JP5919185B2 - ポリエーテルイミド多孔質体及びその製造方法 - Google Patents
ポリエーテルイミド多孔質体及びその製造方法 Download PDFInfo
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- JP5919185B2 JP5919185B2 JP2012274842A JP2012274842A JP5919185B2 JP 5919185 B2 JP5919185 B2 JP 5919185B2 JP 2012274842 A JP2012274842 A JP 2012274842A JP 2012274842 A JP2012274842 A JP 2012274842A JP 5919185 B2 JP5919185 B2 JP 5919185B2
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- Prior art keywords
- polyetherimide
- porous body
- phase separation
- separation structure
- breakdown voltage
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D179/00—Coating compositions based on 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 C09D161/00 - C09D177/00
- C09D179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C09D179/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/303—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups H01B3/38 or H01B3/302
- H01B3/306—Polyimides or polyesterimides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/42—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes polyesters; polyethers; polyacetals
- H01B3/427—Polyethers
-
- 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
- C08J2201/02—Foams characterised by the foaming process characterised by mechanical pre- or post-treatments
- C08J2201/026—Crosslinking before of after foaming
-
- 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
- C08J2201/046—Elimination of a polymeric phase
- C08J2201/0464—Elimination of a polymeric phase using water or inorganic fluids
-
- 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
- C08J2205/00—Foams characterised by their properties
- C08J2205/04—Foams characterised by their properties characterised by the foam pores
- C08J2205/044—Micropores, i.e. average diameter being between 0,1 micrometer and 0,1 millimeter
-
- 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
- C08J2207/00—Foams characterised by their intended use
- C08J2207/06—Electrical wire insulation
-
- 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
- C08J2379/00—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 C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Insulation, Fastening Of Motor, Generator Windings (AREA)
- Laminated Bodies (AREA)
- Organic Insulating Materials (AREA)
- Insulating Bodies (AREA)
- Power Engineering (AREA)
Description
割れ頻度(%)=(折り曲げ部の総割れ長さ/折り曲げ部の長さ)×100
割れ頻度(%)=(折り曲げ部の総割れ長さ/折り曲げ部の長さ)×100
(ゲル分率)
多孔質体(0.5g)を樹脂フィルム(日東電工株式会社製、TEMISH NTF1133)で包んで容器内に入れ、そこに溶媒であるN−メチル−2−ピロリドンを約50ml添加し、スターラー撹拌を24時間行った。その後、樹脂フィルムの溶媒を拭き取り、240℃で3時間加熱乾燥させた後にゲル体の重量を測定した。ゲル分率は、下記式により算出した。
ゲル分率(%)=(ゲル体の重量 /多孔質体の重量)×100
多孔質体を液体窒素で冷却し、刃物を用いてシート面に対して垂直に切断して評価サンプルを作製した。サンプルの切断面にPd−Pt蒸着処理を施し、該切断面を走査型電子顕微鏡(SEM)(日本電子社製「JSM−6510LV」)で観察した。その画像を画像処理ソフト(ナノシステム社製「NanoHunter NS2K−Lt」)で二値化処理し、気泡部と樹脂部とに分離して気泡の最大水平弦長を測定した。気泡径の大きいほうから40個の気泡について平均値をとり、その値を平均気泡径とした。
電子比重計(アルファーミラージュ社製、MD−300S)を用いて多孔質体の比重と無孔体の比重を測定し、下記式により体積空孔率を計算した。
体積空孔率(%)={1−(多孔質体の比重)/(無孔体の比重)}×100
JlS C2110の規格に準拠した方法により、多孔質体の絶縁破壊電圧を測定した。昇圧速度は1kV/secとした。
