JP2024508632A - 複合プロトン伝導性膜 - Google Patents
複合プロトン伝導性膜 Download PDFInfo
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- JP2024508632A JP2024508632A JP2023546071A JP2023546071A JP2024508632A JP 2024508632 A JP2024508632 A JP 2024508632A JP 2023546071 A JP2023546071 A JP 2023546071A JP 2023546071 A JP2023546071 A JP 2023546071A JP 2024508632 A JP2024508632 A JP 2024508632A
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- KIUKXJAPPMFGSW-DNGZLQJQSA-N (2S,3S,4S,5R,6R)-6-[(2S,3R,4R,5S,6R)-3-Acetamido-2-[(2S,3S,4R,5R,6R)-6-[(2R,3R,4R,5S,6R)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylic acid Chemical compound CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 KIUKXJAPPMFGSW-DNGZLQJQSA-N 0.000 claims description 12
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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 9
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- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 claims description 7
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- 229920009441 perflouroethylene propylene Polymers 0.000 claims description 7
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- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
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- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 4
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- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000013153 zeolitic imidazolate framework Substances 0.000 claims description 3
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- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims 1
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- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 30
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 17
- YACKEPLHDIMKIO-UHFFFAOYSA-N methylphosphonic acid Chemical compound CP(O)(O)=O YACKEPLHDIMKIO-UHFFFAOYSA-N 0.000 description 16
- 239000001257 hydrogen Substances 0.000 description 15
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 14
- 125000000217 alkyl group Chemical group 0.000 description 14
