CN110931692A - Polyolefin diaphragm and preparation method and application thereof - Google Patents
Polyolefin diaphragm and preparation method and application thereof Download PDFInfo
- Publication number
- CN110931692A CN110931692A CN201911246089.9A CN201911246089A CN110931692A CN 110931692 A CN110931692 A CN 110931692A CN 201911246089 A CN201911246089 A CN 201911246089A CN 110931692 A CN110931692 A CN 110931692A
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- CN
- China
- Prior art keywords
- polypropylene
- polyethylene
- polyolefin
- copolymerized polypropylene
- separator according
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 229920000098 polyolefin Polymers 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title abstract description 6
- -1 polyethylene Polymers 0.000 claims abstract description 64
- 239000004743 Polypropylene Substances 0.000 claims abstract description 42
- 229920001155 polypropylene Polymers 0.000 claims abstract description 37
- 239000004698 Polyethylene Substances 0.000 claims abstract description 29
- 229920000573 polyethylene Polymers 0.000 claims abstract description 29
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000005977 Ethylene Substances 0.000 claims abstract description 13
- 239000012982 microporous membrane Substances 0.000 claims abstract description 13
- 239000000178 monomer Substances 0.000 claims abstract description 12
- 239000012528 membrane Substances 0.000 claims description 11
- 229920005606 polypropylene copolymer Polymers 0.000 claims description 8
- 229920001400 block copolymer Polymers 0.000 claims description 6
- 239000000155 melt Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 238000009998 heat setting Methods 0.000 claims description 4
- 239000011148 porous material Substances 0.000 claims description 3
- 238000005266 casting Methods 0.000 claims description 2
- 239000003792 electrolyte Substances 0.000 claims description 2
- 239000004014 plasticizer Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 2
- 238000005336 cracking Methods 0.000 abstract description 2
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- 238000002844 melting Methods 0.000 description 9
- 230000008018 melting Effects 0.000 description 9
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000010410 layer Substances 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000004699 Ultra-high molecular weight polyethylene Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000002457 bidirectional effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229920001903 high density polyethylene Polymers 0.000 description 1
- 239000004700 high-density polyethylene Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000010220 ion permeability Effects 0.000 description 1
- 229920000092 linear low density polyethylene Polymers 0.000 description 1
- 239000004707 linear low-density polyethylene Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229920001684 low density polyethylene Polymers 0.000 description 1
- 239000004702 low-density polyethylene Substances 0.000 description 1
- 229920001179 medium density polyethylene Polymers 0.000 description 1
- 239000004701 medium-density polyethylene Substances 0.000 description 1
- 238000001471 micro-filtration Methods 0.000 description 1
- 229920005604 random copolymer Polymers 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229920000785 ultra high molecular weight polyethylene Polymers 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
-
- 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
-
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a polyolefin diaphragm and a preparation method and application thereof; the polyolefin diaphragm comprises at least one layer of microporous membrane, wherein the microporous membrane contains polyethylene and copolymerized polypropylene, and the copolymerized polypropylene contains 1 wt% -50 wt% of ethylene monomer. According to the invention, the co-polypropylene and the polyethylene are blended, polypropylene molecular chains are mutually interpenetrated among the polyethylene molecular chains to play a role of rigid framework support, and the diaphragm is prevented from cracking, and the co-polypropylene contains the polyethylene molecular chains, so that the problem that the polyethylene and the polypropylene are respectively crystallized to form a multiphase system with poor compatibility is solved, the homogeneous phase capacity of the polyethylene and the polypropylene in a molten state is improved, and thus, higher film breaking temperature and excellent heat shrinkage performance are obtained, and a closed-cell film breaking platform is prolonged.
Description
Technical Field
The invention belongs to the field of lithium battery diaphragm materials, and particularly relates to a polyolefin diaphragm and a preparation method and application thereof.
Background
Polyolefin microporous membranes are used for microfiltration membranes, battery separators, capacitor separators, fuel cell materials, and the like. Among these applications, when used as a battery separator, particularly a lithium ion battery separator, the polyolefin microporous membrane is required to have excellent ion permeability, excellent mechanical strength, and the like.
