WO2016111323A1 - 微多孔膜およびその製造方法 - Google Patents
微多孔膜およびその製造方法 Download PDFInfo
- Publication number
- WO2016111323A1 WO2016111323A1 PCT/JP2016/050307 JP2016050307W WO2016111323A1 WO 2016111323 A1 WO2016111323 A1 WO 2016111323A1 JP 2016050307 W JP2016050307 W JP 2016050307W WO 2016111323 A1 WO2016111323 A1 WO 2016111323A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- microporous membrane
- film
- membrane according
- porosity
- microporous
- Prior art date
Links
- 239000012982 microporous membrane Substances 0.000 title claims abstract description 65
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- -1 polypropylene Polymers 0.000 claims abstract description 26
- 239000004743 Polypropylene Substances 0.000 claims abstract description 25
- 229920001155 polypropylene Polymers 0.000 claims abstract description 25
- 229920000642 polymer Polymers 0.000 claims abstract description 22
- 239000000155 melt Substances 0.000 claims abstract description 13
- 230000035699 permeability Effects 0.000 claims description 17
- 238000002844 melting Methods 0.000 claims description 14
- 230000008018 melting Effects 0.000 claims description 14
- 230000005611 electricity Effects 0.000 claims description 9
- 239000003990 capacitor Substances 0.000 claims description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 4
- 125000004432 carbon atom Chemical group C* 0.000 claims description 4
- 229910001416 lithium ion Inorganic materials 0.000 claims description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 3
- 239000005977 Ethylene Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000004711 α-olefin Substances 0.000 claims description 3
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 claims description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 2
- 230000002040 relaxant effect Effects 0.000 claims description 2
- 239000012229 microporous material Substances 0.000 claims 1
- 229920005989 resin Polymers 0.000 abstract description 6
- 239000011347 resin Substances 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 238000000034 method Methods 0.000 description 31
- 239000002994 raw material Substances 0.000 description 23
- 229920005672 polyolefin resin Polymers 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000654 additive Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 229920001384 propylene homopolymer Polymers 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 229920000098 polyolefin Polymers 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- WSSSPWUEQFSQQG-UHFFFAOYSA-N 4-methyl-1-pentene Chemical compound CC(C)CC=C WSSSPWUEQFSQQG-UHFFFAOYSA-N 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000010622 cold drawing Methods 0.000 description 2
- 150000001993 dienes Chemical class 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000012188 paraffin wax Substances 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920003002 synthetic resin Polymers 0.000 description 2
- 239000000057 synthetic resin Substances 0.000 description 2
- YHQXBTXEYZIYOV-UHFFFAOYSA-N 3-methylbut-1-ene Chemical compound CC(C)C=C YHQXBTXEYZIYOV-UHFFFAOYSA-N 0.000 description 1
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical compound CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 239000003484 crystal nucleating agent Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 229920005653 propylene-ethylene copolymer Polymers 0.000 description 1
- 150000003440 styrenes Chemical class 0.000 description 1
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/001—Combinations of extrusion moulding with other shaping operations
- B29C48/0018—Combinations of extrusion moulding with other shaping operations combined with shaping by orienting, stretching or shrinking, e.g. film blowing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/07—Flat, e.g. panels
- B29C48/08—Flat, e.g. panels flexible, e.g. films
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/88—Thermal treatment of the stream of extruded material, e.g. cooling
- B29C48/91—Heating, e.g. for cross linking
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C55/00—Shaping by stretching, e.g. drawing through a die; Apparatus therefor
- B29C55/02—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C55/00—Shaping by stretching, e.g. drawing through a die; Apparatus therefor
- B29C55/02—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets
- B29C55/04—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets uniaxial, e.g. oblique
- B29C55/06—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets uniaxial, e.g. oblique parallel with the direction of feed
- B29C55/065—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets uniaxial, e.g. oblique parallel with the direction of feed in several stretching steps
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F10/00—Homopolymers and copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F10/04—Monomers containing three or four carbon atoms
- C08F10/06—Propene
-
- 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
-
- 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
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/52—Separators
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/02—Diaphragms; Separators
-
- 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
- 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
-
- 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
- H01M50/406—Moulding; Embossing; Cutting
-
- 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
- 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
- H01M50/414—Synthetic resins, e.g. thermoplastics or thermosetting resins
- H01M50/417—Polyolefins
-
- 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
- H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
-
- 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
- H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
- H01M50/491—Porosity
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2023/00—Use of polyalkenes or derivatives thereof as moulding material
- B29K2023/10—Polymers of propylene
- B29K2023/12—PP, i.e. polypropylene
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
- B29K2105/04—Condition, form or state of moulded material or of the material to be shaped cellular or porous
- B29K2105/041—Microporous
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2031/00—Other particular articles
- B29L2031/755—Membranes, diaphragms
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2500/00—Characteristics or properties of obtained polyolefins; Use thereof
- C08F2500/12—Melt flow index or melt flow ratio
-
- 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
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
-
- 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
- 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
- Y02E60/13—Energy storage using capacitors
Definitions
- the present invention relates to a microporous membrane made of a polypropylene polymer, an electricity storage device obtained therefrom, and a method for producing the microporous membrane.