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- 239000000203 mixture Substances 0.000 description 14
- NSETWVJZUWGCKE-UHFFFAOYSA-N propylphosphonic acid Chemical compound CCCP(O)(O)=O NSETWVJZUWGCKE-UHFFFAOYSA-N 0.000 description 14
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- 150000002500 ions Chemical class 0.000 description 12
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- MGRVRXRGTBOSHW-UHFFFAOYSA-N (aminomethyl)phosphonic acid Chemical compound NCP(O)(O)=O MGRVRXRGTBOSHW-UHFFFAOYSA-N 0.000 description 10
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 description 10
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Abstract
Description
本出願は、2021年1月29日に出願された米国出願第17/162,421号の優先権を主張するものであり、その全体が本明細書に組み込まれる。
6.5重量%のアルギン酸ナトリウム水溶液を、アルギン酸ナトリウムポリマーをDI水に溶解することによって調製した。Daramic,LLCから購入したDaramic(登録商標)175微孔性支持膜の一方の表面を、6.5重量%のアルギン酸ナトリウム水溶液の薄層でコーティングし、60℃で2時間オーブン中で乾燥させて、Daramic(登録商標)支持膜の表面上に15マイクロメートルの厚さを有する薄い非多孔性のアルギン酸ナトリウム層を形成した。乾燥させた膜を、1.0M塩酸水溶液で30分間処理して、水溶性アルギン酸ナトリウムコーティング層を水不溶性アルギン酸コーティング層に変換した。
水中の、480~550m2/gの高表面積を有するアミノプロピル-N,N-ビス(メチルホスホン酸)官能化シリカゲル(Silicycleから購入したSilicaMetS(登録商標)AMPA;AMPA-SiO2と略記)及びアルギン酸ナトリウムの分散液を、0.5gのAMPA-SiO2及び10.0gのアルギン酸ナトリウムを150.0mLのDI水に添加し、混合物を8時間撹拌することによって調製した。Daramic,LLCから購入したDaramic(登録商標)175微孔性支持膜を分散液の薄層でコーティングし、60℃で2時間オーブン中で乾燥させて、Daramic(登録商標)支持膜の一方の表面に15マイクロメートルの厚さを有するAMPA-SiO2及びアルギン酸ナトリウムを含む薄い非多孔性層を形成した。乾燥させた膜を、1.0M塩酸水溶液で30分間処理して、水溶性アルギン酸ナトリウムコーティング層を水不溶性アルギン酸に変換した。
比較例1で調製されたAA/Daramic膜及び実施例1で調製されたAMPA-SiO2-AA/Daramic(登録商標)複合膜のイオン伝導率、バッテリ充電/放電サイクル数、VE、CE、及びEEを、BCS-810バッテリサイクリングシステム(Biologic,FRANCE)を備えたEISを用いて室温で測定し、結果を表1に示した。表1から、AMPA-SiO2無機充填剤を含む新たなAMPA-SiO2-AA/Daramic(登録商標)膜は、AMPA-SiO2無機充填剤を含まないAA/Daramic膜よりも低い面積比抵抗、長いバッテリサイクル、高いCE、及び高いEEを示した。
a負の電解質溶液:1.5M FeCl2、3.5M NH4Cl、0.2Mホウ酸;正の電解質:1.5M FeCl2、3.5M NH4Cl、0.4M HCl;充電電流密度:30mA/cm2;充電時間:4時間;放電電流密度:30mA/cm2;放電時間:4時間;サイクル数を70%以上のCEで計数した。
AMPA-SiO2/Nafion(登録商標)複合材膜を調製するために、Silicycleから購入した480~550m2/g(SilicaMetS(登録商標)AMPA;AMPA-SiO2と略記)の高表面積を有するアミノプロピル-N,N-ビス(メチルホスホン酸)官能化シリカゲル及びNafion(登録商標)を含む分散液を、AMPA-SiO2をNafion(登録商標)分散液D2021(1100 EW、アルコール中20重量%)に超音波処理及び撹拌下で添加することによって調製した。AMPA-SiO2とNafion(登録商標)ポリマーとの重量比は、1:20である。分散液の薄層を、流延ナイフを使用して清浄なガラス板上に分散液を流延することによって形成し、ホットプレート上で30℃で12時間乾燥させて、AMPA-SiO2/Nafion(登録商標)膜を形成した。膜を80℃で9時間更に乾燥させた。乾燥させた膜をガラス板から剥がし、更に100℃で9時間加熱した。膜の最終的な厚さは、60μmであった。