In order to ensure the safety of batteries, separators for high-capacity batteries in recent years are required to have "low closed-cell temperature characteristics", "high rupture temperature characteristics", and "low heat shrinkability".
The "low closed cell temperature characteristic" is a function of ensuring the safety of the battery by melting the separator to form a film covering the electrode and blocking the current when the inside of the battery is overheated due to an overcharge state or the like. It is known that in the case of a polyethylene microporous membrane, the closed cell temperature, i.e., the temperature at which the melt characteristics are exhibited, is about 140 ℃. However, in order to prevent runaway reaction and the like in the battery as early as possible, it is preferable that the melting temperature is lower.
The "high rupture temperature characteristic" means a property of the separator that the separator does not crack even when heated to a temperature higher than the melting temperature. Further, "low heat shrinkability" means a property that the heat shrinkability is small even when heated to a temperature equal to or higher than the melting temperature. Both of these are necessary in order to maintain the shape even after melting and to maintain the insulation between the electrodes.
In order to ensure the safety of the battery at 150 ℃, the battery separator is required to have a performance that meets the battery safety evaluation Standard specified in the us Standard UL1642 "Standard for Lithium B atteries". The evaluation was performed by keeping the separator in an oven at 150 ℃ for 10 minutes. To meet this standard, it is desirable that the membrane melt at 130 ℃ - & 140 ℃ without porosity, and that no rupture of the membrane occurs and that thermal shrinkage is minimized to maintain the shape even when heated above 150 ℃.
In the prior art, polyethylene and polypropylene have been mixed in order to obtain a lower closing temperature and a higher rupture temperature. However, the melting points of polyethylene and polypropylene are different greatly, which causes crystallization of two phases, and the compatibility problem is prominent, thereby affecting the stable obtainment of low closed pore temperature characteristic, high film breaking temperature characteristic and thermal shrinkage.
Disclosure of Invention
In view of the above, the present invention provides a polyolefin separator, and a preparation method and an application thereof, which can solve the problem of compatibility between polyethylene and polypropylene, and achieve better low-closed-cell temperature characteristics, high-rupture-temperature characteristics, and thermal shrinkage.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a polyolefin diaphragm, which comprises at least one layer of microporous membrane, wherein the microporous membrane contains polyethylene and polypropylene copolymer, and the polypropylene copolymer contains 1 wt% -50 wt% of ethylene monomer.
As a preferable technical scheme, the copolymerized polypropylene contains 3 to 20 weight percent of ethylene monomer.
As a preferable technical scheme, the copolymerized polypropylene contains 9 wt% -15 wt% of ethylene monomer.
As a preferred technical scheme, M of the copolymerized polypropylenewBetween 20 and 60 million, and the melt index at 190 ℃ and 21.6KG is between 10 and 18.
As a preferred technical scheme, the copolymerized polypropylene is a block copolymer.
As a preferable technical scheme, the microporous membrane contains 80-95 wt% of polyethylene and 5-20 wt% of copolymerized polypropylene.
As a preferred technical scheme, the closed pore temperature of the microporous membrane is less than or equal to 138 ℃, and the membrane breaking temperature is more than or equal to 150 ℃.
The invention also provides a preparation method of the polyolefin diaphragm, which comprises the following steps: mixing polyethylene, polypropylene copolymer and plasticizer, melt-extruding, and at least carrying out steps of sheet casting, stretching, extracting and heat setting to obtain the microporous membrane.
The invention also provides the application of the polyolefin diaphragm as a battery diaphragm, wherein a battery comprises a positive electrode, a negative electrode, an electrolyte and the battery diaphragm positioned between the positive electrode and the negative electrode, and the battery diaphragm comprises the polyolefin diaphragm.
The invention has the beneficial effects that:
according to the invention, the co-polypropylene and the polyethylene are blended, polypropylene molecular chains are mutually interpenetrated among the polyethylene molecular chains to play a role of rigid framework support, and the diaphragm is prevented from cracking, and the co-polypropylene contains the polyethylene molecular chains, so that the problem that the polyethylene and the polypropylene are respectively crystallized to form a multiphase system with poor compatibility is solved, the homogeneous phase capacity of the polyethylene and the polypropylene in a molten state is improved, and thus, higher film breaking temperature and excellent heat shrinkage performance are obtained, and a closed-cell film breaking platform is prolonged.