- microporous membranes are used as separators for power storage devices such as batteries and capacitors.
- a microporous membrane for a separator is required to have a basic performance as a separator, in which an electrode can be isolated and has ion conductivity.
- Polyolefin resins are useful as battery separator materials because they have high chemical resistance and can be made porous by various methods. Moreover, since polyolefin resins are relatively inexpensive among synthetic resins, polyolefin battery separators are also advantageous in reducing battery manufacturing costs.
- the method for making a polyolefin resin film porous is roughly classified into a wet method and a dry method.
- a molten mixture of a polyolefin-based resin and a plasticizer, oil, paraffin or the like is developed into a film.
- components other than the polyolefin are extracted, and the portions where these components exist are voided.
- the polyolefin resin is molded into a microporous film.
- the dry method is a method in which a polyolefin resin is molded into a microporous film by stretching a raw material mainly containing a polyolefin resin that does not contain components such as plasticizer, oil, paraffin, and a solvent.
- Patent Documents 1, 2, and 3 describe that a polyolefin resin is made porous to produce a microporous membrane having a high porosity and that the obtained microporous membrane is used as a battery separator.
- Patent Document 1 describes that a raw material composed of a mixture of a polyolefin resin and a conjugated diene polymer is processed into a microporous film having a desired porosity by a wet method.
- Patent Document 2 describes that a mixture of polypropylene and polyethylene is processed into a microporous film having a desired porosity by stretching it in two stages by a dry method.
- Patent Document 3 describes that a mixture in which a low molecular weight substance is blended with polyolefin is processed into a microporous film having a desired porosity by stretching it in two stages by a dry method.
- the inventors of the present invention have studied diligently to produce a microporous film having a good porosity by a dry method using an inexpensive polypropylene resin as a raw material without blending with other resins. .
- a polypropylene resin having a specific melt mass flow rate was used as a raw material, and a microporous membrane having a high porosity was successfully produced by a dry method.
- the present invention is as follows.
- (Invention 1) It consists of a polypropylene-based polymer whose melt mass flow rate (measured in accordance with MFR, JIS K6758 (230 ° C., 21.18 N)) is 1.0 g / 10 min or less, and has a porosity of 50%. This is the microporous membrane.
- Invention 2 The microporous membrane of Invention 1 having a porosity in the range of 50 to 60%.
- Invention 3 The microporous membrane of Invention 1 or 2 having an air permeability of 200 sec / 100 mL or more.
- invention 4 The microporous membrane according to any one of Inventions 1 to 3, wherein the air permeability is in the range of 200 to 300 sec / 100 mL.
- the polypropylene polymer has a melting point in the range of 150 to 170 ° C., and a melt mass flow rate (measured in accordance with MFR, JIS K6758 (230 ° C., 21.18 N)) is 1.0 g / 10
- Invention 6 The microporous membrane according to any one of Inventions 1 to 5, which is used for a separator of an electricity storage device.
