KR101349420B1 - The pore multi-layer film and the method of it - Google Patents
The pore multi-layer film and the method of it Download PDFInfo
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- KR101349420B1 KR101349420B1 KR1020100121456A KR20100121456A KR101349420B1 KR 101349420 B1 KR101349420 B1 KR 101349420B1 KR 1020100121456 A KR1020100121456 A KR 1020100121456A KR 20100121456 A KR20100121456 A KR 20100121456A KR 101349420 B1 KR101349420 B1 KR 101349420B1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/065—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of foam
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
- B32B27/281—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polyimides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
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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
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
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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
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/08—Heat treatment
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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
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2323/00—Polyalkenes
- B32B2323/04—Polyethylene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2323/00—Polyalkenes
- B32B2323/10—Polypropylene
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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
- 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
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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
- C08J2479/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2461/00 - C08J2477/00
- C08J2479/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2479/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
Abstract
본 발명은 필터, 분리막, 전지용 세퍼레이터, 인쇄 기판 등에 사용할 수 있는 다공성 다층필름 및 이의 제조방법에 관한 것으로서, 본 발명에 의한 다공성 다층필름은 다공성 폴리에틸렌 필름 또는 다공성 폴리프로필렌 필름과 상기 다공성 폴리에틸렌 필름 또는 다공성 폴리프로필렌 필름의 일면 또는 양면에 형성된 다공성 폴리아미드이미드층을 포함하고, 본 발명에 의한 다공성 다층필름의 제조방법은 본 발명에 의한 다공성 다층 필름의 제조방법은 미반응 무수물 말단 또는 미반응 카르복실 말단을 포함하는 폴리아미드이미드 바니쉬 및 이소시아네이트계 화합물을 포함하는 혼합용액을 제조하는 공정과, 다공성 폴리에틸렌 필름 또는 다공성 폴리프로필렌 필름의 일면 또는 양면에 상기 혼합용액을 코팅하는 공정 및 상기 필름에 코팅된 혼합용액을 건조 및 열처리하는 공정을 포함한다. The present invention relates to a porous multilayer film that can be used for filters, separators, battery separators, printed boards, and the like, and to a method for manufacturing the same. The porous multilayer film according to the present invention includes a porous polyethylene film or a porous polypropylene film and the porous polyethylene film or a porous Including a porous polyamideimide layer formed on one or both sides of the polypropylene film, the method for producing a porous multilayer film according to the present invention is a method for producing a porous multilayer film according to the present invention is an unreacted anhydride terminal or an unreacted carboxyl terminal Process for preparing a mixed solution comprising a polyamideimide varnish and an isocyanate compound comprising a; and coating the mixed solution on one side or both sides of a porous polyethylene film or a porous polypropylene film and a mixed solution coated on the film Drying and heat treatment.
Description
본 발명은 필터, 분리막, 전지용 세퍼레이터, 인쇄 기판 등에 사용할 수 있는 다공성 다층필름 및 이의 제조방법에 관한 것이다.The present invention relates to a porous multilayer film that can be used for filters, separators, battery separators, printed boards, and the like, and to a method of manufacturing the same.
최근에는 고용량, 고전압, 고에너지 밀도의 달성이 가능한 유기 전해액 2차전지가 많이 개발되고 있고, 이러한 유기 전해액 2차 전지에는 양극과 음극의 두 전극 사이에 이온의 유통이 가능한 다공성 필름이 세퍼레이터로 설치된다.Recently, many organic electrolyte secondary batteries that can achieve high capacity, high voltage, and high energy density have been developed. In such organic electrolyte secondary batteries, a porous film capable of distributing ions between two electrodes of a positive electrode and a negative electrode is installed as a separator. .
상기 세퍼레이터로 이용되는 다공성 필름으로는 주로 폴리에틸렌 필름 또는 폴리프로필렌 필름 등이 사용되나, 이들은 내열성 및 강도가 약하여 그 두께를 두껍게 해야하는 등의 단점이 있었다.As the porous film used as the separator, a polyethylene film or a polypropylene film is mainly used. However, these films have disadvantages such as high heat resistance and low strength to increase their thickness.
