CN109817866A - Method for preparing polyolefin microporous membrane and device - Google Patents
Method for preparing polyolefin microporous membrane and device Download PDFInfo
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- CN109817866A CN109817866A CN201811642183.1A CN201811642183A CN109817866A CN 109817866 A CN109817866 A CN 109817866A CN 201811642183 A CN201811642183 A CN 201811642183A CN 109817866 A CN109817866 A CN 109817866A
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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
Abstract
A kind of method for preparing polyolefin microporous membrane and device, this method comprises: two or more materials is extruded into melt through two or more extruders；Melt introducing multilayer distributor is subjected to layering superposition and forms composite multi-layer melt；The composite multi-layer melt is squeezed out via die head；And it forms and makes annealing treatment through chill roll slab；Simple tension pore-forming is carried out again, obtains multilayer polyolefine microporous film.The present invention can be avoided MIcroporous polyolefin film micro-short circuit in the battery, improve battery capacity holding and cycle performance.
Description
Technical field
The present invention relates to macromolecule member material technical fields, and in particular to a kind of method for preparing polyolefin microporous membrane and dress
It sets.
Background technique
Lithium ion battery is made of positive and negative electrode material, electrolyte, diaphragm and battery case, diaphragm as core component it
One, main function shows two aspects: (1) positive and negative electrode is isolated, is the insulator of electronics, prevents positive and negative anodes contact short circuit；
(2) allow ion to pass freely through, transmit electronics.Therefore, the microcellular structure superiority and inferiority of diaphragm is to battery capacity, cycle performance, multiplying power
Performance generates vital influence.
Currently, lithium ion battery separator is mainly MIcroporous polyolefin film, common preparation method includes dry method (fusion drawn
Method) and wet process (thermally induced phase separation), the micropore formation mechenism of two methods it is entirely different.Wet process biaxial stretching film is using extraction
Technique pore-creating prepares three-dimensional network-like structure, and the tortuosity in hole is relatively high, but aperture is bigger than normal.Wet process is due to using
A large amount of organic diluents, the device is complicated, at high cost, easily causes environmental pollution, while PE material is heat-shrinked greatly, and thermal stability is poor,
Application security is lower in the battery, although can be effectively improved using ceramic coated, cost increases many.
Using beta crystal to a crystal transfer, crystal volume, which is shunk, generates micropore, this technique system for dry method biaxial tension
Standby aperture is big and distribution is extremely irregular, largely can be only applied to low side field.Dry method simple tension is since equipment is simple, cost
It is low, non-environmental-pollution problem, and prepare that aperture consistency is good, and thickness is uniform, become current dry method tension prevailing technology.But
Dry method list is drawn due to causing platelet to separate using longitudinal stretching and a large amount of fentos occur, and then generates the netted knot of slit-shaped hole
Structure is easy to appear certain amount clear opening, and hole tortuosity is extremely low, simultaneously because being influenced by molding equipment, aperture is generally all larger,
The micro-short circuit in battery is eventually resulted in, battery capacity is caused, cycle life reduces.
Summary of the invention
The present invention provides a kind of method for preparing polyolefin microporous membrane and device, can be avoided MIcroporous polyolefin film in the battery
Micro-short circuit improves battery capacity holding and cycle performance.
According in a first aspect, providing a kind of method for preparing polyolefin microporous membrane in a kind of embodiment, comprising: will be two or more
Material be extruded into melt through two or more extruders；Above-mentioned melt introducing multilayer distributor is carried out layering superposition to be formed
Composite multi-layer melt；Above-mentioned composite multi-layer melt is squeezed out via die head；And it forms and makes annealing treatment through chill roll slab；Again into
Row simple tension pore-forming, obtains multilayer polyolefine microporous film.
In a preferred embodiment, polypropylene or poly- second of the above two above material selected from the identical trade mark or the different trades mark
Alkene.
