CN107200903A - Ultra high molecular polyethylene/amylene blending microporous membrane of poly- 4 methyl 1 prepared by a kind of thermally induced phase separation and preparation method thereof - Google Patents
Ultra high molecular polyethylene/amylene blending microporous membrane of poly- 4 methyl 1 prepared by a kind of thermally induced phase separation and preparation method thereof Download PDFInfo
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- CN107200903A CN107200903A CN201710375509.8A CN201710375509A CN107200903A CN 107200903 A CN107200903 A CN 107200903A CN 201710375509 A CN201710375509 A CN 201710375509A CN 107200903 A CN107200903 A CN 107200903A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D7/00—Producing flat articles, e.g. films or sheets
- B29D7/01—Films or sheets
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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
- C08J5/18—Manufacture of films or sheets
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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
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/26—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a solid phase from a macromolecular composition or article, e.g. leaching out
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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
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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
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/05—Elimination by evaporation or heat degradation of a liquid phase
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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
- 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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/068—Ultra high molecular weight polyethylene
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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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- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
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- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
The ultra high molecular polyethylene prepared the invention discloses a kind of thermally induced phase separation/poly-（The amylene of 4 methyl 1）Blending microporous membrane and preparation method thereof.Wherein, 100 parts of ultra-high molecular weight polyethylene, gather（The amylene of 4 methyl 1）1 ~ 20 part, 0.1 ~ 5 part of antioxidant, 0.01 ~ 2 part of aid anti-oxidants.The molecular weight M of described supermolecule weight northylenw=0.5×106~3×106；The invention has the advantages that, gather（The amylene of 4 methyl 1）High-melting-point, high Vicat softening point, excellent mechanical property and low-crystallinity, highly-breathable so that composite micro porous film remains TPX excellent properties.Implementation with other method of modifying is contrasted, and its equipment requirement is simple, only need to slightly be improved and just can directly be produced on original UHMWPE micropores membrane production equipment.Micropore film thickness of the present invention is 5 40 μm of barrier film, and average pore size is 25 100 nanometers, and at 130 DEG C, percent thermal shrinkage is not more than 4.0, and stretch modulus is more than 160MPa, and broken film temperature is more than 200 DEG C.The invention also discloses the method for preparing above-mentioned microporous barrier.
Description
Technical field
The present invention relates to barrier film production technical field, supra polymer prepared by specifically related to a kind of thermally induced phase separation gathers
Ethene/poly- (4-methyl-1-pentene) blending microporous membrane and preparation method thereof.
Background technology
The lithium electric separator of existing market is MIcroporous polyolefin film, and its material mainly has polyethylene and polypropylene.It is such micro-
Pore membrane is functional, price is low, is widely used in fields such as 3C, energy storage and power.But, with to lithium ion battery in electricity
More and more higher is required in terms of pressure, power, electricity and security, heat resistance, absorbency and the security of conventional membrane are more and more not
It can meet and require.Therefore, modified diaphragm and new types of diaphragm are developed into recent years very important study hotspot.
Improved polyalkene diaphragm is after one of focus of attention of polyolefin micropore barrier diaphragm.The present invention intends using poly- (4- first
Base -1- amylenes) enhancing modified ultra-high molecular weight polyethylene, preparing has high softening temperature, high-fire resistance, high stretch modulus and height
The microporous barrier of the performances such as fusing-off temperature.
Poly- (4-methyl-1-pentene), the entitled TPX of business is a kind of Crystalline plastics with three-dimensional isotactic structure,
Natta was synthesized first in 1956.TPX is the thermoplastic of density minimum so far, and density is 0.83g/cm3, mainly
Feature has：Heat-resist, 195 DEG C or so of Vicat softening point, fusing point is up to 240 DEG C, and resistance to environment and chemical-resistance are good, mechanics
Performance is outstanding, disclosure satisfy that at present to membrane material under severe conditions use the need for.
The content of the invention
To improve microporous barrier combination property, there is provided a kind of high softening temperature, high-fire resistance, high stretch modulus and high fusing temperature
Ultra high molecular polyethylene/poly- (4-methyl-1-pentene) blending microporous membranes of performance such as degree and preparation method thereof.