- invention 7 The microporous membrane of Invention 6, wherein the electricity storage device is a lithium ion battery.
- (Invention 12) A method for producing a microporous membrane according to any one of Inventions 1 to 11, comprising the following steps.
- (Process 1) A polypropylene film having a melt mass flow rate (MFR) measured at 230 ° C. and a load of 21.18 N in accordance with JIS K6758 of 1.0 g / 10 min or less is extruded to produce a raw film. The film forming step.
- (Step 2) A step of heat-treating the raw film obtained in Step 1.
- (Step 3) A step of stretching the heat-treated raw film obtained in Step 2 at ⁇ 5 to 45 ° C. in the length direction by 1.0 to 1.1 times.
- Step 4 A step of stretching the stretched film after Step 3 at a temperature lower by 5 to 65 ° C. than the melting point of the polypropylene polymer by 1.5 to 4.0 times in the length direction.
- Step 5 A step of relaxing the hot-stretched film obtained in Step 4 under heating so that the length becomes 0.7 to 1.0 times.
- the microporous membrane of the present invention has a high porosity of 50% or more, preferably 50 to 60%. This can be expected to have high ionic conductivity when the microporous membrane of the present invention is used as a separator material.
- the microporous membrane of the present invention has an air permeability of 200 sec / 100 mL or more, preferably 200 to 300 sec / mL.
- the number of pores per surface area of the microporous membrane is reflected in the porosity, and the average size of the micropores in the microporous membrane is reflected in the air permeability.
- the balance between the porosity and the air permeability of the present invention can be expected to have many relatively small micropores formed on the surface of the microporous film of the present invention. From this, the microporous membrane of the present invention can be expected to have relatively stable and uniform material permeability.
- the microporous membrane of the present invention comprises a polypropylene polymer having a melt mass flow rate (measured in accordance with MFR, JIS K6758 (230 ° C., 21.18N)) of 1.0 g / 10 min or less, and has pores. The rate is 50% or more.
- the raw material of the microporous membrane of the present invention is a polypropylene polymer, which corresponds to a propylene homopolymer or a copolymer obtained by copolymerizing a comonomer.
- the polypropylene polymer used in the present invention preferably has a relatively high crystallinity and a melting point in the range of 150 to 170 ° C., more preferably a melting point in the range of 155 to 168 ° C.
- the comonomer is generally at least one selected from ethylene and an ⁇ -olefin having 4 to 8 carbon atoms.
- these may be copolymerized with branched olefins having 4 to 8 carbon atoms such as 2-methylpropene, 3-methyl-1-butene, 4-methyl-1-pentene, styrenes and dienes. Good.
- the content of the comonomer may be in any range as long as the microporous film exhibits desired properties. Preferably, it is 5 parts by weight or less, particularly 2 parts by weight or less with respect to 100 parts by weight of the polymer, which is a range giving a highly crystalline polypropylene polymer.
- the polypropylene-based polymer has a melt mass flow rate (measured in accordance with MFR, JIS K6758 (230 ° C., 21.18 N)) of 1.0 g / 10 min or less, preferably 0.2 to 0.6. .
- additives such as a crystal nucleating agent and a filler can be blended.
- the type and amount of the additive are not limited as long as the porosity is not impaired.
- the microporous membrane of the present invention is produced by a so-called dry method using the above-described raw materials.
- the method for producing a microporous membrane of the present invention includes the following steps 1 to 5.
- Step 1 Film-forming step
- MFR melt mass flow rate
- JIS K6758 JIS K6758
- any of a single screw extruder, a twin screw extruder, and a tandem type extruder can be used.
- Any die can be used as long as it is used for film forming.
- the dice for example, various T-type dice can be used.
- the thickness and shape of the raw film are not particularly limited.
- the ratio (draft ratio) between the die slip clearance and the raw film thickness is 100 or more, more preferably 150 or more.
- the thickness of the raw film is 10 to 200 ⁇ m, more preferably 15 to 100 ⁇ m.
- Process 2 Heat treatment process This is a step of heat-treating the raw film after step 1 is completed.