이러한 단점을 극복하기 위하여 한국특허공개공보 제2007-0103453호에서는 제막원액 중에 중합체 빈용매 또는 수용성 중합체를 포함하는 방향족 폴리아미드 및 유기용매를 포함하는 제막원액을 유연 도포하여 필름을 얻고, 이를 습식욕에 도입하여 중합체 빈용매 또는 수용성 중합체가 습식욕에서 용출되도록 하여 다공성 폴리아미드 필름을 제조하는 방법을 개시하여, 방향족 폴리아미드 다공성 필름을 제공함으로써, 내열성 및 강도가 우수한 세퍼레이터를 제공하고 있다.In order to overcome these disadvantages, Korean Patent Publication No. 2007-0103453 obtains a film by flexibly applying a film forming solution containing an aromatic polyamide and an organic solvent containing a polymer poor solvent or a water-soluble polymer in a film forming solution, and a wet bath. A method of preparing a porous polyamide film by introducing into a polymer poor solvent or a water-soluble polymer in a wet bath is disclosed to provide an aromatic polyamide porous film, thereby providing a separator having excellent heat resistance and strength.
그러나, 이러한 공정을 이용할 경우, 제막공정 이후에 습식욕조에서의 용출 공정을 추가로 도입함으로써 공정이 복잡해지고, 생산원가가 상승되는 원인이 된다.However, when such a step is used, the step is further complicated by introducing an elution step in the wet bath after the film forming step, which causes the production cost to increase.
본 발명은 기존에 이용되고 있던 다공성 폴리에틸렌 필름 또는 폴리프로필렌 필름의 내열성 및 강도를 보강한 다공성 다층필름 및 이의 제조방법을 제공하려는 것이다. The present invention is to provide a porous multilayer film and a method for manufacturing the same reinforcing the heat resistance and strength of the porous polyethylene film or polypropylene film used in the prior art.
본 발명에 의한 다공성 다층필름은 다공성 폴리에틸렌 필름 또는 다공성 폴리프로필렌 필름과 상기 다공성 폴리에틸렌 필름 또는 다공성 폴리프로필렌 필름의 일면 또는 양면에 형성된 다공성 폴리아미드이미드층을 포함하는 것을 특징으로 하고, 상기 폴리아미드이미드층은 TMA로부터 유래된 단위구조를 포함하거나, TMA로부터 유래된 단위구조 및 PMDA로부터 유래된 단위구조를 포함할 수 있다. The porous multilayer film according to the present invention is characterized in that it comprises a porous polyethylene film or porous polypropylene film and a porous polyamideimide layer formed on one or both sides of the porous polyethylene film or porous polypropylene film, wherein the polyamideimide layer May include a unit structure derived from TMA, or may include a unit structure derived from TMA and a unit structure derived from PMDA.
본 발명에 의한 다공성 다층 필름의 제조방법은 미반응 무수물 말단 또는 미반응 카르복실 말단을 포함하는 폴리아미드이미드 바니쉬 및 이소시아네이트계 화합물을 포함하는 혼합용액을 제조하는 공정과, 다공성 폴리에틸렌 필름 또는 다공성 폴리프로필렌 필름의 일면 또는 양면에 상기 혼합용액을 코팅하는 공정 및 상기 필름에 코팅된 혼합용액을 건조 및 열처리하는 공정을 포함하는 것을 특징으로 한다. Method for producing a porous multilayer film according to the present invention is a process for preparing a mixed solution containing a polyamideimide varnish and an isocyanate compound containing an unreacted anhydride end or an unreacted carboxyl end, and a porous polyethylene film or a porous polypropylene It characterized in that it comprises a step of coating the mixed solution on one side or both sides of the film and a step of drying and heat-treating the mixed solution coated on the film.
이때, 상기 혼합용액을 제조하는 공정에서 상기 미반응 무수물 말단 또는 미반응 카르복실 말단을 포함하는 폴리아미드이미드 바니쉬는 저분자화합물로 TMA(Trimellitic Anhydride)로부터 유래된 단위구조를 포함하거나, TMA로부터 유래된 단위구조 및 PMDA(1,2,4,5-benzenetetracarboxylic dianhydride)로부터 유래된 단위구조를 포함할 수 있다.In this case, the polyamideimide varnish containing the unreacted anhydride terminal or the unreacted carboxyl terminal in the process of preparing the mixed solution includes a unit structure derived from trimellitic anhydride (TMA) as a low molecular weight compound, or derived from TMA. Unit structures and unit structures derived from PMDA (1,2,4,5-benzenetetracarboxylic dianhydride).
또, 상기 혼합용액을 제조하는 공정에서 상기 이소시아네이트계 화합물은 4,4-MDI(4,4-methylen dipnenyl isocyanate) 및 TDI(Toluene diisocyanate)로 이루어진 군에서 선택된 1종 이상일 수 있다. The isocyanate compound may be at least one selected from the group consisting of 4,4-MDI (4,4-methylen dipnenyl isocyanate) and TDI (toluene diisocyanate) in the process of preparing the mixed solution.
