JP4584886B2 - 電解質膜の製造方法および電解質膜 - Google Patents
電解質膜の製造方法および電解質膜 Download PDFInfo
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- H01M8/103—Polymeric electrolyte materials characterised by the chemical structure of the main chain of the ion-conducting polymer having nitrogen, e.g. sulfonated polybenzimidazoles [S-PBI], polybenzimidazoles with phosphoric acid, sulfonated polyamides [S-PA] or sulfonated polyphosphazenes [S-PPh]
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- H01M8/10—Fuel cells with solid electrolytes
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- H01M8/1018—Polymeric electrolyte materials
- H01M8/1069—Polymeric electrolyte materials characterised by the manufacturing processes
- H01M8/1072—Polymeric electrolyte materials characterised by the manufacturing processes by chemical reactions, e.g. insitu polymerisation or insitu crosslinking
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- 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
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- H01M4/90—Selection of catalytic material
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Description
フェノール1mol、p−ホルムアルデヒド2.2mol及びアニリン1.1molを混合し、これを110℃で1時間攪拌して、粗生性物を得た。
ターシャリブチルフェノル1mol、p−ホルムアルデヒド2.2mol及びアニリン1.1molを混合し、これを110℃で1時間、溶媒なしに攪拌して、粗生性物を得た。
ターシャリブチルフェノル1mol、p−ホルムアルデヒド2.2mol及び3−アミノプロピルイミダゾール1.1molを混合し、これを、110℃で1時間、溶媒なしに溶融状態で攪拌して、粗生性物を得た。
ビスフェノールA(BP)1mol、p−ホルムアルデヒド4.4mol及びアニリン2.2molを混合し、これを、110℃で1時間攪拌して、粗生性物を得た。
4,4’−ヘキサフルオロイソプロピリデンジフェノル(4,4’−HFIDPH)1mol、p−ホルムアルデヒド4.4mol及びアニリン2.2molを混合し、これを、110℃で1時間、溶媒なしに攪拌して、粗生性物を得た。
4,4’−ジヒドロキシベンゾフェノン1mol、p−ホルムアルデヒド2.2mol及び3−アミノプロピルイミダゾール1.1molを混合し、これを、110℃で1時間、溶媒なしに溶融状態で攪拌して、粗生性物を得た。
ビスフェノール(Bisphenol S:BS)1mol、p−ホルムアルデヒド4.4mol及び1−(3−アミノプロピル)イミダゾール2.2molを混合し、これを、110℃で1時間、溶媒なしに溶融状態で攪拌して、粗生性物を得た。
1,1,1−トリス(4−ヒドロキシフェニル)エタン(THPE)1mol、p−ホルムアルデヒド6.6mol及びアリルアミン3.3molを混合し、これを、110℃で1時間、溶媒なしに溶融状態で攪拌して、粗生性物を得た。
ポリベンズイミダゾール100質量部を、ジメチルアセトアミド900質量部に溶解して、ポリベンズイミダゾール溶液を製造した。
ポリベンズイミダゾール100質量部を、ジメチルアセトアミド900質量部に溶解して、ポリベンズイミダゾール溶液を製造した。
CELAZOLE(商品名)PBI(Celanese Corp.製)を使用してPBI膜を作り、85質量%リン酸に常温で4時間含浸させた。
CELAZOLE(商品名)PBI(Celanese Corp.製)を使用してPBI膜を作り、85質量%リン酸に常温で4時間含浸させた。
Claims (11)
- (a)架橋性化合物を溶媒に溶解して、10〜20質量%の架橋性化合物溶液を得る工程と、
(b)前記架橋性化合物溶液とベンゾオキサジン系モノマーとを混合して、ベンゾオキサジン系モノマーと架橋性化合物との混合物を得る工程と、
(c)前記混合物を利用して、膜を形成する工程と、
(d)前記膜を、80〜250℃の温度に加熱して硬化する工程と、
(e)前記硬化結果物を酸に含浸して、電解質膜を形成する工程と、
を含み、
前記電解質膜は、ベンゾオキサジン系モノマーと架橋性化合物との重合結果物であるポリベンゾオキサジン系化合物の架橋体からなり、
前記ベンゾオキサジン系モノマーは、下記化学式1または化学式2で示される化合物であり、
前記架橋性化合物は、ポリベンズイミダゾール、ポリベンズチアゾール、ポリベンゾオキサゾールからなる群より選択された一つ以上であることを特徴とする、電解質膜の製造方法。
ここで、前記化学式1において、R1は、水素、または、置換もしくは非置換のC1−C20のアルキル基であり、
前記化学式2において、前記R 3 は、−C(CH 3 ) 2 −、−C(CF 3 ) 2 −、−C(=O)−、−SO 2 −、−CH 2 −、−C(CCl 3 )−、−CH(CH 3 )−、−CH(CF 3 )−、または、以下の構造式1で示される連結基であり、
- 前記(c)工程で膜を形成する工程は、前記(b)工程から得た前記ベンゾオキサジン系モノマーと架橋性化合物との混合物を、テープキャスティングして行われることを特徴とする、請求項1に記載の電解質膜の製造方法。
- 前記(c)工程で膜を形成する工程は、前記(b)工程から得た前記ベンゾオキサジン系モノマーと架橋性化合物との混合物を、支持体上にキャスティングして行われることを特徴とする、請求項1に記載の電解質膜の製造方法。
- 前記(d)工程である硬化工程以後に、前記支持体から前記硬化結果物を剥離して、前記支持体を除去する工程をさらに行うことを特徴とする、請求項3に記載の電解質膜の製造方法。
- 前記支持体を除去する工程は、前記硬化結果物を60〜80℃の蒸溜水に浸漬することにより行われることを特徴とする、請求項4に記載の電解質膜の製造方法。
- 前記化学式1において、前記R1は、ターシャリブチル基であることを特徴とする、請求項1に記載の電解質膜の製造方法。
- 前記化学式1の化合物は、下記化学式3〜化学式12で示される化合物より選択された一つ以上であることを特徴とする、請求項2に記載の電解質膜の製造方法。
- 前記化学式2の化合物は、下記化学式13〜17で示される化合物から選択された一つ以上であることを特徴とする、請求項1に記載の電解質膜の製造方法。
- 前記架橋性化合物の含有量は、前記ベンゾオキサジン系モノマー100質量部を基準として、10〜90質量部であることを特徴とする、請求項1に記載の電解質膜の製造方法。
- 前記架橋性化合物の含有量は、前記ベンゾオキサジン系モノマー100質量部を基準として、30〜60質量部であることを特徴とする、請求項9に記載の電解質膜の製造方法。
- 請求項1〜請求項10のいずれか1項に記載の製造方法で製造された、ベンゾオキサジン系モノマーと架橋性化合物との重合結果物であるポリベンゾオキサジン系化合物の架橋体を含み、
リン酸含浸量は、電解質膜の総質量100質量部に対して、300〜600質量部であり、
降伏ひずみが0.5%以下であり、
降伏応力が0.3MPa以下であることを特徴とする、電解質膜。
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KR1020060011831A KR100754374B1 (ko) | 2006-02-07 | 2006-02-07 | 폴리벤조옥사진계 화합물을 이용한 전해질막 및 그제조방법 |
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JP (1) | JP4584886B2 (ja) |
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