TA-SiO2/Nafion(登録商標)複合膜を調製するために、Silicycleから購入した4-エチルベンゼンスルホン酸官能化シリカ(SilicaBond(登録商標)トシル酸;TA-SiO2と略記)及びNafion(登録商標)を含む分散液を、超音波処理及び撹拌下でTA-SiO2をNafion(登録商標)分散液D2021(1100 EW、アルコール中20重量%)に添加することによって調製した。TA-SiO2とNafion(登録商標)ポリマーとの重量比は、1:20である。分散液の薄層を、流延ナイフを使用して清浄なガラス板上に分散液を流延することによって形成し、ホットプレート上で30℃で12時間乾燥させて、TA-SiO2/Nafion(登録商標)膜を形成した。膜を80℃で9時間更に乾燥させた。乾燥させた膜をガラス板から剥がし、更に100℃で9時間加熱した。膜の最終的な厚さは、60μmであった。
AMPA-SiO2/Nafion(登録商標)複合膜を含む5AMPA-D2021 MEAを、アノード用にIrO2酸素発生反応(OER)触媒を、カソード用にPt/C水素発生反応(HER)触媒を使用して、ガス拡散層上コーティング触媒(catalyst coated on gas diffusion layer、CCG)法によって調製した。噴霧用の触媒インクは、DI水及びアルコール中で触媒及びNafion(登録商標)アイオノマー(アルコール中5重量%)を混合することによって調製した。混合物を、超音波浴中で微細に分散させた。アノード及びカソードの両方におけるNafion(登録商標)アイオノマー含有量を、触媒及びNafion(登録商標)アイオノマーの総含有量において30重量%に制御した。Pt/Cインクを、カソードガス拡散層として使用されるカーボン紙上に噴霧した。Pt担持量は、0.3mg/cm2であった。IrO2インクを、アノードガス拡散層として使用されるPt-Tiフェルト上に噴霧した)。IrO2担持量は、1.0mg/cm2であった。AMPA-SiO2/Nafion(登録商標)複合膜を、2つの触媒コーティングガス拡散層の間に挟んだ。次に、5AMPA-D2021 MEAを用いて試験セルを設置した。
AMPA-SiO2/Nafion(登録商標)複合膜の代わりに市販のNafion(登録商標)212膜を使用したことを除いて、実施例5で使用したものと同じガス拡散層上コーティング触媒(CCG)法によって、市販のNafion(登録商標)212膜を含むNafion(登録商標)212MEAを調製した。
PEM水電解試験ステーション(Scribner 600電解槽試験システム)を使用して、5cm2の活性膜面積を有する単一電解槽セルにおける5AMPA-D2021 MEA及びNafion(登録商標)212 MEAそれぞれの水電解性能を評価した。試験ステーションは、統合された電源、ポテンシオスタット、電気化学インピーダンス分光法(electrochemical impedance spectroscopy、EIS)及び高周波抵抗(HFR)のためのインピーダンス分析器、並びに生成物流量及びクロスオーバー監視のためのリアルタイムセンサーを含んだ。試験は、80~100℃及び大気圧で実施した。超純水を、100mL/分の流量でMEAのアノードに供給した。試験前に、セルをプレコンディショニングプロセスに供した。セルを60℃に加熱し、200mA/cm2で1時間、1A/cm2で1時間、続いて1.7Vで4時間保持した。次いで、セルを80℃に加熱し、200mA/cm2で1時間、1A/cm2で1時間保持した。これらのステップは、1つのコンディショニングサイクルとして一緒に数えられた。コンディショニング後、分極曲線を調製した(1分間保持の各データポイント端)。2回のコンディショニングサイクル後の分極結果を図1に示した。5AMPA-D2021 MEAは、Nafion(登録商標)212 MEAよりも低い分極電圧を示し、これは、新たなAMPA-SiO2/Nafion(登録商標)複合膜を含む5AMPA-D2021 MEAが、市販のNafion(登録商標)212膜を含むNafion(登録商標)212 MEAよりも高いプロトン伝導性を有することを示した。図1は、80℃、大気圧での5AMPA-D2021及びNafion(登録商標)212 MEAの水電解性能を示す。
