is 1%-3%.But
It is that it exists the problem being difficult to plastify in the course of processing, is easily generated brilliant point, the unfavorable condition such as uneven thickness.
Summary of the invention
Present invention solves the technical problem that the preparation method being to provide a kind of lithium ion battery separator, technique is simple, system
Standby lithium ion battery separator has high puncture strength, and thickness is uniform.
In view of this, the invention provides the preparation method of a kind of high puncture strength lithium ion battery separator, including following
Step: high isotactic poly 1-butene is mixed by step a) with antioxidant, obtains the first mixture after stirring；Step b) is by described
One mixture is put in extrusion casting apparatus and is carried out slab, obtains precursor film；Step c) by described precursor film at 80-180
Carry out heat treatment, longitudinal stretching at DEG C, obtain lithium ion battery separator.
Preferably, the isotacticity of described high isotactic poly 1-butene is 95%.
Preferably, described antioxidant is antioxidant 1076.
Preferably, described high isotactic poly 1-butene is 100-300:1 with the mass ratio of antioxidant.
Preferably, in step b, the temperature of the extruder of extrusion casting apparatus is 160-290 DEG C, and die head temperature is 160-
269 DEG C, casting roller temperature is 50-180 DEG C.
Preferably, the thickness of described precursor film is 10-50 μm.
Preferably, in step c, the time of heat treatment is 150-1000 minute.
Preferably, the draft temperature of described longitudinal stretching is 120-250 DEG C, and stretching ratio is 0.5-5.0.
Preferably, also include: the polypropylene agglomerate containing calcium hydroxide is melted, be coated in described lithium ion battery separator
On, coat thickness is 15-30 micron, obtains compound non-porous film after placement；By described compound non-porous film in being placed in hydrochloric acid, leaching
Bubble.
Preferably, in described polypropylene agglomerate, the weight ratio of polypropylene and calcium hydroxide is 10-20:1.
The invention provides the preparation method of a kind of high puncture strength lithium ion battery separator, including: high isotactic is gathered
1-butylene mixes with antioxidant, obtains the first mixture after stirring；Put into described first mixture in extrusion casting apparatus
Row slab, obtains precursor film；Described precursor film is carried out at 80-180 DEG C heat treatment, longitudinal stretching, obtains lithium ion
Battery diaphragm.Compared with prior art, the present invention utilizes high isotactic resin directly to carry out being cast, stretching, it is to avoid thickness occur
Unequal situation, it is uniform, without the brilliant feature put that the lithium ion battery separator of preparation has thickness.Second, owing to high isotactic gathers
1-butylene has the features such as prominent heat-resisting creep properties, environmental stress crack resistance and good toughness, it is ensured that the lithium of preparation
Ion battery barrier film has higher high puncture strength.Secondly, the preparation technology of the present invention is simple, it is adaptable to industrialized production.
Test result indicate that, the puncture strength of lithium ion battery separator prepared by the present invention is at more than 430g.
Detailed description of the invention
In order to be further appreciated by the present invention, below in conjunction with embodiment, the preferred embodiment of the invention is described, but
Should be appreciated that these describe simply as to further illustrate the features and advantages of the present invention rather than to the claims in the present invention
Limit.
The embodiment of the invention discloses the preparation method of a kind of high puncture strength lithium ion battery separator, including following step
Rapid: high isotactic poly 1-butene is mixed by step a) with antioxidant, obtain the first mixture after stirring；Step b) is by described first
Mixture is put in extrusion casting apparatus and is carried out slab, obtains precursor film；Step c) by described precursor film at 80-180 DEG C
Under carry out heat treatment, longitudinal stretching, obtain lithium ion battery separator.
High isotactic poly 1-butene is referred to as " plastics gold ", has prominent heat-resisting creep properties, resisting environmental stress and cracking
Property and good toughness.The present invention is with high isotactic poly 1-butene as raw material, and the lithium ion battery separator of preparation has higher
High puncture strength.Preferably, the isotacticity of described high isotactic poly 1-butene is preferably 95%.
Preferably, described antioxidant is antioxidant 1076.The production of the present invention antioxidant 1076 for using
Producer is not particularly limited.Meanwhile, the mass ratio of described high isotactic resin with antioxidant is controlled, preferably by the present invention
For 100-300:1, more preferably 120-280:1, more preferably 200:1.