- a constant tension in the length direction is applied to the original film at a temperature 5 to 65 ° C., preferably 10 to 25 ° C. lower than the melting point of the polypropylene polymer.
- the tension is preferably such that the length of the raw film exceeds 1.0 and is 1.1 times or less.
- the stretching temperature is ⁇ 5 to 45 ° C., preferably 5 to 30 ° C.
- the draw ratio is 1.0 to 1.1, preferably 1.00 to 1.08, more preferably 1.02 or more and less than 1.05 in the length direction. However, the draw ratio is greater than 1.0.
- the stretching means is not limited. Known means such as a roll stretching method and a tenter stretching method can be used. The number of stretching stages can be set arbitrarily. One-stage stretching may be performed, and two or more stages of stretching may be performed through a plurality of rolls.
- the molecules of the polypropylene polymer constituting the raw film are oriented.
- a stretched film having a lamellar portion with a dense molecular chain and a region (craze) with a loose molecular chain between lamellas is obtained.
- Step 4 Warm stretching process
- the stretching temperature is 5 to 65 ° C. lower than the melting point of the polypropylene polymer, preferably 10 to 45 ° C. lower than the melting point of the polypropylene polymer.
- the draw ratio is 1.5 to 4.5 times in the length direction, preferably 2.0 to 4.0 times.
- the stretching means is not limited. Known means such as a roll stretching method and a tenter stretching method can be used.
- the number of stretching stages can be set arbitrarily. One-stage stretching may be performed, and two or more stages of stretching may be performed through a plurality of rolls.
- the warm drawing step the craze produced in step 3 is stretched and voids are generated.
- Step 5 Relaxation process
- the relaxation temperature is slightly higher than the temperature of warm drawing, and is generally 0 to 20 ° C. higher.
- the degree of relaxation is adjusted so that the length of the stretched film after Step 4 is finally 0.7 to 1.0 times.
- the “porosity” and “air permeability” of the microporous membrane of the present invention are measured under the following conditions.
- Air permeability This is the air permeability determined by the Gurley test in an atmosphere of room temperature 23 ° C. ⁇ 2 ° C. and humidity 50% ⁇ 5% based on JIS P8117.
- the porosity of the microporous membrane of the present invention is 50% or more, preferably 50 to 60%.
- the air permeability of the microporous membrane of the present invention is 200 sec / 100 mL or more, preferably in the range of 200 to 300 sec / 100 mL.
- Example 1 (Raw material) A propylene homopolymer having a melt mass flow rate (MFR) of 0.5 g / 10 minutes and a melting point of 165 ° C. measured according to JIS K6758 (230 ° C., 21.18 N) was used as a raw material for the microporous membrane.
- MFR melt mass flow rate
- Step 1 The raw material melt-kneaded with a single screw extruder was extruded from a T-die at a draft ratio of 159 to produce a raw film having a thickness of 22 ⁇ m.
- Step 2 Next, the raw film was heat-treated at 150 ° C.
- Step 4 The obtained stretched film was warm-stretched 3.0 times in the length direction at 145 ° C. (Step 5) It was relaxed at 150 ° C. so that the length of the obtained stretched film was 0.88 times.
- the microporous membrane of the present invention having a final thickness of 20 ⁇ m was obtained.
- the porosity and air permeability of the obtained microporous membrane were measured by the method described above, and the results are shown in Table 1 together with the production conditions.
- an air permeability meter (Gurley type densometer) manufactured by Toyo Seiki Seisakusho was used.
- Example 2 (Raw material) A propylene homopolymer having a melt mass flow rate (MFR) of 0.5 g / 10 minutes and a melting point of 165 ° C. measured according to JIS K6758 (230 ° C., 21.18 N) was used as a raw material for the microporous membrane.
- MFR melt mass flow rate
- Step 1 The raw material melt-kneaded with a single screw extruder was extruded from a T-die at a draft ratio of 159 to produce a raw film having a thickness of 22 ⁇ m.
- Step 2 Next, the raw film was heat-treated at 150 ° C.
