CN111138741A - High-performance polyolefin diaphragm and preparation method thereof - Google Patents
High-performance polyolefin diaphragm and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/20—Manufacture of shaped structures of ion-exchange resins
- C08J5/22—Films, membranes or diaphragms
- C08J5/2206—Films, membranes or diaphragms based on organic and/or inorganic macromolecular compounds
- C08J5/2218—Synthetic macromolecular compounds
- C08J5/2231—Synthetic macromolecular compounds based on macromolecular compounds obtained by reactions involving unsaturated carbon-to-carbon bonds
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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
- 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
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—Polyethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/06—Polyethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2453/00—Characterised by the use of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
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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 invention discloses a polyolefin diaphragm and a preparation method thereof; the polyolefin separator comprises at least one microporous membrane, wherein the microporous membrane comprises a polyethylene composition and a polypropylene copolymer; the polyethylene composition comprises a first polyethylene, a second polyethylene and a third polyethylene, wherein M of the first polyethylenewM of said second polyethylene in the range of 10 to 30 ten thousandwM of said third polyethylene ranging from 40 to 60 ten thousandwIs 90-120 ten thousand; the copolymerized polypropylene contains 1-50 wt% of ethylene monomer. The invention can solve the problem of compatibility of polyethylene and polypropylene, and achieves better compatibilityLow closed-cell temperature characteristic, high film rupture temperature characteristic and heat shrinkability.
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 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 thereof, which can solve the problem of compatibility between polyethylene and polypropylene, and achieve better low-closed-cell temperature characteristics, high film-breaking temperature characteristics, high elongation, and low 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 a polyethylene composition and polypropylene copolymer; the polyethylene composition comprises a first polyethylene, a second polyethylene and a third polyethylene, wherein M of the first polyethylenewM of said second polyethylene in the range of 10 to 30 ten thousandwM of said third polyethylene ranging from 40 to 60 ten thousandwIs 90-120 ten thousand; the copolymerized polypropylene contains 1-50 wt% of ethylene monomer.
In a preferred embodiment, the polyethylene composition comprises 8 wt% to 20 wt% of the first polyethylene, 5 wt% to 20 wt% of the second polyethylene, and 60 wt% to 87 wt% of the third polyethylene.
As a preferred technical scheme, M of the first polyethylenewM of said second polyethylene of 20 ten thousandwM of said third polyethylene of 50 ten thousandwIs 100 ten thousand.
As a preferable technical scheme, the melting point of the first polyethylene is less than or equal to 126 ℃, and the enthalpy is less than or equal to 157J/g; the melting point of the second polyethylene is 132-137 ℃, and the enthalpy is 192-202J/g; the melting point of the third polyethylene is 135-142 ℃, and the enthalpy is not more than 173J/g.
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 polypropylenewMelting at 190 ℃ and 21.6KG under 20-60 ten thousandThe fusion index 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 to 95 weight percent of polyethylene composition and 5 to 20 weight percent of polypropylene copolymer.
The invention also provides a preparation method of the polyolefin diaphragm, which comprises the following steps:
(1) extruding the polyethylene composition, co-polypropylene and plasticizer through a die, cooling to form a gel-like sheet; wherein the extrusion amount is controlled to be 30-170kg/h, the casting speed is controlled to be less than or equal to 20m/min, the casting temperature is controlled to be less than or equal to 35 ℃, and the thickness of the sheet is controlled to be less than or equal to 300 mu m;
(2) sequentially performing longitudinal stretching, first transverse stretching and second transverse stretching on the gel-like sheet; wherein the longitudinal stretching temperature is controlled between 40 ℃ and 130 ℃, and the longitudinal stretching speed ratio is controlled to be less than or equal to 10; the first transverse stretching temperature is controlled between 80 ℃ and 130 ℃, and the first transverse stretching speed ratio is controlled to be less than or equal to 12; the second transverse stretching temperature is controlled to be less than or equal to 130 ℃, and the second transverse stretching speed ratio is controlled to be less than or equal to 2.0.
The invention has the beneficial effects that:
1. according to the invention, the co-polypropylene and the polyethylene are blended, polypropylene molecular chains are mutually interpenetrated among polyethylene molecular chains, a rigid framework supporting effect is achieved, 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.
2. According to the invention, through blending of high/medium/low molecular weight polyethylene, the melting temperature of the polyolefin diaphragm is reduced, the melting process is lengthened, the duration time of the hole closing process is prolonged, and the characteristic of continuous hole closing is formed, so that the characteristic of better low hole closing temperature is achieved.
3. In addition, the invention greatly improves the biaxial elongation of the polyolefin diaphragm through reasonable polyolefin molecular weight distribution combination design and specific casting and stretching process adjustment, and the biaxial elongation under the thickness of 5 mu m is more than or equal to 100 percent, even more than or equal to 150 percent.
