JP2021521322A - 表面イオン交換高分子電解質が除去された細孔充填イオン交換高分子電解質複合膜及びその製造方法 - Google Patents
表面イオン交換高分子電解質が除去された細孔充填イオン交換高分子電解質複合膜及びその製造方法 Download PDFInfo
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Abstract
Description
陽イオン基を有する4級アンモニウム塩の電解質モノマーまたは、陰イオン基を有するスルホン酸含有電解質モノマー、3級アミン作用基を有するアクリルアミド系架橋剤、開始剤及び溶媒を含むイオン交換前駆体溶液700を製造する段階と、前記イオン交換前駆体溶液700に多孔性高分子支持体を含浸させる段階と、上部フィルム、前記多孔性高分子支持体及び下部フィルムを圧着ロールに投入させて前記高分子支持体の上部及び下部にそれぞれ前記上部フィルム及び下部フィルムを圧着させる段階と、前記上部フィルム及び下部フィルムが圧着された多孔性高分子支持体に紫外線を照射して前記イオン交換前駆体溶液700を架橋反応させて細孔充填イオン交換高分子電解質を製造する段階と、前記製造された細孔充填イオン交換高分子電解質を含む高分子支持体、上部フィルム及び下部フィルムを着脱ロールから脱着させる段階と、を含む表面イオン交換高分子電解質が除去されたイオン交換高分子電解質複合膜の製造方法を提供する。
多孔性構造を有する高分子支持体と、前記高分子支持体に含浸されたイオン交換高分子電解質と、を含む細孔充填イオン交換高分子電解質複合膜であって、前記イオン交換高分子電解質は、前記高分子支持体の外部に形成されず、前記イオン交換高分子電解質複合膜の表面に前記高分子支持体の多孔性構造が露出されることを特徴とする表面イオン交換高分子電解質が除去された細孔充填イオン交換高分子電解質複合膜を提供する。
陽イオン基を有する4級アンモニウム塩の電解質モノマーまたは、陰イオン基を有するスルホン酸含有電解質モノマー、3級アミン作用基を有するアクリルアミド系架橋剤、開始剤及び溶媒を含むイオン交換前駆体溶液700を製造する段階と、前記イオン交換前駆体溶液700に多孔性高分子支持体110を含浸させる段階と、上部フィルム200、前記多孔性高分子支持体110及び下部フィルム300を圧着ロールに投入させて前記高分子支持体110の上部及び下部にそれぞれ前記上部フィルム200及び下部フィルム300を圧着させる段階と、前記上部フィルム200及び下部フィルム300が圧着された多孔性高分子支持体110に紫外線を照射して前記イオン交換前駆体溶液700を架橋反応させて細孔充填イオン交換高分子電解質を製造する段階と、前記製造された細孔充填イオン交換高分子電解質を含む高分子支持体110、上部フィルム200及び下部フィルム300を着脱ロールから脱着させる段階と、を含む表面イオン交換高分子電解質が除去された細孔充填イオン交換高分子電解質複合膜の製造方法を提供する。
多孔性構造を有する高分子支持体と、前記高分子支持体に含浸されたイオン交換高分子電解質と、を含む細孔充填イオン交換高分子電解質複合膜であって、前記イオン交換高分子電解質は、前記高分子支持体の外部に形成されず、前記イオン交換高分子電解質複合膜の表面に前記高分子支持体の多孔性構造が露出されることを特徴とする表面イオン交換高分子電解質が除去された細孔充填イオン交換高分子電解質複合膜を提供する。
陰イオン交換高分子電解質複合膜を製造するために、(3−アクリルアミドプロピル)塩化トリメチルアンモニウム[(3-acrylamidopropyl)trimethylammonium chloride]、1,4−ビスアクリロイルピペラジン[1,4-bis(acryloyl)piperazine]、脱イオン化された水を12:1:10の重量比で混合撹拌し、前記混合溶液100重量部に対して光開始剤としてメタノールに10重量%で希釈させた2−ヒドロキシ−2−メチル−1−フェニルプロパン−1−オン(2-hydroxy-2-methyl-1-phenylpropane-1-one)を0.1〜0.5重量部で混合して陰イオン交換前駆体溶液700を製造した。
陽イオン交換高分子電解質複合膜は、前記製造例1の陰イオン交換高分子電解質複合膜と同じ方法を利用して製造し、ただ陽イオン交換前駆体溶液700を製造するために、下記のような方法を遂行した。
スクイズ圧着を行わないことを除いては、前記製造例1及び2と同じ方法を使用して陰イオン及び陽イオン交換高分子電解質複合膜を製造した。
Fuma-tech社の陰イオン交換高分子電解質複合膜(FAS)及び陽イオン交換高分子電解質複合膜(FKS)を準備した。