- Step 4 The obtained stretched film was warm-stretched 3.0 times in the length direction at 145 ° C. (Step 5) It was relaxed at 150 ° C. so that the length of the obtained stretched film was 0.88 times.
- the microporous membrane of the present invention having a final thickness of 20 ⁇ m was obtained.
- the evaluation results are shown in Table 1 together with the production conditions.
- Step 4 The obtained stretched film was warm-stretched 3.2 times in the length direction at 145 ° C. (Step 5) It was relaxed at 150 ° C. so that the length of the obtained stretched film was 0.88 times. A comparative microporous membrane having a final thickness of 20 ⁇ m was thus obtained. The evaluation results are shown in Table 1 together with the production conditions.
- Step 4 The obtained stretched film was warm-stretched 3.0 times in the length direction at 128 ° C. (Step 5) It was relaxed at 150 ° C. so that the length of the obtained stretched film was 0.88 times. A comparative microporous membrane having a final thickness of 20 ⁇ m was thus obtained. The evaluation results are shown in Table 1 together with the production conditions.
- the porosity of the microporous membrane of the present invention obtained in Examples 1 and 2 shows a high value of 54%.
- the porosity of the microporous membranes of Comparative Examples 1 and 2 does not reach 50%, and the practicality as a battery separator is poor.
- Examples 1 and 2 are predicted to have a high density of micropores having a relatively small pore diameter as compared with Comparative Examples 1 and 2. Such a micropore shape is also reflected in the air permeability per thickness of the microporous membrane.
- Examples 1 and 2 are considered to exhibit relatively high ionic conductivity stably.
- the microporous membrane of the present invention is made of a raw material that has sufficient porosity and does not contain any special additives. Such a microporous membrane of the present invention is useful as a battery separator material that has excellent ionic conductivity and can be produced at low cost.
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- Microelectronics & Electronic Packaging (AREA)
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Abstract
Description
(工程1)JIS K6758に準拠して230℃、荷重21.18Nで測定したメルトマスフローレイト(MFR)が1.0g/10分以下であるポリプロピレン系重合体を押出成形して原反フィルムを製膜する工程。