또, 상기 혼합용액을 제조하는 공정에서 상기 혼합용액은 발포제를 더 포함할 수 있으며, 발포제는 화학 발포제, 열분해 발포제 등 다양한 발포제를 사용할 수 있다.In addition, in the process of preparing the mixed solution, the mixed solution may further include a blowing agent, and the blowing agent may use various blowing agents such as chemical blowing agents and pyrolytic blowing agents.
본 발명은 기존에 이용되고 있던 다공성 폴리에틸렌 필름 또는 폴리프로필렌 필름의 내열성 및 강도를 보강한 다공성 다층 필름의 제조방법을 제공하였다.The present invention provides a method for producing a porous multilayer film that reinforces the heat resistance and strength of the porous polyethylene film or polypropylene film.
본 발명에 의한 다공성 다층필름은 다공성 폴리에틸렌 필름 또는 다공성 폴리프로필렌 필름과 상기 다공성 폴리에틸렌 필름 또는 다공성 폴리프로필렌 필름의 일면 또는 양면에 형성된 다공성 폴리아미드이미드층을 포함하는 것을 특징으로 하고, 상기 폴리아미드이미드층은 TMA로부터 유래된 단위구조를 포함하거나, TMA로부터 유래된 단위구조 및 PMDA로부터 유래된 단위구조를 포함할 수 있다. 이에 따라, 종래에 일반적으로 이용되는 다공성 폴리에틸렌 필름 또는 폴리프로필렌 필름의 표면에 내열성 및 강도가 우수한 폴리아미드이미드층이 형성됨으로서 필름의 내열성 및 강도 등을 향상시킬 수 있는 것이다. The porous multilayer film according to the present invention is characterized in that it comprises a porous polyethylene film or porous polypropylene film and a porous polyamideimide layer formed on one or both sides of the porous polyethylene film or porous polypropylene film, wherein the polyamideimide layer May include a unit structure derived from TMA, or may include a unit structure derived from TMA and a unit structure derived from PMDA. Accordingly, the polyamideimide layer having excellent heat resistance and strength is formed on the surface of the porous polyethylene film or the polypropylene film generally used in the related art, thereby improving heat resistance and strength of the film.
본 발명에 의한 다공성 다층 필름의 제조방법은 미반응 무수물 말단 또는 미반응 카르복실 말단을 포함하는 폴리아미드이미드 바니쉬 및 이소시아네이트계 화합물을 포함하는 혼합용액을 제조하는 공정과, 다공성 폴리에틸렌 필름 또는 다공성 폴리프로필렌 필름의 일면 또는 양면에 상기 혼합용액을 코팅하는 공정 및 상기 필름에 코팅된 혼합용액을 건조 및 열처리하는 공정을 포함하는 것을 특징으로 한다. 이와 같이 미반응 무수물 말단 또는 미반응 카르복실 말단을 포함하는 폴리아미드이미드 바니쉬와 이소시아네이트계 화합물을 포함하는 혼합용액을 필름의 일면 또는 양면에 코팅한 상태에서 이를 건조 및 열처리를 할 때, 폴리아미드이미드 바니쉬에 존재하는 미반응 무수물 말단 또는 미반응 카르복실 말단과 이소시아네이트계 화합물의 이소시아네이트기가 반응경화되면서 이산화탄소가 발생하고, 이산화탄소의 발생에 의한 기포에 의하여 폴리아미드이미드층을 다공성으로 형성할 수 있는 것이다. Method for producing a porous multilayer film according to the present invention is a process for preparing a mixed solution containing a polyamideimide varnish and an isocyanate compound containing an unreacted anhydride end or an unreacted carboxyl end, and a porous polyethylene film or a porous polypropylene It characterized in that it comprises a step of coating the mixed solution on one side or both sides of the film and a step of drying and heat treating the mixed solution coated on the film. Thus, when the mixed solution containing the polyamideimide varnish containing the unreacted anhydride terminal or the unreacted carboxyl terminal and the isocyanate compound on one or both sides of the film is dried and heat treated, the polyamideimide Carbon dioxide is generated as the unreacted anhydride terminal or unreacted carboxyl terminal and the isocyanate group of the isocyanate compound present in the varnish react and harden, and the polyamideimide layer can be formed porous by bubbles caused by the generation of carbon dioxide.