Tokuyama社の陰イオン交換高分子電解質複合膜(AMX)及び陽イオン交換高分子電解質複合膜(CMX)を準備した。
Asahi社の陰イオン交換高分子電解質複合膜(AMV)及び陽イオン交換高分子電解質複合膜(CMV)を準備した。
前記製造例1及び比較例1で使用したポリオレフィン多孔性高分子支持体の表面及び断面のSEM写真をそれぞれ図2及び図5に示した。また、前記製造例1で製造した陰イオン交換高分子電解質複合膜の表面及び断面のSEM写真を図3及び図6にそれぞれ示した。図3に示したように前記製造例1で製造された陰イオン交換高分子電解質複合膜は、表面に形成された架橋重合された高分子樹脂が除去されて表面の細孔構造が示されることが確認できた。また、図6に示したように複合膜厚が約16.55μmであって、多孔性高分子支持体の厚さ(約16μm)と特に差がなく、表面に形成された架橋重合された高分子樹脂が除去されたということを確認することができた。
前記製造例1(図8)、製造例2(図12)及び比較例2(図9、図13)、比較例3(図10、図14)、比較例4(図11、図15)による陰イオン及び陽イオン交換高分子電解質複合膜表面の粗度(roughness)をAFM(Atomic Force Microscopy)で分析して図8及び図15に示し、下記表1に粗さ値を示した。
前記製造例1~2及び比較例2〜4による陰イオン及び陽イオン交換高分子電解質複合膜の特性を分析して下記表2に示した。
200 ・・・上部フィルム
300 ・・・下部フィルム
400 ・・・上部圧着ロール
450 ・・・下部圧着ロール
500 ・・・上部着脱ロール
550 ・・・下部着脱ロール
600 ・・・照射装置
700 ・・・イオン交換前駆体溶液
710 ・・・高分子樹脂
Claims (19)
- 陽イオン基を有する4級アンモニウム塩の電解質モノマーまたは、陰イオン基を有するスルホン酸含有電解質モノマー、3級アミン作用基を有するアクリルアミド系架橋剤、開始剤及び溶媒を含むイオン交換前駆体溶液を製造する段階と、
前記イオン交換前駆体溶液に多孔性高分子支持体を含浸させる段階と、
上部フィルム、前記多孔性高分子支持体及び下部フィルムを圧着ロールに投入させて前記高分子支持体の上部及び下部にそれぞれ前記上部フィルム及び下部フィルムを圧着させる段階と、
前記上部フィルム及び下部フィルムが圧着された多孔性高分子支持体に紫外線を照射して前記イオン交換前駆体溶液を架橋反応させて細孔充填イオン交換高分子電解質を製造する段階と、
前記製造された細孔充填イオン交換高分子電解質を含む高分子支持体、上部フィルム及び下部フィルムを着脱ロールから脱着させる段階と、
を含む、表面イオン交換高分子電解質が除去された細孔充填イオン交換高分子電解質複合膜の製造方法。 - 前記陽イオン基を有する4級アンモニウム塩の電解質モノマーは、(3−アクリルアミドプロピル)塩化トリメチルアンモニウム[(3-acrylamidopropyl)trimethylammonium chloride]、塩化(ビニルベンジル)トリメチルアンモニウム[(vinylbenzyl)trimethylammonium chloride]及びそれらの組み合わせからなる群から選択される物質を含む、請求項1に記載の表面イオン交換高分子電解質が除去された細孔充填イオン交換高分子電解質複合膜の製造方法。
- 前記陰イオン基を有するスルホン酸含有電解質モノマーは、2−アクリルアミド−2−メチルプロパンスルホン酸ナトリウム(sodium 2-acrylamido-2-methylpropane sulfonate)、ビニルスルホン酸ナトリウム(sodium vinylsulfonate)、ビニルスルホン酸(vinylsulfonic acid)、アリルスルホン酸ナトリウム(sodium allyl sulfonate)、2−メチル−2−プロペン−1−スルホン酸ナトリウム(sodium 2-methyl-2-propene-1-sulfonate)、3−スルホプロピルアクリレートナトリウム塩(3-sulfopropyl acrylate sodium salt)及びそれらの組み合わせからなる群から選択される物質を含む、請求項1に記載の表面イオン交換高分子電解質が除去された細孔充填イオン交換高分子電解質複合膜の製造方法。