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:
polyethylene composition: 15 wt% of the first polyethylene, 8 wt% of the second polyethylene and 77 wt% of the third polyethylene were mixed to obtain a polyethylene composition. Wherein M of the first polyethylenew20 ten thousand, the melting point is 122 ℃, and the enthalpy is 150J/g; m of the second polyethylenew50 ten thousand, the melting point is 133 ℃, and the enthalpy is 198J/g; m of the third polyethylenew100 ten thousand, a melting point of 138 ℃ and an enthalpy of 168J/g.
Copolymerized polypropylene: m of 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%.
Polyolefin composition: 95 wt% of polyethylene composition and 5 wt% of copolymerized polypropylene powder were mixed to obtain a polyolefin composition.
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 to form a high-temperature melt, accurately metering the high-temperature melt by a metering pump, feeding the high-temperature melt into a die head, allowing the high-temperature melt to flow out of a slit opening of the die head, and cooling to form a gel sheet; wherein the extrusion amount is controlled at 40kg/h, the casting speed is controlled at 15m/min, the casting temperature is controlled at 30 ℃, and the thickness of the sheet is controlled at 200 mu m;
c. stretching: sequentially performing longitudinal stretching, first transverse stretching and second transverse stretching on the gel-like sheet; wherein the longitudinal stretching temperature (preheating, stretching and shaping) is controlled between 40 ℃ and 130 ℃, and the longitudinal stretching speed ratio is controlled at 4; the first transverse stretching temperature (preheating, stretching and shaping) is controlled between 80 ℃ and 130 ℃, and the first transverse stretching speed ratio is controlled to be 5; the second transverse stretching temperature (preheating, stretching and shaping) is controlled to be less than or equal to 130 ℃, and the second transverse stretching speed ratio is controlled to be 1.5;
d. and (3) extraction: immersing the oil-containing film into an extraction tank containing dichloromethane to extract white oil;
e. and (3) drying: and (3) putting the extracted film into a drying oven, and volatilizing an extracting agent dichloromethane to obtain a dried film, namely the polyolefin diaphragm.
Example 2:
example 2 differs from example 1 in that: mixing 90 wt% of polyethylene composition and 10 wt% of copolymerized polypropylene powder to obtain the 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%.
Example 4:
example 4 differs from example 1 in that: 15 wt% of the first polyethylene, 5 wt% of the second polyethylene and 80 wt% of the third polyethylene were mixed to obtain a polyethylene composition.
Example 5:
example 5 differs from example 1 in that: 10 wt% of the first polyethylene, 20 wt% of the second polyethylene and 70 wt% of the third polyethylene were mixed to obtain a polyethylene composition.
Example 6:
example 6 differs from example 1 in that: 20 wt% of the first polyethylene, 20 wt% of the second polyethylene and 60 wt% of the third polyethylene are mixed to obtain a polyethylene composition.
Comparative example 1:
comparative example 1 differs from example 1 in that: the polyolefin composition comprises only a polyethylene composition and no co-polypropylene.
Comparative example 2:
comparative example 2 differs from example 1 in that: the polyethylene composition comprises only the second polyethylene, and no first polyethylene and no third polyethylene.
The separators obtained in examples 1 to 6 and comparative examples 1 to 2 were subjected to performance tests under the same conditions, and the results are shown in tables 1 and 2.
TABLE 1 comparison of results of membrane Performance tests
TABLE 2 comparison of results of membrane Performance tests
From the closed cell temperature and rupture temperature test data, the closed cell temperature was decreased, while the rupture temperature was increased and the closed cell rupture window was longer for examples 1-6 compared to comparative examples 1-2.
From the elongation test data, the 5 μm separator of examples 1-6 had a longitudinal/transverse elongation of 150% or more, while the 5 μm separator of comparative example 2 had a lower longitudinal/transverse elongation than the examples.
It should be noted that one of the keys of the present invention is the copolymerized polypropylene containing 1 wt% to 50 wt% of ethylene monomer, preferably 3 wt% to 20 wt% of ethylene monomer, and more preferably 9 wt% 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.
The second key to the invention is the polyethylene composition, M of the first polyethylenewNeeds to be controlled between 10 and 30 ten thousand, and the M of the second polyethylenewThe M of the third polyethylene needs to be controlled between 40 and 60 ten thousandwThe temperature is controlled to be between 90 and 120 ten thousand; preferably, the melting point of the first polyethylene is less than or equal to 126 ℃, and the enthalpy is less than or equal to 157J/g; what is needed isThe melting point of the second polyethylene is 132-137 ℃, and the enthalpy is 192-202J/g; the melting point of the third polyethylene is 135-142 ℃, and the enthalpy is not more than 173J/g.
The third key point of the invention is the preparation process parameters, wherein the extrusion amount is controlled to be 30-170kg/h, the casting speed is controlled to be less than or equal to 20m/min, the casting temperature is controlled to be less than or equal to 35 ℃, and the thickness of the sheet is controlled to be less than or equal to 300 mu m; the longitudinal stretching temperature is controlled between 40 ℃ and 130 ℃, and the longitudinal stretching speed ratio is controlled to be less than or equal to 10; the first transverse stretching temperature is controlled between 80 ℃ and 130 ℃, and the first transverse stretching speed ratio is controlled to be less than or equal to 12; the second transverse stretching temperature is controlled to be less than or equal to 130 ℃, and the second transverse stretching speed ratio is controlled to be less than or equal to 2.0.