In a preferred embodiment, above-mentioned polyacrylic melt index be 0.5~6.0g/10min, weight average molecular weight be 2 ×
105~6 × 106；The melt index of above-mentioned polyethylene is 0.2~5.0g/10min, and weight average molecular weight is 1 × 105~2.5 ×
105。
In a preferred embodiment, above-mentioned multilayer distributor is the multilayer distributor of 2~9 runners.
In a preferred embodiment, the temperature of above-mentioned extruder squeezes out temperature, above-mentioned layering superposition and above-mentioned die head squeeze out
Temperature be 190~260 DEG C.
In a preferred embodiment, the temperature of above-mentioned chill roll is 30~120 DEG C.
In a preferred embodiment, above-mentioned annealing is to toast at 100~160 DEG C, and the time is 1~20h.
In a preferred embodiment, the draft temperature of above-mentioned stretching pore-forming is 110~160 DEG C, and stretching speed ratio is 1~3, is stretched
Speed is 1~10m/min.
In a preferred embodiment, above-mentioned multilayer polyolefine microporous film with a thickness of 6~30 μm, average pore size is 18~
23nm, pore size distribution range are 15~25nm.
In a preferred embodiment, the hole tortuosity of above-mentioned multilayer polyolefine microporous film is 3.0~4.0.
According to second aspect, a kind of polyolefin micropore membrane preparation device is provided in a kind of embodiment, comprising: at least two are squeezed
Machine, multilayer distributor, die head and cooling and traction module out；Wherein, above-mentioned multilayer distributor front end connection above-mentioned at least two
Platform extruder, rear end connect above-mentioned die head, and above-mentioned die head rear end connects above-mentioned cooling and traction module, above-mentioned at least two extrusions
Machine is used to for two or more materials being extruded into melt, and above-mentioned multilayer distributor is used to carry out above-mentioned melt layering superposition shape
At composite multi-layer melt, above-mentioned die head is used for above-mentioned composite multi-layer melt extrusion, above-mentioned cooling and traction module for that will squeeze
The cooling slab molding of above-mentioned composite multi-layer melt out and simple tension pore-forming, obtain multilayer polyolefine microporous film.
In a preferred embodiment, above-mentioned multilayer distributor is the multilayer distributor of 2~9 runners.
In a preferred embodiment, the above two above material is respectively in the form of interval into above-mentioned multilayer distributor
In different runners.
In a preferred embodiment, the operating temperature of above-mentioned extruder, the operating temperature of above-mentioned multilayer distributor and above-mentioned mould
The operating temperature of head is 190~260 DEG C.
According to the third aspect, a kind of method for preparing polyolefin microporous membrane or second of first aspect is provided in a kind of embodiment
The multilayer polyolefine microporous film that the polyolefin micropore membrane preparation device of aspect is prepared.
In a preferred embodiment, above-mentioned multilayer polyolefine microporous film with a thickness of 6~30 μm, average pore size is 18~
23nm, pore size distribution range are 15~25nm.
In a preferred embodiment, the hole tortuosity of above-mentioned multilayer polyolefine microporous film is 3.0~4.0.
Method for preparing polyolefin microporous membrane and device of the invention is distributed during being cast extrusion molding using multilayer
Device is repeatedly layered melt and cuts thin, refinement platelet size, reduction pore size, simultaneously because the layering occurred at bed boundary is folded
Sliding phenomenon is summed it up, increases the tortuosity in hole, macropore is avoided to occur.It is small (20nm or so) that the present invention can prepare average pore size
Multilayer polyolefine microporous film, reduce by 50% or so compared to the aperture existing product (average pore size 40nm) in the market, pore-size distribution
Narrow (15~25nm or so), uniformity is good, while tortuosity is high (3.0~4.0 or so), and pressure voltage is big (3.0kv), avoids polyene
Hydrocarbon microporous barrier micro-short circuit in the battery improves battery capacity and keeps and cycle performance.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the polyolefin micropore membrane preparation device of the embodiment of the present invention；
Fig. 2 is the cross section structure schematic diagram of multilayer distributor in the polyolefin micropore membrane preparation device of the embodiment of the present invention；
Fig. 3 is the graph of pore diameter distribution of the MIcroporous polyolefin film of the embodiment of the present invention；
Fig. 4 is the cycle performance test result figure of the MIcroporous polyolefin film of the embodiment of the present invention；
Fig. 5 is that the high rate performance of the MIcroporous polyolefin film of the embodiment of the present invention tests (1C/2C/3C) result figure.