作製した多孔質体から25mm(TD方向)×50mmの大きさで切り出したサンプルを二つ折りにし(25mm×25mm)、折り曲げ部から25mm×10mmの面積を油圧プレス機を用いて圧力2MPaで1秒間プレスした。その後、光学顕微鏡(Nikon社製、ELIPSE ME600)を用いて倍率100〜500倍でサンプルの折り曲げ部の総割れ長さを測定した。割れ頻度(%)は下記式より算出した。
割れ頻度(%)=(折り曲げ部の総割れ長さ/折り曲げ部の長さ)×100
作製した多孔質体から25mm(TD方向)×50mmの大きさで切り出したサンプルの絶縁破壊電圧を前記と同様の方法で測定した。また、同じ大きさのサンプルを前記と同様の方法で折り曲げ、折り曲げ部の絶縁破壊電圧を前記と同様の方法で測定した。折り曲げ前後の絶縁破壊電圧保持率は下記式より算出した。
絶縁破壊電圧保持率(%)=(折り曲げ部の絶縁破壊電圧/折り曲げ前のサンプルの絶縁破壊電圧)×100
空洞共振器摂動法により、周波数1GHzにおける複素誘電率を測定し、その実数部を比誘電率とした。測定機器は、円筒空洞共振機(アジレント・テクノロジー社製「ネットワークアナライザ N5230C」、関東電子応用開発社製「空洞共振器1GHz」)を用い、短冊状のサンプル(サンプルサイズ2mm×70mm長さ)を用いて測定した。
1000m1の4つ口フラスコに、N−メチル−2−ピロリドン(NMP)730gを加えて70℃に加熱した。そこにポリエーテルイミド(PEI)樹脂(SABIC Innovative Plastics社製、UItem1000−1000)189gとPEI樹脂(SABIC Innovative Plastics社製、UItemXH−6050)81gとを加え、5時間撹拌してPEI樹脂溶液(I)を得た。
PEI樹脂のイミド基1モル当量に対してアミノ基0.04モル当量になる量の1,10−デカンジアミンを添加する代わりに、PEI樹脂のイミド基1モル当量に対してアミノ基0.02モル当量になる量の両末端アミン変性ジメチルシロキサン(信越シリコーン社製、KF−8010)を添加した以外は実施例1と同様の方法でPEI多孔質体を作製した。
PEI樹脂のイミド基1モル当量に対してアミノ基0.04モル当量になる量の1,10−デカンジアミンを添加する代わりに、PEI樹脂のイミド基1モル当量に対してアミノ基0.02モル当量になる量の側鎖の一部がフェニル基に置換された両末端アミン変性ジメチルシロキサン(信越シリコーン社製、X−22−9409)を添加した以外は実施例1と同様の方法でPEI多孔質体を作製した。
1,10−デカンジアミンを添加しなかった以外は実施例1と同様の方法でPEI多孔質体を作製した。
Claims (6)
- モーター用の絶縁シートとして用いられ、ポリエーテルイミド架橋体を含み、ゲル分率が10%以上、平均気泡径が8μm以下、体積空孔率が30%以上、かつ絶縁破壊電圧が30kV/mm以上であるポリエーテルイミド多孔質体。
- 前記ポリエーテルイミド架橋体は、ポリエーテルイミドを、アミノ基を2つ以上有するポリアミンで架橋したものである請求項1記載のポリエーテルイミド多孔質体。
- 下記式にて表される割れ頻度が20%以下、かつ折り曲げ前後の絶縁破壊電圧保持率が60%以上である請求項1又は2記載のポリエーテルイミド多孔質体。
割れ頻度(%)=(折り曲げ部の総割れ長さ/折り曲げ部の長さ)×100 - 請求項1〜3のいずれかに記載のポリエーテルイミド多孔質体の少なくとも片面にシート材を有するモーター用絶縁積層シート。
- ポリエーテルイミド、ポリエーテルイミドと相分離する相分離化剤、及びアミノ基を2つ以上有するポリアミンを含有するポリマー溶液を基板上に塗布し、乾燥させてミクロ相分離構造を有する相分離構造体を作製する工程、相分離構造体から相分離化剤を除去して多孔質体を作製する工程を含む請求項1〜3のいずれかに記載のポリエーテルイミド多孔質体の製造方法。
- ポリエーテルイミド、ポリエーテルイミドと相分離する相分離化剤、及びアミノ基を2つ以上有するポリアミンを含有するポリマー溶液を基板上に塗布し、乾燥させてミクロ相分離構造を有する相分離構造体を作製する工程、相分離構造体から相分離化剤を除去して多孔質体を作製する工程を含み、ポリエーテルイミド架橋体を含み、ゲル分率が10%以上、平均気泡径が8μm以下、体積空孔率が30%以上、かつ絶縁破壊電圧が30kV/mm以上である、ポリエーテルイミド多孔質体の製造方法。
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2012274842A JP5919185B2 (ja) | 2012-12-17 | 2012-12-17 | ポリエーテルイミド多孔質体及びその製造方法 |
EP13863784.8A EP2933287A4 (en) | 2012-12-17 | 2013-12-09 | POROUS POLYETHERIMIDE BODY AND PROCESS FOR PRODUCING THE SAME |
CN201380065936.6A CN104870538A (zh) | 2012-12-17 | 2013-12-09 | 聚醚酰亚胺多孔体及其制造方法 |
PCT/JP2013/082984 WO2014097920A1 (ja) | 2012-12-17 | 2013-12-09 | ポリエーテルイミド多孔質体及びその製造方法 |
KR1020157019231A KR20150095910A (ko) | 2012-12-17 | 2013-12-09 | 폴리에테르이미드 다공질체 및 그 제조 방법 |
US14/652,627 US20150329675A1 (en) | 2012-12-17 | 2013-12-09 | Polyetherimide porous body and method for producing same |
Applications Claiming Priority (1)
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JP2012274842A JP5919185B2 (ja) | 2012-12-17 | 2012-12-17 | ポリエーテルイミド多孔質体及びその製造方法 |
Publications (2)
Publication Number | Publication Date |
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JP2014118489A JP2014118489A (ja) | 2014-06-30 |
JP5919185B2 true JP5919185B2 (ja) | 2016-05-18 |
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JP2012274842A Expired - Fee Related JP5919185B2 (ja) | 2012-12-17 | 2012-12-17 | ポリエーテルイミド多孔質体及びその製造方法 |