(工程2)工程1で得られた原反フィルムを熱処理する工程。
(工程3)工程2で得られた熱処理後の原反フィルムを、-5~45℃で、長さ方向に1.0~1.1倍に延伸する工程。
(工程4)工程3を終えた延伸フィルムを、ポリプロピレン系重合体の融点よりも5~65℃低い温度で、長さ方向に1.5~4.0倍に延伸する工程。
(工程5)工程4で得られた温延伸後のフィルムを、加熱下、長さが0.7~1.0倍になるように弛緩させる工程。
本発明の微多孔膜の原料は、ポリプロピレン系重合体であって、プロピレンの単独重合体あるいはコモノマーを共重合した共重合体がこれに相当する。本発明で使用するポリプロピレン系重合体としては、結晶性が比較的高い、融点が150~170℃の範囲にあるものが好ましく、融点が155~168℃の範囲にあるものがさらに好ましい。上記コモノマーは、一般的には、エチレンおよび炭素数4~8のα-オレフィンから選ばれる少なくとも1種である。またこれらと共に、2-メチルプロペン、3-メチル-1-ブテン、4-メチル-1-ペンテンなどの炭素数4~8の分岐オレフィン類、スチレン類、ジエン類を共重合したものであってもよい。
本発明の微多孔膜は、上述の原料を用いて、いわゆる乾式法によって製造される。本発明の微多孔膜の製造方法は、以下の工程1~5を含む。
原料を押出成形して原反フィルムを製膜する工程である。JIS K6758に準拠して230℃、荷重21.18Nで測定したメルトマスフローレイト(MFR)が1.0g/10分以下であるポリプロピレン系重合体を押出機に供給し、ポリプロピレン系重合体をその融点以上の温度で溶融混練し、押出機の先端に取り付けたダイスからポリプロピレン系重合体フィルムを押出す。使用される押出機は限定されない。押出機としては、例えば、単軸押出機、二軸押出機、タンデム型押出機のいずれもが使用可能である。使用されるダイスはフィルム成形に用いられるものであれば、いずれも使用できる。ダイスとしては、例えば、各種T型ダイス使用することができる。原反フィルムの厚みや形状は特に限定されない。好ましくは、ダイスリップクリアランスと原反フィルム厚さの比(ドラフト比)は100以上、さらに好ましくは150以上である。好ましくは、原反フィルムの厚みは10~200μm、さらに好ましくは15~100μmである。
工程1を終えた原反フィルムを熱処理する工程である。ポリプロピレン系重合体の融点よりも5~65℃、好ましくは10~25℃低い温度で、原反フィルムに長さ方向の一定の張力を加える。張力は、好ましくは、原反フィルムの長さが1.0倍を超え1.1倍以下となる大きさである。
工程2を終えた熱処理後の原反フィルムを比較的低い温度で延伸する工程である。延伸温度は-5~45℃、好ましくは5~30℃である。延伸倍率は、長さ方向に1.0~1.1、好ましくは1.00~1.08、さらに好ましくは1.02以上1.05未満である。ただし、延伸倍率は1.0倍より大きい。延伸手段は制限されない。ロール延伸法、テンター延伸法などの公知の手段が使用できる。延伸の段数は任意に設定できる。1段延伸でもよく、複数のロールを経て2段以上の延伸を行ってもよい。冷延伸工程で、原反フィルムを構成するポリプロピレン系重合体の分子が配向する。その結果、分子鎖が密なラメラ部と、ラメラ間の分子鎖が疎な領域(クレーズ)とを有する延伸フィルムが得られる。
工程3を終えた延伸フィルムを比較的高い温度で延伸する工程である。延伸温度はポリプロピレン系重合体の融点よりも5~65℃低い温度、好ましくはポリプロピレン系重合体の融点よりも10~45℃低い温度である。延伸倍率は、長さ方向に1.5~4.5倍、好ましくは2.0~4.0倍である。延伸手段は制限されない。ロール延伸法、テンター延伸法などの公知の手段が使用できる。延伸の段数は任意に設定できる。1段延伸でもよく、複数のロールを経て2段以上の延伸を行ってもよい。温延伸工程で工程3で生じたクレーズが引き延ばされ、空孔が発生する。
工程4を終えた温延伸後のフィルムの収縮を防ぐためにフィルムを弛緩させる工程である。弛緩温度は、温延伸の温度よりもやや高い温度であり、0~20℃高い温度が一般的である。弛緩の度合いは、工程4を終えた延伸フィルムの長さが最終的に0.7~1.0倍になるように調整される。
幅50mm×長さ120mmの微多孔膜切片について、以下の計算式により算出した値である。
空孔率(%)=[1-(切片重量)/(切片面積×樹脂密度×切片厚み)]×100
JIS P8117に準拠し、室温23℃±2℃、湿度50%±5%の雰囲気における、ガーレー試験によって求めた通気度である。
(原料)微多孔膜の原料として、JIS K6758(230℃、21.18N)に従い測定したメルトマスフローレイト(MFR)が0.5g/10分、融点が165℃のプロピレン単独重合体を使用した。(工程1)単軸押出機で溶融混練した原料をドラフト比159でTダイから押出し、厚さ22μmの原反フィルムを製造した。(工程2)次いで、原反フィルムを150℃で熱処理した。(工程3)原反フィルムを30℃で長さ方向に1.03倍に冷延伸した。(工程4)得られた延伸フィルムを145℃で長さ方向に3.0倍に温延伸した。(工程5)得られた延伸フィルムの長さが0.88倍になるように150℃で弛緩させた。こうして最終厚みが20μmの本発明の微多孔膜が得られた。得られた微多孔膜の空孔率と通気度を上述の方法で測定し、その結果を製造条件と共に表1に示す。なお通気度の測定には、東洋精機製作所社製の通気度計(ガーレ式デンソメータ)を用いた。