Detailed Description
The present invention is further described with reference to specific examples to enable those skilled in the art to better understand the present invention and to practice the same, but the examples are not intended to limit the present invention.
Example 1:
and pre-blending 95 wt% of polyethylene powder and 5 wt% of copolymerized polypropylene powder to obtain the polyolefin composition. Wherein M of the copolymerized polypropylenew40 ten thousand, a melt index at 190 ℃ and 21.6KG of 13, a block copolymer of the copolymerized polypropylene, the content of ethylene monomer in the copolymerized polypropylene being 9 wt%.
A polyolefin separator was prepared according to the following steps:
a. melting the ingredients: respectively putting 30 wt% of polyolefin composition and 70 wt% of white oil into a double screw, and mixing and melting to form a high-temperature melt;
b. die head extrusion: melting the materials in a double screw into high-temperature melt, accurately metering the high-temperature melt by a metering pump, and allowing the high-temperature melt to flow out of a slit opening of a die head;
c. cooling and forming the cast sheet: the high-temperature melt flows out of a slot of the die head to the surface of the chill roll, and is rapidly cooled and formed to form an oil-containing cast sheet; the chilling roller can be cooled in a mode of controlling temperature by a plurality of chilling rollers in a grading way;
d. and (3) bidirectional stretching: preheating an oil-containing cast sheet and then performing biaxial stretching to obtain an oil-containing film;
e. and (3) extraction: immersing the oil-containing film into an extraction tank containing dichloromethane to extract white oil;
f. and (3) drying: putting the extracted film into a drying oven, and volatilizing an extracting agent dichloromethane to obtain a dried film;
g. transversely stretching and expanding: feeding the dried film into a transverse drawing machine, heating and transversely drawing and expanding to ensure that the film holes are not shrunk;
h. heat setting: and (3) feeding the transversely-pulled film into a heat setting device, eliminating the internal stress of the film, and improving the heat shrinkage performance of the diaphragm to obtain the polyolefin diaphragm.
Example 2:
example 2 differs from example 1 in that: 90 wt% of polyethylene powder and 10 wt% of copolymerized polypropylene powder were previously blended to obtain a polyolefin composition.
Example 3:
example 3 differs from example 1 in that: m of copolymerized Polypropylenew38 million, the melt index at 190 ℃ and 21.6KG is 15, the copolymerized polypropylene is a block copolymer, and the content of ethylene monomer in the copolymerized polypropylene is 15 wt%.
Comparative example 1:
comparative example 1 differs from example 1 in that: the polyolefin composition contains only polyethylene powder and no polypropylene.
The separators obtained in examples 1 to 3 and comparative example 1 were subjected to performance tests under the same conditions, and the results are shown in table 1.
TABLE 1 comparison of results of membrane Performance tests
From the performance test data in table 1, the membrane closing temperature of example 1 is 134 ℃ and the membrane rupture temperature is 158 ℃; compared with the embodiment 1, the embodiment 2 has the advantages that the membrane rupture temperature can be obviously improved by increasing the content of the polypropylene copolymer; compared with the embodiment 1, the embodiment 3 has the advantages that the ethylene molecular content in the co-polypropylene is increased, the compatibility and the uniformity of the blended material can be improved, the hole closing temperature is reduced to 133 ℃, the hole closing temperature is increased to 166 ℃, the hole closing and membrane breaking platform is 33 ℃, and the safety is excellent after the co-polypropylene is assembled into a battery cell. Comparative example 1 was prepared from a polyethylene material and compared to the examples, the closed cell rupture window was narrow with only a plateau at 13 ℃, demonstrating the effect of the co-polypropylene in polyolefin separators.