Country Status (6)
Country | Link |
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US (1) | US20150329675A1 (ja) |
EP (1) | EP2933287A4 (ja) |
JP (1) | JP5919185B2 (ja) |
KR (1) | KR20150095910A (ja) |
CN (1) | CN104870538A (ja) |
WO (1) | WO2014097920A1 (ja) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
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JP6255227B2 (ja) * | 2013-12-04 | 2017-12-27 | 日東シンコー株式会社 | モーター用絶縁シート |
KR101714201B1 (ko) * | 2015-08-28 | 2017-03-08 | 현대자동차주식회사 | 초경량 전도성 플라스틱 및 그 제조방법 |
JP7058704B1 (ja) | 2020-11-25 | 2022-04-22 | 三菱電機株式会社 | 絶縁シート及びその製造方法、並びに回転電機 |
Family Cites Families (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB8628938D0 (en) * | 1986-12-03 | 1987-01-07 | Domnick Hunter Filters Ltd | Microporous polyetherimide membranes |
JP2965278B2 (ja) * | 1991-12-24 | 1999-10-18 | 松下電工株式会社 | 熱硬化型ポリイミド樹脂組成物と熱硬化品およびその製造方法 |
US5670102A (en) | 1993-02-11 | 1997-09-23 | Minnesota Mining And Manufacturing Company | Method of making thermoplastic foamed articles using supercritical fluid |
JP3115215B2 (ja) | 1995-10-05 | 2000-12-04 | 松下電器産業株式会社 | 低誘電率プラスチック絶縁フィルムおよびその製造方法 |
JP2922856B2 (ja) | 1996-08-06 | 1999-07-26 | 大塚化学株式会社 | シンジオタクチックポリスチレン発泡体、その製造方法及び該発泡体を用いた電気回路用基板 |
KR100380425B1 (ko) * | 1998-09-17 | 2003-04-18 | 마쯔시다덴기산교 가부시키가이샤 | 다공질체 및 그 제조방법 |
JP4159199B2 (ja) | 1999-09-16 | 2008-10-01 | 日東電工株式会社 | 多孔質体及び多孔質体の製造方法 |
US20060249018A1 (en) * | 2005-05-04 | 2006-11-09 | Hua Wang | Nucleophilic modifier functionalized and/or crosslinked solvent-resistant polymide and copolymer membranes |
US20090163610A1 (en) * | 2007-12-20 | 2009-06-25 | Lanning Vincent L | Continuous process for making polyetherimide foam materials and articles made therefrom |
WO2010111755A2 (en) * | 2009-04-01 | 2010-10-07 | Katholieke Universiteit Leuven - K.U.Leuven R & D | Improved method for making cross-linked polyimide membranes |
JP2012182116A (ja) * | 2011-02-03 | 2012-09-20 | Nitto Denko Corp | モーター用電気絶縁性樹脂シート及びその製造方法 |
JP5458137B2 (ja) * | 2012-03-29 | 2014-04-02 | 日東電工株式会社 | 電気絶縁性樹脂シート |
-
2012
- 2012-12-17 JP JP2012274842A patent/JP5919185B2/ja not_active Expired - Fee Related
-
2013
- 2013-12-09 CN CN201380065936.6A patent/CN104870538A/zh active Pending
- 2013-12-09 KR KR1020157019231A patent/KR20150095910A/ko not_active Application Discontinuation
- 2013-12-09 WO PCT/JP2013/082984 patent/WO2014097920A1/ja active Application Filing
- 2013-12-09 US US14/652,627 patent/US20150329675A1/en not_active Abandoned
- 2013-12-09 EP EP13863784.8A patent/EP2933287A4/en not_active Withdrawn
Also Published As
Publication number | Publication date |
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CN104870538A (zh) | 2015-08-26 |
JP2014118489A (ja) | 2014-06-30 |
WO2014097920A1 (ja) | 2014-06-26 |
EP2933287A1 (en) | 2015-10-21 |
EP2933287A4 (en) | 2016-08-10 |
US20150329675A1 (en) | 2015-11-19 |
KR20150095910A (ko) | 2015-08-21 |
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