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 characteristics of the invention.
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 (10)
1. A polyolefin separator film comprising at least one microporous film characterized by: the microporous membrane comprises a polyethylene composition and a co-polypropylene; the polyethylene composition comprises a first polyethylene, a second polyethylene and a third polyethylene, wherein M of the first polyethylenewM of said second polyethylene in the range of 10 to 30 ten thousandwM of said third polyethylene ranging from 40 to 60 ten thousandwIs 90-120 ten thousand; the copolymerized polypropylene contains 1-50 wt% of ethylene monomer.
2. The polyolefin separator according to claim 1, wherein: in the polyethylene composition, the first polyethylene accounts for 8-20 wt%, the second polyethylene accounts for 5-20 wt%, and the third polyethylene accounts for 60-87 wt%.
3. The polyolefin separator according to claim 1, wherein: m of the first polyethylenewM of said second polyethylene of 20 ten thousandwM of said third polyethylene of 50 ten thousandwIs 100 ten thousand.
4. The polyolefin separator according to claim 1, wherein: the melting point of the first polyethylene is less than or equal to 126 ℃, and the enthalpy of the first polyethylene is less than or equal to 157J/g; the melting point of the second polyethylene is 132-137 ℃, and the enthalpy is 192-202J/g; the melting point of the third polyethylene is 135-142 ℃, and the enthalpy is not more than 173J/g.
5. The polyolefin separator according to claim 1, characterized in that: the copolymerized polypropylene contains 3-20 wt% of ethylene monomer.
6. The polyolefin separator according to claim 5, characterized in that: the copolymerized polypropylene contains 9-15 wt% of ethylene monomer.
7. 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.
8. The polyolefin separator according to claim 1, characterized in that: the copolymerized polypropylene is a block copolymer.
9. The polyolefin separator according to any one of claims 1 to 8, characterized in that: the microporous membrane contains 80-95 wt% of polyethylene composition and 5-20 wt% of copolymerized polypropylene.
10. The method for preparing a polyolefin separator according to any one of claims 1 to 9, wherein: the method comprises the following steps:
(1) extruding the polyethylene composition, co-polypropylene and plasticizer through a die, cooling to form a gel-like sheet; wherein the extrusion amount is controlled to be 30-170kg/h, the casting speed is controlled to be less than or equal to 20m/min, the casting temperature is controlled to be less than or equal to 35 ℃, and the thickness of the sheet is controlled to be less than or equal to 300 mu m;
(2) sequentially performing longitudinal stretching, first transverse stretching and second transverse stretching on the gel-like sheet; wherein the longitudinal stretching temperature is controlled between 40 ℃ and 130 ℃, and the longitudinal stretching speed ratio is controlled to be less than or equal to 10; the first transverse stretching temperature is controlled between 80 ℃ and 130 ℃, and the first transverse stretching speed ratio is controlled to be less than or equal to 12; the second transverse stretching temperature is controlled to be less than or equal to 130 ℃, and the second transverse stretching speed ratio is controlled to be less than or equal to 2.0.
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Cited By (5)
| 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 |
| WO2022002094A1 (en) * | 2020-07-01 | 2022-01-06 | 华为技术有限公司 | Separator and manufacturing method therefor, and battery, electronic device, and mobile device |
| CN113964448A (en) * | 2020-07-01 | 2022-01-21 | 华为技术有限公司 | Separator, method for manufacturing separator, battery, electronic device, and mobile device |
| CN115458342A (en) * | 2022-09-30 | 2022-12-09 | 浙江海滨薄膜科技有限公司 | BOPP (biaxially-oriented Polypropylene) capacitor film and preparation process thereof |
| CN116435707A (en) * | 2023-06-09 | 2023-07-14 | 宁德新能源科技有限公司 | Electrochemical device and electronic device |
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Cited By (7)
| 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 |
| WO2022002094A1 (en) * | 2020-07-01 | 2022-01-06 | 华为技术有限公司 | Separator and manufacturing method therefor, and battery, electronic device, and mobile device |
| CN113964448A (en) * | 2020-07-01 | 2022-01-21 | 华为技术有限公司 | Separator, method for manufacturing separator, battery, electronic device, and mobile device |
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| CN115458342A (en) * | 2022-09-30 | 2022-12-09 | 浙江海滨薄膜科技有限公司 | BOPP (biaxially-oriented Polypropylene) capacitor film and preparation process thereof |
| CN116435707A (en) * | 2023-06-09 | 2023-07-14 | 宁德新能源科技有限公司 | Electrochemical device and electronic device |
| CN116435707B (en) * | 2023-06-09 | 2023-09-19 | 宁德新能源科技有限公司 | Electrochemical device and electronic device |
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