The present invention utilizes high isotactic resin directly to carry out being cast, stretching, it is to avoid the situations such as uneven thickness occur.As excellent
Selecting scheme, in step b, the temperature of the extruder of extrusion casting apparatus is preferably 160-290 DEG C, more preferably 180-280 DEG C, more
It is preferably 200-270 DEG C；Die head temperature is preferably 160-269 DEG C, more preferably 180-260 DEG C, more preferably 200-255 DEG C；
Casting roller temperature is preferably 50-180 DEG C, more preferably 100-180 DEG C, more preferably 120-175 DEG C.The thickness of described precursor film
Degree is preferably 10-50 μm, more preferably 20-40 μm.
Then, the present invention precursor film to obtaining carries out heat treatment, to eliminate crystalline region defect, improves and takes phase platelet knot
Structure, thus improve puncture strength.According to micropore formation basic theory, curtain coating basement membrane takes the factor of phase lamellar structure degree of perfection, except
Outside casting technique, also include heat treatment condition, including heat treatment temperature, heat treatment time etc..The present invention passes through heat treatment, changes
Sub-chain motion in crystalline region defect, plays the effect improving puncture strength.Preferably, in step c, the temperature of heat treatment is excellent
Elect 100-180 DEG C as, more preferably 120-180 DEG C, more preferably 170-180 DEG C；The time of heat treatment is preferably 150-1000
Minute, more preferably 300-800 minute, more preferably 500-700 minute.
After heat treatment completes, the present invention carries out longitudinal stretching to precursor film.By longitudinal stretching, make orientations sheet
It is separated from each other after brilliant flexural deformation, forms micropore.Preferably, the draft temperature of described longitudinal stretching is preferably 120-
250 DEG C, more preferably 140-220 DEG C；Stretching ratio is preferably 0.5-5.0, more preferably 2-4.
In order to improve the intensity of the lithium ion battery separator of preparation further, the present invention further preferably includes: will be containing hydrogen-oxygen
The polypropylene agglomerate changing calcium melts, and being coated in coat thickness on described lithium ion battery separator is 15-30 micron, after placement
To compound non-porous film；By described compound non-porous film in immersing hydrochloric acid, soak.Wherein, in described polypropylene agglomerate polypropylene and
The weight ratio of calcium hydroxide is preferably 10-20:1, more preferably 12-18:1；Coat thickness is preferably 20-30 micron；Place
Time is preferably 1-3 hour, more preferably 1-2 hour；Soak time is preferably 60-120 minute, more preferably 90 minutes.
In above-mentioned preferred version, the present invention is not particularly limited for the mode of coating, includes but not limited to following
Various method well known in the art, such as: spin-coating method, knife coating, the tape casting or dip coating etc., wants according to film thickness
Ask, adjust coated weight, finally make the lithium ion battery separator of preparation reach thickness requirement.
By above-mentioned preferred process, the lithium ion battery separator of preparation forms double-layer structure, and polyolefin porous membrane layer bonds
On poly 1-butene film layer, there is the strongest inter-layer bonding force, further increase lithium ion battery separator puncture strength.
From above scheme it can be seen that the present invention utilizes high isotactic resin directly to carry out being cast, stretching, it is to avoid thickness occurs
Spending unequal situation, it is uniform, without the brilliant feature put that the lithium ion battery separator of preparation has thickness.Second, due to high isotactic
Poly 1-butene has the features such as prominent heat-resisting creep properties, environmental stress crack resistance and good toughness, it is ensured that preparation
Lithium ion battery separator has higher high puncture strength.Secondly, the preparation technology of the present invention is simple, it is adaptable to industry metaplasia
Produce.Lithium ion battery separator prepared by the present invention has high puncture strength, can be applicable to prepare the barrier film of lithium ion battery, especially
For lithium-ion power battery dissepiment, be conducive to improving the safety of lithium ion battery.
In order to be further appreciated by the present invention, the technical scheme provided the present invention below in conjunction with embodiment is carried out specifically
Bright, protection scope of the present invention is not limited by the following examples.
In following example, poly 1-butene resin uses film-grade High isotactic polybutene-1, and melt index is 4.0g/
10min (2.16kg), isotacticity is 95%, density 0.85g/cm3.Other auxiliary agent during preparation casting films, antioxidant 1076
Addition is 0.5%.
Embodiment 1
Precise poly 1-butene: 200kg, antioxidant 1076: 1kg, mixing.Presoma is prepared by casting apparatus slab
Film A, extruder temperature: 250 DEG C, die head temperature: 200 DEG C, casting roller temperature: 140 DEG C, die head aperture: 2.0mm, it is cast thickness
Degree: 20um, rolling length: 1500m.