(原料)微多孔膜の原料として、JIS K6758(230℃、21.18N)に従い測定したメルトマスフローレイト(MFR)が0.5g/10分、融点が165℃のプロピレン単独重合体を使用した。(工程1)単軸押出機で溶融混練した原料をドラフト比159でTダイから押出し、厚さ22μmの原反フィルムを製造した。(工程2)次いで、原反フィルムを150℃で熱処理した。(工程3)原反フィルムを30℃で長さ方向に1.04倍に冷延伸した。(工程4)得られた延伸フィルムを145℃で長さ方向に3.0倍に温延伸した。(工程5)得られた延伸フィルムの長さが0.88倍になるように150℃で弛緩させた。こうして最終厚みが20μmの本発明の微多孔膜が得られた。評価結果を製造条件と共に表1に示す。
(原料)微多孔膜の原料として、JIS K6758(230℃、21.18N)に従い測定したメルトマスフローレイト(MFR)が2.0g/10分、融点が165℃のプロピレン単独重合体を使用した。(工程1)単軸押出機で溶融混練した原料をドラフト比159でTダイから押出し、厚さ22μmの原反フィルムを製造した。(工程2)次いで、原反フィルムを150℃で熱処理した。(工程3)原反フィルムを30℃で長さ方向に1.07倍に温延伸した。(工程4)得られた延伸フィルムを145℃で長さ方向に3.2倍に温延伸した。(工程5)得られた延伸フィルムの長さが0.88倍になるように150℃で弛緩させた。こうして最終厚みが20μmの比較用の微多孔膜が得られた。評価結果を製造条件と共に表1に示す。
(原料)微多孔膜の原料として、JIS K6758(230℃、21.18N)に従い測定したメルトマスフローレイト(MFR)が1.5g/10分、融点が158℃のプロピレン-エチレン共重合体を使用した。(工程1)単軸押出機で溶融混練した原料をドラフト比159でTダイから押出し、厚さ22μmの原反フィルムを製造した。(工程2)次いで、原反フィルムを150℃で熱処理した。(工程3)原反フィルムを30℃で長さ方向に1.04倍に冷延伸した。(工程4)得られた延伸フィルムを128℃で長さ方向に3.0倍に温延伸した。(工程5)得られた延伸フィルムの長さが0.88倍になるように150℃で弛緩させた。こうして最終厚みが20μmの比較用の微多孔膜が得られた。評価結果を製造条件と共に表1に示す。
Claims (12)
- メルトマスフローレイト(MFR、JIS K6758(230℃、21.18N)に準拠した条件で測定)が1.0g/10分以下であるポリプロピレン系重合体からなり、空孔率が50%以上である、微多孔膜。
- 空孔率が50~60%の範囲にある、請求項1に記載の微多孔膜。
- 通気度が200sec/100mL以上である、請求項1または2に記載の微多孔膜。
- 通気度が200~300sec/100mLの範囲にある、請求項1~3のいずれか1項に記載の微多孔膜。
- ポリプロピレン系重合体が、融点が150~170℃の範囲にあり、メルトマスフローレイト(MFR、JIS K6758(230℃、21.18N)に準拠した条件で測定)が1.0g/10分以下である、任意にエチレン、炭素数4~8のα-オレフィンから選ばれる少なくとも1種を含んでいてもよい、プロピレン主体の重合体である、請求項1~4のいずれか1項に記載の微多孔膜。
- 蓄電デバイスのセパレータに用いられることを特徴とする請求項1~5のいずれか1項に記載の微多孔膜。
- 蓄電デバイスがリチウムイオン電池である、請求項6に記載の微多孔膜。
- 蓄電デバイスがキャパシタである、請求項6に記載の微多孔膜。
- 請求項6に記載の微多孔膜を備える蓄電デバイス。
- 請求項7に記載の微多孔膜を備えるリチウムイオン電池。
- 請求項8に記載の微多孔膜を備えるキャパシタ。
- 以下の工程を含む、請求項1~11のいずれか1項に記載の微多孔膜の製造方法。
(工程1)JIS K6758に準拠して230℃、荷重21.18Nで測定したメルトマスフローレイト(MFR)が1.0g/10分以下であるポリプロピレン系重合体を押出成形して原反フィルムを製膜する工程。
(工程2)工程1で得られた原反フィルムを熱処理する工程。
(工程3)工程2で得られた熱処理後の原反フィルムを、-5~45℃で、長さ方向に1.0~1.1倍に延伸する工程。
(工程4)工程3を終えた延伸フィルムを、ポリプロピレン系重合体の融点よりも5~65℃低い温度で、長さ方向に1.5~4.0倍に延伸する工程。
(工程5)工程4で得られた温延伸後のフィルムを、加熱下、長さが0.7~1.0倍になるように弛緩させる工程。
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US15/541,712 US20180022004A1 (en) | 2015-01-09 | 2016-01-07 | Microporous membrane and production method therefor |
KR1020177021626A KR20170102929A (ko) | 2015-01-09 | 2016-01-07 | 미세 다공막 및 그 제조 방법 |
CN201680005139.2A CN107207754A (zh) | 2015-01-09 | 2016-01-07 | 微多孔膜及其制造方法 |
EP16735062.8A EP3246354A4 (en) | 2015-01-09 | 2016-01-07 | Microporous membrane and production method therefor |