Specific embodiment
Below by specific embodiment combination attached drawing, invention is further described in detail.In the following embodiments and the accompanying drawings
In, many datail descriptions are in order to enable the present invention can be better understood.However, those skilled in the art can be without lifting an eyebrow
Recognize, part of feature is dispensed in varied situations, or can be by other elements, material, method institute
Substitution.
It is formed respectively in addition, feature described in this description, operation or feature can combine in any suitable way
Kind embodiment.Meanwhile each step in method description or movement can also can be aobvious and easy according to those skilled in the art institute
The mode carry out sequence exchange or adjustment seen.Therefore, the various sequences in the description and the appended drawings are intended merely to clearly describe a certain
A embodiment is not meant to be necessary sequence, and wherein some sequentially must comply with unless otherwise indicated.
Firstly, the present invention provides a kind of method for preparing polyolefin microporous membrane, comprising: by two or more materials through two with
On extruder be extruded into melt；Above-mentioned melt introducing multilayer distributor is subjected to layering superposition and forms composite multi-layer melt；
Above-mentioned composite multi-layer melt is squeezed out via die head；And it forms and makes annealing treatment through chill roll slab；Carry out again simple tension at
Hole obtains multilayer polyolefine microporous film.
In a preferred embodiment, material is two kinds, both materials can be selected from the identical trade mark or the different trade mark
Polypropylene (PP) or polyethylene (PE) correspondingly squeeze out two kinds of materials using two extruders respectively.Polypropylene and/or poly- second
Alkene can be not particularly limited, however in preferably embodiment, polyacrylic melt index is 0.5~6.0g/10min, weight
Average molecular weight is 2 × 105~6 × 106；The melt index of polyethylene is 0.2~5.0g/10min, and weight average molecular weight is 1 × 105
~2.5 × 105。
The number of plies of multilayer distributor/runner number can be not particularly limited, it is however generally that the more the number of plies/runner number the more advantageous
In realizing effect of the invention, in a preferred embodiment, multilayer distributor has 2~9 runners, i.e. 2~9 Layer assignments
Device.
The operating temperature of each step can be arranged as the case may be in method of the invention, such as not according to selection
The operating temperature of each step is arranged in property with material etc..In a preferred embodiment, the temperature of extruder extrusion, layering
The temperature that the temperature and die head of superposition squeeze out is 190~260 DEG C, such as 195 DEG C, 200 DEG C, 205 DEG C, 215 DEG C, 220 DEG C, 230
DEG C, 240 DEG C, 250 DEG C, 255 DEG C or 258 DEG C etc..The temperature of chill roll is 30~120 DEG C, such as 35 DEG C, 40 DEG C, 50 DEG C, 60
DEG C, 70 DEG C, 80 DEG C, 90 DEG C, 100 DEG C, 110 DEG C or 115 DEG C etc..It makes annealing treatment to be toasted at 100~160 DEG C, such as 110 DEG C,
120 DEG C, 130 DEG C, 140 DEG C, 145 DEG C or 155 DEG C etc., the time be 1~20h, such as 2h, 4h, 5h, 6h, 8h, 10h, 12h, 15h,
18h or 19h etc..Stretch pore-forming draft temperature be 110~160 DEG C, such as 110 DEG C, 120 DEG C, 130 DEG C, 140 DEG C, 145 DEG C or
155 DEG C etc., stretching speed ratio is 1~3, such as 1,1.2,1.5,1.8,1.9,2,2.2,2.5 or 2.8 etc., tensile speed is 1~
10m/min, for example, 1m/min, 2m/min, 3m/min, 4m/min, 5m/min, 6m/min, 7m/min, 8m/min, 9m/min or
10m/min etc..