Precursor film A is put into constant temperature oven and carries out heat treatment, heat treatment temperature: 170 DEG C, heat treatment time: 500 points
Clock.
Precursor film A through Overheating Treatment is stretched, prepares lithium ion battery separator, stretch rate: 3.0,
Draft temperature 165 DEG C, setting temperature 175 DEG C.
Embodiment 2
Precise poly 1-butene: 100kg, antioxidant 1010: 0.5kg, mixing.Forerunner is prepared by casting apparatus slab
Body film B, extruder temperature: 285 DEG C, die head temperature: 255 DEG C, casting roller temperature: 175 DEG C, die head aperture: 3.5mm, casting films
Thickness: 30um, rolling length: 1500m.
Precursor film B is put into constant temperature oven and carries out heat treatment, heat treatment temperature: 180 DEG C, heat treatment time: 700 points
Clock.
Precursor film B through Overheating Treatment is stretched, prepares lithium ion battery separator, stretch rate: 3.5,
Draft temperature 170 DEG C, setting temperature 180 DEG C.
Embodiment 3
Precise poly 1-butene: 200kg, antioxidant 1076: 1kg.Precursor film C is prepared by casting apparatus slab,
Extruder temperature: 250 DEG C, die head temperature: 200 DEG C, casting roller temperature: 140 DEG C, die head aperture: 2.0mm, casting films thickness:
20um, rolling length: 1500m.
Precursor film C is put into constant temperature oven and carries out heat treatment, heat treatment temperature: 170 DEG C, heat treatment time: 500 points
Clock.
Precursor film C through Overheating Treatment is stretched, prepares lithium ion battery prefabricated membrane, stretch rate:
3.0, draft temperature 165 DEG C, setting temperature 175 DEG C.
After melted for the polypropylene agglomerate containing calcium hydroxide, it is coated on lithium ion battery prefabricated membrane, coat thickness
It is 15 microns, places at normal temperatures and obtain compound non-porous film after 1 hour, polypropylene and calcium hydroxide in described polypropylene agglomerate
Weight ratio is 20:1；
Compound non-porous film is completely immersed in the hydrochloric acid of concentration 10% at 25 DEG C, soaks 90 minutes, completely remove hydrogen-oxygen
Take out after changing calcium, obtain lithium ion battery separator.
Embodiment 4
Precise poly 1-butene: 200kg, antioxidant 1076: 1kg.Precursor film D is prepared by casting apparatus slab,
Extruder temperature: 250 DEG C, die head temperature: 200 DEG C, casting roller temperature: 140 DEG C, die head aperture: 2.0mm, casting films thickness:
20um, rolling length: 1500m.
Precursor film D is put into constant temperature oven and carries out heat treatment, heat treatment temperature: 170 DEG C, heat treatment time: 500 points
Clock.
Precursor film D through Overheating Treatment is stretched, prepares lithium ion battery prefabricated membrane, stretch rate:
3.0, draft temperature 165 DEG C, setting temperature 175 DEG C.
After melted for the polypropylene agglomerate containing calcium hydroxide, it is coated on lithium ion battery prefabricated membrane, coat thickness
It is 20 microns, places at normal temperatures and obtain compound non-porous film after 1 hour, polypropylene and calcium hydroxide in described polypropylene agglomerate
Weight ratio is 15:1；
Compound non-porous film is completely immersed in the hydrochloric acid of concentration 12% at 25 DEG C, soaks 90 minutes, completely remove hydrogen-oxygen
Take out after changing calcium, obtain lithium ion battery separator.
Embodiment 5
Precise poly 1-butene: 100kg, antioxidant 1010: 0.5kg.Precursor film is prepared by casting apparatus slab
E, extruder temperature: 285 DEG C, die head temperature: 255 DEG C, casting roller temperature: 175 DEG C, die head aperture: 3.5mm, casting films thickness:
30um, rolling length: 1500m.
Precursor film E is put into constant temperature oven and carries out heat treatment, heat treatment temperature: 180 DEG C, heat treatment time: 700 points
Clock.
Precursor film E through Overheating Treatment is stretched, prepares lithium ion battery separator, stretch rate: 3.5,
Draft temperature 170 DEG C, setting temperature 180 DEG C.