Technical scheme：
Ultra high molecular polyethylene/poly- (4-methyl-1-pentene) blending microporous membrane of the present invention is by superhigh molecular weight polyethylene
Alkene, poly- (4-methyl-1-pentene), antioxidant and aid anti-oxidants are constituted, wherein：
The molecular weight M of described supermolecule weight northylenw=0.5 × 106~3 × 106。
As a kind of mode of priority, described antioxidant is the conventional antioxidant of this area, such as hindered phenol, phosphite ester or
Organic sulfur compound, preferably β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid isooctanol ester, β-(3,5- di-t-butyl -4-
Hydroxy phenyl) the positive octadecanol ester of propionic acid, N, N-1,6- inferior hexyls-bis- [3- (3,5- di-tert-butyl-hydroxy phenyls) propionamide
One or both of more than mixture.
As a kind of mode of priority, described aid anti-oxidants are the conventional aid anti-oxidants of this area, preferably diphosphorous acid season
The hard ester alcohol ester of penta tetrol two, thio-2 acid 2 stearyl ester, phosphorous acid three (2,4-di-tert-butyl-phenyl) ester, thio dipropyl
Mixture more than one or both of sour dilauryl.
To ensure ultra high molecular polyethylene/original excellent properties of poly- (4-methyl-1-pentene) blending microporous membrane, preferably
Improve its high softening temperature, high-fire resistance, high stretch modulus and high fusing-off temperature etc., its preparation method is very crucial, the present invention
There is provided a kind of ultra high molecular polyethylene/poly- (4-methyl-1-pentene) blending microporous membrane and preparation method thereof, this method is included such as
Lower step：
(1) poly- (4-methyl-1-pentene) is well mixed with antioxidant and aid anti-oxidants；
(2) by the mixed of diluent and ultra-high molecular weight polyethylene, poly- (4-methyl-1-pentene) and antioxidant and aid anti-oxidants
Compound is proportionally added into double screw extruder and is plastified, be blended；
(3) oil film is carried out two-way drawing by the melt for forming double screw extruder by die head, chilling roller formation oil film
Stretch, extract, ultra high molecular polyethylene/poly- (4-methyl-1-pentene) blending microporous membrane is made in thermal finalization.
As a kind of mode of priority, described processing and forming is extrusion molding, and extrusion temperature is 150 DEG C~260 DEG C, curtain coating
Die head temperature is 150 DEG C~260 DEG C.
The beneficial effects of the present invention are：
The present invention only need to slightly be improved on original UHMWPE micropores membrane production equipment and can directly produced；Institute of the present invention
The micropore film thickness of preparation is 5-40 μm, and average pore size is 25-100 nanometers, and at 130 DEG C, percent thermal shrinkage is not more than 4.0, stretching
Modulus is more than 160MPa, and broken film temperature is more than 200 DEG C.Microporous barrier prepared by the present invention has high softening temperature, high-fire resistance, height
The advantages of stretch modulus and high fusing-off temperature.
Embodiment
The present invention is described in further detail with reference to embodiment.
Embodiment 1
By 5 parts of TPX (commercially available, MX002) and 1 part of antioxidant (β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid isooctanol
Ester), the blending of 0.05 part of aid anti-oxidants (the hard ester alcohol ester of diphosphorous acid pentaerythrite two).By the above-mentioned TPX and UHMWPE mixed
Powder presses 5：100 parts of proportionings are added in extruder, uniform with paraffin oil plasticizing, blending.
Oil film is carried out biaxial tension, extraction by the melt that double screw extruder is formed by die head, chilling roller formation oil film
Take, ultra high molecular polyethylene/poly- (4-methyl-1-pentene) blending microporous membrane is made in thermal finalization, you can obtain the micropore of the present invention
Film.The performance test results such as table 1.
Comparative example 1
In addition to without any TPX, preparation process as described above prepares ultra-high molecular mass polyethylene micropore
Film.The performance test results such as table 1.