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EP3438170A4 (en) * | 2016-03-31 | 2019-11-13 | JNC Corporation | MICROPOROUS MEMBRANE WITH EXCELLENT LOW TEMPERATURE CHARACTERISTICS AND METHOD FOR PRODUCING THE SAME |
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JP2012038655A (ja) * | 2010-08-10 | 2012-02-23 | Asahi Kasei E-Materials Corp | 微多孔性フィルム及び電池用セパレータ |
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JP2013199545A (ja) * | 2012-03-23 | 2013-10-03 | Asahi Kasei E-Materials Corp | 微多孔性フィルム及び電池用セパレータ |
CN102769115B (zh) * | 2012-08-02 | 2015-05-13 | 常州大学 | 一种由聚丙烯混合物制备的锂离子电池隔膜及其制备方法 |
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- 2015-01-09 JP JP2015002950A patent/JP6550754B2/ja not_active Expired - Fee Related
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2016
- 2016-01-07 EP EP16735062.8A patent/EP3246354A4/en not_active Withdrawn
- 2016-01-07 US US15/541,712 patent/US20180022004A1/en not_active Abandoned
- 2016-01-07 KR KR1020177021626A patent/KR20170102929A/ko unknown
- 2016-01-07 WO PCT/JP2016/050307 patent/WO2016111323A1/ja active Application Filing
- 2016-01-07 CN CN201680005139.2A patent/CN107207754A/zh active Pending
- 2016-01-08 TW TW105100482A patent/TW201637266A/zh unknown
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JP2014223812A (ja) * | 2007-05-11 | 2014-12-04 | 三菱樹脂株式会社 | 積層多孔性フィルム、電池用セパレータおよび電池 |
JP2010265414A (ja) * | 2009-05-15 | 2010-11-25 | Asahi Kasei E-Materials Corp | 微多孔性フィルム及びその製造方法並びに電池用セパレータ |
JP2012038655A (ja) * | 2010-08-10 | 2012-02-23 | Asahi Kasei E-Materials Corp | 微多孔性フィルム及び電池用セパレータ |
JP2016023255A (ja) * | 2014-07-22 | 2016-02-08 | 旭化成イーマテリアルズ株式会社 | 多孔性フィルム捲回物 |
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EP3438170A4 (en) * | 2016-03-31 | 2019-11-13 | JNC Corporation | MICROPOROUS MEMBRANE WITH EXCELLENT LOW TEMPERATURE CHARACTERISTICS AND METHOD FOR PRODUCING THE SAME |
Also Published As
Publication number | Publication date |
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JP6550754B2 (ja) | 2019-07-31 |
TW201637266A (zh) | 2016-10-16 |
KR20170102929A (ko) | 2017-09-12 |
US20180022004A1 (en) | 2018-01-25 |
EP3246354A1 (en) | 2017-11-22 |
EP3246354A4 (en) | 2018-09-19 |
JP2016128530A (ja) | 2016-07-14 |
CN107207754A (zh) | 2017-09-26 |
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