After melted for the polypropylene agglomerate containing calcium hydroxide, it is coated on lithium ion battery prefabricated membrane, coat thickness
It is 30 microns, places at normal temperatures and obtain compound non-porous film after 2 hours, polypropylene and calcium hydroxide in described polypropylene agglomerate
Weight ratio is 18:1；
Compound non-porous film is completely immersed in the hydrochloric acid of concentration 11% at 25 DEG C, soaks 120 minutes, completely remove hydrogen-oxygen
Take out after changing calcium, obtain lithium ion battery separator.
The thickness of the lithium ion battery separator prepared embodiment of the present invention 1-5 respectively is measured, and result shows, this
The thickness of the lithium ion battery separator of bright preparation is uniform.
In order to the puncture strength of lithium ion battery separator is prepared by inspection institute, lithium ion battery prepared by the embodiment of the present invention
The puncture strength of barrier film is measured, and with commercially available polypropylene diaphragm as a comparison case, result is as shown in table 1:
The puncture strength of the lithium ion battery separator of table 1 embodiment and comparative example
| Puncture strength (g) | |
| Embodiment 1 | 430 |
| Embodiment 1 | 432 |
| Embodiment 3 | 450 |
| Embodiment 4 | 448 |
| Embodiment 5 | 455 |
| Comparative example | 325 |
The explanation of above example is only intended to help to understand method and the core concept thereof of the present invention.It is right to it should be pointed out that,
For those skilled in the art, under the premise without departing from the principles of the invention, it is also possible to the present invention is carried out
Some improvement and modification, these improve and modify in the protection domain also falling into the claims in the present invention.
Described above to the disclosed embodiments, makes professional and technical personnel in the field be capable of or uses the present invention.
Multiple amendment to these embodiments will be apparent from for those skilled in the art, as defined herein
General Principle can realize without departing from the spirit or scope of the present invention in other embodiments.Therefore, the present invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and principles disclosed herein and features of novelty phase one
The widest scope caused.
Claims (10)
1. the preparation method of one kind high puncture strength lithium ion battery separator, it is characterised in that comprise the following steps:
High isotactic poly 1-butene is mixed by step a) with antioxidant, obtains the first mixture after stirring；
Described first mixture is put in extrusion casting apparatus and is carried out slab by step b), obtains precursor film；
Described precursor film is carried out heat treatment, longitudinal stretching at 80-180 DEG C by step c), obtains lithium ion battery separator.
Preparation method the most according to claim 1, it is characterised in that the isotacticity of described high isotactic poly 1-butene is
95%.
Preparation method the most according to claim 1, it is characterised in that described antioxidant is antioxidant 1076.
Preparation method the most according to claim 1, it is characterised in that described high isotactic poly 1-butene and the matter of antioxidant
Amount ratio is 100-300:1.
Preparation method the most according to claim 1, it is characterised in that in step b, the temperature of the extruder of extrusion casting apparatus
Degree is for 160-290 DEG C, and die head temperature is 160-269 DEG C, and casting roller temperature is 50-180 DEG C.
Preparation method the most according to claim 1, it is characterised in that the thickness of described precursor film is 10-50 μm.
Preparation method the most according to claim 1, it is characterised in that in step c, the time of heat treatment is that 150-1000 divides
Clock.
Preparation method the most according to claim 1, it is characterised in that the draft temperature of described longitudinal stretching is 120-250
DEG C, stretching ratio is 0.5-5.0.
Preparation method the most according to claim 1, it is characterised in that also include:
Being melted by polypropylene agglomerate containing calcium hydroxide, be coated on described lithium ion battery separator, coat thickness is 15-
30 microns, after placement, obtain compound non-porous film；
Described compound non-porous film is placed in hydrochloric acid, soaks.
Preparation method the most according to claim 9, it is characterised in that polypropylene and hydroxide in described polypropylene agglomerate
The weight ratio of calcium is 10-20:1.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109585749A (en) * | 2017-09-29 | 2019-04-05 | 清华大学 | Lithium ion battery separator and lithium ion battery with it |
| US11264677B2 (en) | 2018-06-06 | 2022-03-01 | Ningde Amperex Technology Limited | Separator and electrochemical device |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109585749A (en) * | 2017-09-29 | 2019-04-05 | 清华大学 | Lithium ion battery separator and lithium ion battery with it |
| US11264677B2 (en) | 2018-06-06 | 2022-03-01 | Ningde Amperex Technology Limited | Separator and electrochemical device |
| US12021183B2 (en) | 2018-06-06 | 2024-06-25 | Ningde Amperex Technology Limited | Electrochemical device |
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