In the present invention, the key effect is the copolymerized polypropylene containing 1 to 50 wt% of ethylene monomer, preferably 3 to 20 wt% of ethylene monomer, and more preferably 9 to 15 wt% of ethylene monomer. M of the copolymerized polypropylenewPreferably between 20 and 60 million, and a melt index at 190 ℃ and 21.6KG of between 10 and 18. The co-polypropylene may be a random or block copolymer, preferably a block copolymer.
In the present invention, the polyethylene may be one or more of ultrahigh molecular weight polyethylene, high density polyethylene, medium density polyethylene, branched low density polyethylene, and linear low density polyethylene. The mass ratio of the polyethylene to the polypropylene copolymer is preferably 80-95 wt% of polyethylene and 5-20 wt% of polypropylene copolymer.
In the invention, the polyolefin diaphragm can be a single-layer microporous diaphragm or a multi-layer microporous diaphragm, wherein at least one layer of microporous diaphragm has the blending characteristic of the polypropylene copolymer and the polyethylene.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (9)
1. A polyolefin separator film comprising at least one microporous film characterized by: the microporous membrane contains polyethylene and copolymerized polypropylene, and the copolymerized polypropylene contains 1 wt% -50 wt% of ethylene monomer.
2. The polyolefin separator according to claim 1, characterized in that: the copolymerized polypropylene contains 3-20 wt% of ethylene monomer.
3. The polyolefin separator according to claim 2, characterized in that: the copolymerized polypropylene contains 9-15 wt% of ethylene monomer.
4. The polyolefin separator according to claim 1, characterized in that: m of the copolymerized polypropylenewBetween 20 and 60 million, and the melt index at 190 ℃ and 21.6KG is between 10 and 18.
5. The polyolefin separator according to claim 1, characterized in that: the copolymerized polypropylene is a block copolymer.
6. The polyolefin separator according to any one of claims 1 to 5, characterized in that: the microporous membrane contains 80-95 wt% of polyethylene and 5-20 wt% of copolymerized polypropylene.
7. The polyolefin separator according to claim 6, characterized in that: the closed pore temperature of the microporous membrane is less than or equal to 138 ℃, and the membrane breaking temperature is more than or equal to 150 ℃.
8. The method for preparing a polyolefin separator according to any one of claims 1 to 7, wherein: the method comprises the following steps: mixing polyethylene, polypropylene copolymer and plasticizer, melt-extruding, and at least carrying out steps of sheet casting, stretching, extracting and heat setting to obtain the microporous membrane.
9. A battery comprising a positive electrode, a negative electrode, an electrolyte, and a battery separator between the positive electrode and the negative electrode, wherein: the battery separator includes the polyolefin separator according to any one of claims 1 to 7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911246089.9A CN110931692A (en) | 2019-12-08 | 2019-12-08 | Polyolefin diaphragm and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911246089.9A CN110931692A (en) | 2019-12-08 | 2019-12-08 | Polyolefin diaphragm and preparation method and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110931692A true CN110931692A (en) | 2020-03-27 |
Family
ID=69858206
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911246089.9A Pending CN110931692A (en) | 2019-12-08 | 2019-12-08 | Polyolefin diaphragm and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110931692A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021237767A1 (en) * | 2020-05-29 | 2021-12-02 | 江苏厚生新能源科技有限公司 | Microporous membrane with controllable pore closure, preparation method therefor and use thereof |
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|---|---|---|---|---|
| CN101000952A (en) * | 2006-11-02 | 2007-07-18 | 许贵斌 | Polyalkylene microporous diaphragm for lithiam ion battery and manufacturing method thereof |
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2019
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2021237767A1 (en) * | 2020-05-29 | 2021-12-02 | 江苏厚生新能源科技有限公司 | Microporous membrane with controllable pore closure, preparation method therefor and use thereof |
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Address after: 401121 No.22, Qixin Avenue, Yanjia street, Changshou District, Chongqing Applicant after: Chongqing engeniumi Technology Co.,Ltd. Address before: 401121 No.22, Qixin Avenue, Yanjia street, Changshou District, Chongqing Applicant before: CHONGQING YUNTIANHUA NEWMI-TECH Co.,Ltd. |
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Application publication date: 20200327 |