Multilayer polyolefine microporous film produced by the present invention with a thickness of 6~30 μm, such as 7 μm, 10 μm, 12 μm, 15 μm, 18
μm, 20 μm, 22 μm, 24 μm, 26 μm, 28 μm or 29 μm etc., average pore size is 18~23nm, 18nm, 19nm, 20nm, 21nm,
22nm or 23nm etc., pore size distribution range be 15~25nm, such as 16nm, 17nm, 18nm, 19nm, 20nm, 21nm, 22nm,
23nm, 24nm or 25nm etc..The hole tortuosity of multilayer polyolefine microporous film be 3.0~4.0, such as 3.1,3.2,3.3,3.4,
3.5,3.6,3.7,3.8 or 3.9 etc..
Secondly, the present invention provides a kind of polyolefin micropore membrane preparation device, as shown in Figure 1, comprising: at least two extruders
1 (two are shown in figure), multilayer distributor 2, die head 3 and cooling and traction module 4；Wherein, 2 front end of multilayer distributor connects
At least two extruders 1, rear end connect die head 3, and the connection of 3 rear end of die head is cooling and traction module 4, at least two extruders 1 are used
In two or more materials is extruded into melt, multilayer distributor 2 is used to carry out melt layering superposition and forms composite multi-layer
Melt, die head 3 are used for composite multi-layer melt extrusion, and the composite multi-layer melt that cooling and traction module 4 is used to squeeze out is cooling
Slab molding and simple tension pore-forming, obtain multilayer polyolefine microporous film.
The number of plies of multilayer distributor/runner number can be not particularly limited, it is however generally that the more the number of plies/runner number the more advantageous
In realizing effect of the invention, in a preferred embodiment, multilayer distributor has 2~9 runners, i.e. 2~9 Layer assignments
Device.As shown in Fig. 2, multilayer distributor 2 has 7 runners 21, two kinds of materials (A and B) squeeze out from two extruders 1 respectively, are in
The form at interval enters in the different runners of the multilayer distributor with 7 runners 21.
Melt is carried out in layering additive process using multilayer distributor, melt is narrowed by thickness, refining grain size, cooling
Forming process forms tiny lamellar structure, and this structure can prepare small and dense aperture product in posterior drawing process, and due to
The superposition of multilayer staggered floor, hole tortuosity increase.In a specific embodiment, the method for preparing MIcroporous polyolefin film, including such as
Lower step:
(1) curtain coating squeezes out: two extruders squeeze out two kinds of materials of A, B respectively, and (A, B material can be same model polyene
Hydrocarbon is also possible to different model polyolefin) after plastifying fusion, it is flowed into multilayer distributor, as shown in Figure 1, processing temperature is 190
~260 DEG C.
(2) multilayer distributor layering-superposition: as shown in Fig. 2, two extruders material enters the difference in multilayer distributor
In runner, by thick thinning lamination process again, melt structure is combed, keeps macromolecular chain height-oriented, formed composite multi-layer melt, add
Work temperature is 190~260 DEG C.
(3) slab forms: composite multi-layer melt being squeezed out from die head, is formed by chill roll slab, traction film forming is cooling
30~120 DEG C of roll temperature.
(4) it makes annealing treatment: Multi-layer cast film being put into baking oven at 100~160 DEG C and is toasted, the time is 1~20h.
(5) it stretches pore-forming: the casting films after annealing being subjected to longitudinal stretching, stretch speed ratio 1~3, draft temperature is
110~160 DEG C, 1~10m/min of tensile speed prepares multilayer polyolefine microporous film.