Embodiment 2
By 5 parts of TPX (commercially available, MX002) and 1 part of antioxidant (β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid isooctanol
Ester), the blending of 0.05 part of aid anti-oxidants (the hard ester alcohol ester of diphosphorous acid pentaerythrite two).By the above-mentioned TPX and UHMWPE mixed
Powder presses 10：100 parts of proportionings are added in extruder, uniform with paraffin oil plasticizing, blending.
Oil film is carried out biaxial tension, extraction by the melt that double screw extruder is formed by die head, chilling roller formation oil film
Take, ultra high molecular polyethylene/poly- (4-methyl-1-pentene) blending microporous membrane is made in thermal finalization, you can obtain the micropore of the present invention
Film.The performance test results such as table 1.
Embodiment 3
By 5 parts of TPX (commercially available, MX002) and 1 part of antioxidant (β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid isooctanol
Ester), the blending of 0.05 part of aid anti-oxidants (the hard ester alcohol ester of diphosphorous acid pentaerythrite two).By the above-mentioned TPX and UHMWPE mixed
Powder presses 15：100 parts of proportionings are added in extruder, uniform with paraffin oil plasticizing, blending.
Oil film is carried out biaxial tension, extraction by the melt that double screw extruder is formed by die head, chilling roller formation oil film
Take, ultra high molecular polyethylene/poly- (4-methyl-1-pentene) blending microporous membrane is made in thermal finalization, you can obtain the micropore of the present invention
Film.The performance test results such as table 1.
Table 1
From table 1, ultra high molecular polyethylene/poly- (the 4- methyl isophthalic acids-amylene) of poly- (4-methyl-1-pentene) is added altogether
Mixed microporous barrier, due to poly- (4-methyl-1-pentene) high-melting-point, high Vicat softening point, excellent mechanical property so that composite microporous
Film remains TPX excellent properties.Simultaneously as conventional polyolefin (polyethylene, polypropylene) crystallinity is very high, it passes through polymerization
The ability of thing segment transmission lithium ion is very weak, and ultra high molecular polyethylene/poly- (4-methyl-1-pentene) blending microporous membrane is not crystallized
PE segments and the random segments of TPX be swelled by electrolyte, provide polymer segment pipeline for the transmission of lithium ion so that
Blending microporous membrane possesses higher ionic conductivity.
Above is to ultra high molecular polyethylene in the present invention/poly- (4-methyl-1-pentene) blending microporous membrane and its preparation side
Method is set forth, and is used to help understand the present invention, but embodiments of the present invention and is not restricted to the described embodiments, any
Without departing from the change made under the principle of the invention, modification, replacement, combination, simplification, equivalent substitute mode is should be, is all included
Within protection scope of the present invention.
Claims (9)
1. ultra high molecular polyethylene prepared by a kind of thermally induced phase separation/poly-（4-methyl-1-pentene）Blending microporous membrane, its feature
It is, by ultra-high molecular weight polyethylene, gathers（4-methyl-1-pentene）, antioxidant and aid anti-oxidants constitute, wherein：
100 parts of ultra-high molecular weight polyethylene
It is poly-（4-methyl-1-pentene）1 ~ 20 part
0.1 ~ 5 part of antioxidant
0.01 ~ 2 part of aid anti-oxidants.
2. ultra high molecular polyethylene prepared by thermally induced phase separation according to claim 1/poly-（4-methyl-1-pentene）Altogether
Mixed microporous barrier, it is characterised in that：The molecular weight M of described ultra-high molecular weight polyethylenew=0.5×106~3×106。
3. ultra high molecular polyethylene prepared by thermally induced phase separation according to claim 1/poly-（4-methyl-1-pentene）Altogether
Mixed microporous barrier, it is characterised in that：Described is poly-（4-methyl-1-pentene）It is the olefin-copolymerization based on 4-methyl-1-pentene
Thing.
4. ultra high molecular polyethylene prepared by thermally induced phase separation according to claim 1/poly-（4-methyl-1-pentene）Altogether
Mixed microporous barrier, it is characterised in that：The antioxidant is hindered phenol, phosphite ester or organic sulfur compound kind antioxidant.