- 前記3級アミン作用基を有するアクリルアミド系架橋剤は、N,N’−ビス(アクリロイル)ピペラジン[N,N’-bis(acryloyl)piperazine]、N,N’−(1,2−ジヒドロキシエチレン)ビスアクリルアミド[N,N’-(1,2-dihydroxyethylene)bisacrylamide]、N,N’−メチレンビスアクリルアミド(N,N’-methylenebisacrylamide)、N,N’−メチレンビスメタクリルアミド(N,N’-methylenebismethacrylamide)及びそれらの組み合わせからなる群から選択される物質を含む、請求項1に記載の表面イオン交換高分子電解質が除去された細孔充填イオン交換高分子電解質複合膜の製造方法。
- 前記多孔性高分子支持体は、空隙体積が40%〜50%、気孔サイズが0.07μm〜0.1μm、厚さが8μm〜30μmである、請求項1に記載の表面イオン交換高分子電解質が除去された細孔充填イオン交換高分子電解質複合膜の製造方法。
- 前記多孔性高分子支持体は、前記イオン交換前駆体溶液に含浸される前に界面活性剤によって親水化処理されるものである、請求項1に記載の表面イオン交換高分子電解質が除去された細孔充填イオン交換高分子電解質複合膜の製造方法。
- 前記上部フィルム及び下部フィルムは、ポリ(エチレンテレフタレート)[poly(ethylene terephthalate), PET]、ポリイミド(polyimide)、ポリ塩化ビニル(polyvinyl chloride)、低密度ポリエチレン(low density polyethylene)、低密度ポリプロピレン(low density polypropylene)及びそれらの組み合わせからなる群から選択される物質を含む、請求項1に記載の表面イオン交換高分子電解質が除去された細孔充填イオン交換高分子電解質複合膜の製造方法。
- 前記上部フィルム及び下部フィルムは、前記多孔性高分子支持体と接触する一面が親水処理された、請求項1に記載の表面イオン交換高分子電解質が除去された細孔充填イオン交換高分子電解質複合膜の製造方法。
- 前記圧着は、前記圧着ロールに投入される多孔性高分子支持体厚さ及びフィルム厚さの和よりも低い値を有するようにスクイズ圧着を通じて行われる、請求項1に記載の表面イオン交換高分子電解質が除去された細孔充填イオン交換高分子電解質複合膜の製造方法。
- 前記値は、前記圧着ロールに投入される多孔性高分子支持体厚さ及びフィルム厚さの和よりも5μm〜20μmほど小さい、請求項9に記載の表面イオン交換高分子電解質が除去された細孔充填イオン交換高分子電解質複合膜の製造方法。
- 前記照射される紫外線のエネルギーは、30mW/cm2〜50mW/cm2である、請求項1に記載の表面イオン交換高分子電解質が除去された細孔充填イオン交換高分子電解質複合膜の製造方法。
- 前記架橋反応時、前記多孔性高分子支持体及びフィルムの温度は、75℃以下である、請求項1に記載の表面イオン交換高分子電解質が除去された細孔充填イオン交換高分子電解質複合膜の製造方法。
- 前記脱着を通じて前記多孔性高分子支持体の外部に形成された架橋重合された高分子樹脂が前記上部フィルム及び下部フィルムに転写されて除去される、請求項1に記載の表面イオン交換高分子電解質が除去された細孔充填イオン交換高分子電解質複合膜の製造方法。
- 多孔性構造を有する高分子支持体と、
前記高分子支持体に含浸されたイオン交換高分子電解質と、を含む細孔充填イオン交換高分子電解質複合膜であって、
前記イオン交換高分子電解質は、前記高分子支持体の外部に形成されず、
前記イオン交換高分子電解質複合膜の表面に前記高分子支持体の多孔性構造が露出されることを特徴とする表面イオン交換高分子電解質が除去された細孔充填イオン交換高分子電解質複合膜。 - 前記細孔充填イオン交換高分子電解質複合膜の面積比抵抗は、0.35Ω・cm2以下である、請求項14に記載の表面イオン交換高分子電解質が除去された細孔充填イオン交換高分子電解質複合膜。
- 前記細孔充填イオン交換高分子電解質複合膜の支配的表面粗度(roughness height)は、200nm〜350nmである、請求項14に記載の表面イオン交換高分子電解質が除去された細孔充填イオン交換高分子電解質複合膜。
- 前記高分子支持体厚さに対する細孔充填イオン交換高分子電解質複合膜厚比率は、1.0〜1.03である、請求項14に記載の表面イオン交換高分子電解質が除去された細孔充填イオン交換高分子電解質複合膜。
- 前記細孔充填イオン交換高分子電解質複合膜厚は、8μm〜30μmである、請求項14に記載の表面イオン交換高分子電解質が除去された細孔充填イオン交換高分子電解質複合膜。
- 前記高分子支持体及びイオン交換高分子電解質の重さ比率は、1:0.8〜1:1.1である、請求項14に記載の表面イオン交換高分子電解質が除去された細孔充填イオン交換高分子電解質複合膜。
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