Below by way of specific embodiment and the comparative example technical solution that the present invention will be described in detail, it is to be appreciated that these are implemented
Example and comparative example are merely exemplary, and should not be understood as limiting the scope of the invention.
The multilayer polyolefine microporous film prepared in following embodiment is with a thickness of 16 μm, and wherein A, B material are the trade mark of the same race
PP material, shown in specific preparation process following examples:
Embodiment 1:
(1) curtain coating squeezes out: two extruders squeeze out two kinds of materials of A, B respectively, after plastifying fusion, squeeze out into 5 Layer assignments
Device converges, and processing temperature is all 230 DEG C.
(2) multilayer distributor: A, two kinds of materials of B enter in 5 Layer assignment devices, after layering superposition, converge and are flowed into
In die head, processing temperature is 220 DEG C.
(3) slab forms: compound two layers of melt being squeezed out from die head, is formed by chill roll slab, traction film forming is cooling
90 DEG C of roll temperature.
(4) annealing crystallization: being put into baking oven for Multi-layer cast film and be heat-treated, and 140 DEG C of annealing temperature, annealing time 14h.
(5) it stretches pore-forming: the casting films after annealing is stretched, stretch speed ratio 2.5, draft temperature is
150 DEG C, tensile speed 4m/min, two layers of co-extrusion MIcroporous polyolefin film is prepared, product physicochemical property is as shown in table 1.
Embodiment 2:
Difference from Example 1 is that multilayer distributor is 7 Layer assignment devices, prepares 7 layers of co-extrusion MIcroporous polyolefin film,
Properties of product are as shown in table 1.
Embodiment 3:
Difference from Example 1 is that multilayer distributor is 9 Layer assignment devices, prepares 9 layers of co-extrusion MIcroporous polyolefin film,
Properties of product are as shown in table 1.
Embodiment 4:
Single layer MIcroporous polyolefin film is prepared without distributor using separate unit extruder, properties of product are as shown in table 1.
The multi-layer co-extruded alkene microporous barrier the performance test results of 1 Examples 1 to 4 of table preparation
Fig. 3 shows the pore-size distribution for the MIcroporous polyolefin film that different embodiments are prepared.By table 1 and Fig. 3 it is found that implementing
Example 1 compares embodiment 4, using under raw material same case, prepares same porosity product, the hole of 5 layers of co-extrusion MIcroporous polyolefin film
Diameter reduces by 40% (being down to 23.6nm from 39.6nm), and pore size distribution range narrows and (fades to 15~28nm from 25~55nm)；Simultaneously
Since multilayered structure increases, product tortuosity is uprushed 35% (increasing to 2.5 from 1.8), and value of breathing freely also increases accordingly 17%, table
In terms of present electrical property, polyolefin micropore film surface pressure voltage increases, and illustrates that film surface defects count is reduced, micro-short circuit risk drop
It is low.
Fig. 4 shows the cycle performance test result for the MIcroporous polyolefin film that embodiment 3 and embodiment 4 are prepared.
Fig. 5 shows the high rate performance test (1C/2C/3C) for the MIcroporous polyolefin film that embodiment 3 and embodiment 4 are prepared
As a result.It has been shown that, as the MIcroporous polyolefin film distributor number of plies increases, under same thickness, aperture size is further decreased；Multi-laminate
Tortuosity is added to further increase, pressure voltage is also significantly increasing, therefore battery capacity retention property is better, and capacity attenuation is slack-off,
High rate performance is more preferably.
Use above specific case is illustrated the present invention, is merely used to help understand the present invention, not to limit
The system present invention.For those skilled in the art, according to the thought of the present invention, can also make several simple
It deduces, deform or replaces.
Claims (10)
1. a kind of method for preparing polyolefin microporous membrane, which is characterized in that the described method includes: by two or more materials through two
Above extruder is extruded into melt；Melt introducing multilayer distributor is carried out layering superposition to form composite multi-layer and melt
Body；The composite multi-layer melt is squeezed out via die head；And it forms and makes annealing treatment through chill roll slab；Simple tension is carried out again
Pore-forming obtains multilayer polyolefine microporous film.