5. ultra high molecular polyethylene prepared by thermally induced phase separation according to claim 4/poly-（4-methyl-1-pentene）Altogether
Mixed microporous barrier, it is characterised in that：The antioxidant be β-(3,5- di-tert-butyl-hydroxy phenyls) propionic acid isooctanol ester, β-（3,
5- di-tert-butyl-hydroxy phenyls）The positive octadecanol ester of propionic acid, N, N -1,6- inferior hexyls-bis- [3- (3,5- di-t-butyls -4-
Hydroxy phenyl) more than one or both of propionamide mixture.
6. ultra high molecular polyethylene prepared by thermally induced phase separation according to claim 1/poly-（4-methyl-1-pentene）Altogether
Mixed microporous barrier, it is characterised in that：Described aid anti-oxidants are the hard ester alcohol ester of diphosphorous acid pentaerythrite two, thio-2 acid two is hard
Lipidol ester, phosphorous acid three（2,4-di-tert-butyl-phenyl）It is more than one or both of ester, dilauryl thiodipropionate mixed
Compound.
7. any one of preparation claim 1 ~ 6 ultra high molecular polyethylene/poly-（4-methyl-1-pentene）The side of blending microporous membrane
Method, it is characterised in that comprise the following steps：
（1）Will be poly-（4-methyl-1-pentene）It is well mixed with antioxidant and aid anti-oxidants；
（2）By diluent and ultra-high molecular weight polyethylene, gather（4-methyl-1-pentene）With antioxidant and the mixture of aid anti-oxidants
Double screw extruder is proportionally added into be plastified, be blended；
（3）Oil film is carried out biaxial tension, extraction by the melt that double screw extruder is formed by die head, chilling roller formation oil film
Take, ultra high molecular polyethylene/poly- is made in thermal finalization（4-methyl-1-pentene）Blending microporous membrane.
8. preparation method according to claim 7, it is characterised in that：Described processing and forming is extrusion molding, extrusion temperature
Spend for 150 DEG C ~ 260 DEG C, casting head temperature is 150 DEG C ~ 260 DEG C.
9. preparation method according to claim 7, it is characterised in that：Described diluent be saturated fatty acid, mineral oil,
At least one of saturated alcohols, ester, ether.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710375509.8A CN107200903A (en) | 2017-05-24 | 2017-05-24 | Ultra high molecular polyethylene/amylene blending microporous membrane of poly- 4 methyl 1 prepared by a kind of thermally induced phase separation and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710375509.8A CN107200903A (en) | 2017-05-24 | 2017-05-24 | Ultra high molecular polyethylene/amylene blending microporous membrane of poly- 4 methyl 1 prepared by a kind of thermally induced phase separation and preparation method thereof |
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| CN107200903A true CN107200903A (en) | 2017-09-26 |
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| CN201710375509.8A Pending CN107200903A (en) | 2017-05-24 | 2017-05-24 | Ultra high molecular polyethylene/amylene blending microporous membrane of poly- 4 methyl 1 prepared by a kind of thermally induced phase separation and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111748157A (en) * | 2019-03-28 | 2020-10-09 | 合肥杰事杰新材料股份有限公司 | High-transparency modified polyolefin material and preparation method thereof |
| CN112778679A (en) * | 2020-12-31 | 2021-05-11 | 苏州市新广益电子有限公司 | High-strength and high-thermal-stability poly (4-methyl-1-pentene) microporous membrane and preparation method thereof |
| CN112831130A (en) * | 2020-12-31 | 2021-05-25 | 苏州市新广益电子有限公司 | Poly 4-methyl-1-pentene microporous membrane and preparation method thereof |
| CN113121902A (en) * | 2021-03-23 | 2021-07-16 | 江西铜业股份有限公司 | Rapid-forming ultrahigh molecular weight polyethylene pipe and preparation method thereof |
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| CN113121902A (en) * | 2021-03-23 | 2021-07-16 | 江西铜业股份有限公司 | Rapid-forming ultrahigh molecular weight polyethylene pipe and preparation method thereof |
| CN113121902B (en) * | 2021-03-23 | 2022-11-22 | 江西铜业股份有限公司 | Rapid forming ultra-high molecular weight polyethylene pipe and preparation method thereof |
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