이때, 상기 혼합용액을 제조하는 공정에서 상기 미반응 무수물 말단 또는 미반응 카르복실 말단을 포함하는 폴리아미드이미드 바니쉬는 저분자화합물로 TMA(Trimellitic Anhydride)로부터 유래된 단위구조를 포함하거나, TMA로부터 유래된 단위구조 및 PMDA(1,2,4,5-benzenetetracarboxylic dianhydride)로부터 유래된 단위구조를 포함할 수 있다.In this case, the polyamideimide varnish containing the unreacted anhydride terminal or the unreacted carboxyl terminal in the process of preparing the mixed solution includes a unit structure derived from trimellitic anhydride (TMA) as a low molecular weight compound, or derived from TMA. Unit structures and unit structures derived from PMDA (1,2,4,5-benzenetetracarboxylic dianhydride).
또, 상기 혼합용액을 제조하는 공정에서 상기 이소시아네이트계 화합물은 4,4-MDI(4,4-methylen dipnenyl isocyanate) 및 TDI(Toluene diisocyanate)로 이루어진 군에서 선택된 1종 이상일 수 있다. The isocyanate compound may be at least one selected from the group consisting of 4,4-MDI (4,4-methylen dipnenyl isocyanate) and TDI (toluene diisocyanate) in the process of preparing the mixed solution.
또한, 폴리아미드이미드 바니쉬에 존재하는 미반응 무수물 말단 또는 미반응 카르복실 말단과 이소시아네이트계 화합물의 이소시아네이트기가 반응에 의해 발생되는 기포보다 더 많은 기포를 생성시켜 폴리아미드이미드층의 다공성을 더 확보하기 위하여서는 상기 혼합용액을 제조하는 공정에서 상기 혼합용액에 발포제를 더 포함시킬 수 있다. 이 때, 발포제는 화학 발포제, 열분해 발포제 등 다양한 발포제를 사용할 수 있으며, 발포제의 첨가로 기공의 분포 및 크기, 형상 등을 조절할 수 있으며 이를 통해 소재의 밀도, 강도, 경도 등도 조절 할 수 있다. In addition, in order to ensure more porosity of the polyamideimide layer by generating more bubbles than the bubbles generated by the reaction of the unreacted anhydride terminal or the unreacted carboxyl terminal and the isocyanate group of the isocyanate compound present in the polyamideimide varnish May further include a blowing agent in the mixed solution in the process of preparing the mixed solution. At this time, the blowing agent may use a variety of blowing agents, such as chemical blowing agents, pyrolytic blowing agents, and can control the distribution, size, shape, etc. of the pores by the addition of the blowing agent, it can also control the density, strength, hardness, etc. of the material.
Claims (8)
상기 다공성 폴리에틸렌 필름 또는 다공성 폴리프로필렌 필름의 일면 또는 양면에 형성된 다공성 폴리아미드이미드층을 포함하며,
상기 폴리아미드이미드층은 TMA(Trimellitic Anhydride)로부터 유래된 단위구조 및 PMDA(1,2,4,5-benzenetetracarboxylic dianhydride)로부터 유래된 단위구조를 포함하는 것을 특징으로 하는 다공성 다층필름.
Porous polyethylene film or porous polypropylene film;
It comprises a porous polyamideimide layer formed on one side or both sides of the porous polyethylene film or porous polypropylene film,
The polyamideimide layer has a unit structure derived from trimellitic anhydride (TMA) and a unit structure derived from PMDA (1,2,4,5-benzenetetracarboxylic dianhydride).
다공성 폴리에틸렌 필름 또는 다공성 폴리프로필렌 필름의 일면 또는 양면에 상기 혼합용액을 코팅하는 공정; 및
상기 필름에 코팅된 혼합용액을 건조 및 열처리하는 공정을 포함하되,
상기 혼합용액을 제조하는 공정에서, 상기 미반응 무수물 말단 또는 미반응 카르복실 말단을 포함하는 폴리아미드이미드 바니쉬는 TMA(Trimellitic Anhydride)로부터 유래된 단위구조 및 PMDA(1,2,4,5-benzenetetracarboxylic dianhydride)로부터 유래된 단위구조를 포함하는 것을 특징으로 하는 다공성 다층필름의 제조방법.
Preparing a mixed solution containing a polyamideimide varnish and an isocyanate compound having an unreacted anhydride terminal or an unreacted carboxyl terminal;
Coating the mixed solution on one or both surfaces of the porous polyethylene film or the porous polypropylene film; And
Including the process of drying and heat-treating the mixed solution coated on the film,
In the process of preparing the mixed solution, the polyamideimide varnish containing the unreacted anhydride terminal or the unreacted carboxyl terminal has a unit structure derived from trimellitic anhydride (TMA) and PMDA (1,2,4,5-benzenetetracarboxylic). Method of producing a porous multilayer film comprising a unit structure derived from dianhydride).
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