2. the method according to claim 1, wherein described two above materials are selected from the identical trade mark or difference
The polypropylene or polyethylene of the trade mark.
3. according to the method described in claim 2, it is characterized in that, the polyacrylic melt index is 0.5 ~ 6.0g/
10min, weight average molecular weight are 2 × 105~6×106；The melt index of the polyethylene is 0.2 ~ 5.0g/10min, Weight-average molecular
Amount is 1 × 105~2.5×105。
4. the method according to claim 1, wherein the multilayer distributor is the multilayer distribution of 2 ~ 9 runners
Device；
Preferably, the temperature that the temperature of the extruder squeezes out temperature, the layering superposition and the die head squeeze out is 190 ~
260℃；
Preferably, the temperature of the chill roll is 30 ~ 120 DEG C；
Preferably, for the annealing to toast at 100 ~ 160 DEG C, the time is 1 ~ 20h；
Preferably, the draft temperature for stretching pore-forming is 110 ~ 160 DEG C, and stretching speed ratio is 1 ~ 3, and tensile speed is 1 ~ 10m/
min。
5. the method according to claim 1, wherein the multilayer polyolefine microporous film with a thickness of 6 ~ 30 μm,
Average pore size is 18 ~ 23nm, and pore size distribution range is 15 ~ 25nm；
Preferably, the hole tortuosity of the multilayer polyolefine microporous film is 3.0 ~ 4.0.
6. a kind of polyolefin micropore membrane preparation device, which is characterized in that described device includes: that at least two extruders, multilayer is divided
Orchestration, die head and cooling and traction module；Wherein, the multilayer distributor front end connection at least two extruders, after
End connects the die head, and the die head rear end connects the cooling and traction module, and at least two extruders are used for two
Kind or more material be extruded into melt, the multilayer distributor is used to carry out the melt layering superposition and forms composite multi-layer
Melt, the die head are used for the composite multi-layer melt extrusion, the cooling and traction module is described multiple for that will squeeze out
The cooling slab molding of multilayer melt and simple tension pore-forming are closed, multilayer polyolefine microporous film is obtained.
7. device according to claim 6, which is characterized in that the multilayer distributor is the multilayer distribution of 2 ~ 9 runners
Device.
8. device according to claim 7, which is characterized in that described two above materials respectively in the form of interval into
In the different runners for entering the multilayer distributor.
9. device according to claim 6, which is characterized in that the operating temperature of the extruder, the multilayer distributor
Operating temperature and the die head operating temperature be 190 ~ 260 DEG C.
10. polyolefin micropore described in method for preparing polyolefin microporous membrane described in a kind of claim 1-5 or claim 6-9
The multilayer polyolefine microporous film that membrane preparation device is prepared；
Preferably, the multilayer polyolefine microporous film with a thickness of 6 ~ 30 μm, average pore size is 18 ~ 23nm, pore size distribution range
For 15 ~ 25nm；
Preferably, the hole tortuosity of the multilayer polyolefine microporous film is 3.0 ~ 4.0.
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| CN201811642183.1A CN109817866B (en) | 2018-12-29 | 2018-12-29 | Polyolefin microporous membrane preparation method and device |
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| CN201811642183.1A CN109817866B (en) | 2018-12-29 | 2018-12-29 | Polyolefin microporous membrane preparation method and device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111129399A (en) * | 2019-12-27 | 2020-05-08 | 武汉中兴创新材料技术有限公司 | Preparation method of polyolefin microporous membrane and polyolefin microporous membrane |
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| CN105489916A (en) * | 2015-11-26 | 2016-04-13 | 同济大学 | Porous polymer film for lithium-ion battery and preparation method and application of porous polymer film |
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