AMPA-SiO2/Nafion(登録商標)複合膜を含む5AMPA-D2021-C MEAを、アノード用にIrO2酸素発生反応(OER)触媒を、カソード用にPt/C水素発生反応(HER)触媒を使用して、膜上コーティング触媒法によって調製した。噴霧用の触媒インクは、DI水及びアルコール中で触媒及びNafion(登録商標)アイオノマー(アルコール中5重量%)を混合することによって調製した。混合物を、超音波浴中で微細に分散させた。アノード及びカソードの両方におけるNafion(登録商標)アイオノマー含有量を、触媒及びNafion(登録商標)アイオノマーの総含有量において30重量%に制御した。Pt/Cインクを、前処理したAMPA-SiO2/Nafion(登録商標)複合膜の一方の表面上に噴霧した。Pt担持量は、0.3mg/cm2であった。IrO2インクを、前処理したAMPA-SiO2/Nafion(登録商標)複合膜の他方の表面上に噴霧した。IrO2担持量は、1.0mg/cm2であった。触媒コーティングAMPA-SiO2/Nafion(登録商標)複合体膜を、カソードガス拡散層としてのカーボン紙とアノードガス拡散層としてのPt-Tiフェルトとの間に挟んで、5AMPA-D2021-C MEAを形成した。
以下を特定の実施形態と併せて説明するが、本明細書は、前述の説明及び添付の特許請求の範囲の範囲を例解するものであり、限定することを意図するものではないことが理解されよう。
上記の複合プロトン伝導性膜と、複合プロトン伝導性膜の一方の表面上にアノード触媒を含むアノードと、
アノードガス拡散層と、複合プロトン伝導性膜の他方の表面上にカソード触媒を含むカソードと、
カソードガス拡散層と、を含み、複合プロトン伝導性膜は、
共有結合した酸性官能基及び少なくとも150m2/gの高表面積を有する無機充填剤と、水不溶性イオン伝導性ポリマーと、を含む。
Claims (10)
- 複合プロトン伝導性膜であって、
共有結合した酸性官能基及び少なくとも150m2/gの高表面積を有する無機充填剤と、
水不溶性イオン伝導性ポリマーと、を含む、複合プロトン伝導性膜。 - ポリエチレン、ポリプロピレン、ポリテトラフルオロエチレン、フッ素化エチレンプロピレン、ポリフッ化ビニリデン、ポリクロロトリフルオロエチレン、ポリカプロラクタム、ヘキサメチレンジアミン及びアジピン酸から調製されたポリマー、ポリアクリロニトリル、ポリエーテルスルホン、スルホン化ポリエーテルスルホン、ポリスルホン、スルホン化ポリスルホン、ポリ(エーテルエーテルケトン)、スルホン化ポリ(エーテルエーテルケトン)、ポリエステル、酢酸セルロース、三酢酸セルロース、セルロース、フェノール樹脂、ポリベンズイミダゾール、又はそれらの組み合わせから選択されるポリマーから調製された微孔性支持膜を更に含む、請求項1に記載の複合プロトン伝導性膜。
- シリカゲル、沈降シリカ、ヒュームドシリカ、コロイダルシリカ、アルミナ、シリカ-アルミナ、酸化ジルコニウム、モレキュラーシーブ、金属有機骨格、ゼオライトイミダゾレート骨格、共有結合有機骨格、又はそれらの組み合わせから選択され、前記無機充填剤が、共有結合した酸性官能基を含む、請求項1に記載の無機充填剤。
- 前記水不溶性イオン伝導性ポリマーが、過フッ素化カチオン交換ポリマー、架橋過フッ素化カチオン交換ポリマー、部分フッ素化カチオン交換ポリマー、架橋部分フッ素化カチオン交換ポリマー、非フッ素化炭化水素カチオン交換ポリマー、架橋非フッ素化炭化水素カチオン交換ポリマー、又はそれらの組み合わせから選択される、請求項1に記載の複合プロトン伝導性膜。
- 前記水不溶性イオン伝導性ポリマーが、水不溶性親水性ポリマー、又は電気的に中性の繰り返し単位と、-SO3 -、-COO-、-PO3 2-、-PO3H-、-C6H4O-、若しくは-O4B-などのイオン化官能基の画分との両方の繰り返し単位を含む水不溶性親水性ポリマー複合体である、請求項1に記載の複合プロトン伝導性膜。
- 前記水不溶性イオン伝導性ポリマーが、多糖ポリマー、架橋多糖ポリマー、金属イオン錯化多糖ポリマー、酸錯化多糖ポリマー、架橋ポリビニルアルコールポリマー、酸錯化ポリビニルアルコールポリマー、金属イオン錯化ポリビニルアルコールポリマー、架橋ポリ(アクリル酸)ポリマー、金属イオン錯化ポリ(アクリル酸)ポリマー、酸錯化ポリ(アクリル酸)ポリマー、架橋ポリ(メタクリル酸)、金属イオン錯化ポリ(メタクリル酸)、酸錯化ポリ(メタクリル酸)、又はそれらの組み合わせから選択される、請求項1に記載の複合プロトン伝導性膜。
- 前記多糖ポリマーが、アルギン酸、架橋アルギン酸、キトサン、架橋キトサン、ヒアルロン酸、架橋ヒアルロン酸、又はそれらの組み合わせから選択される、請求項6に記載の複合プロトン伝導性膜。
- レドックスフローバッテリシステムであって、
正の電解質と、負の電解質と、請求項1に記載の複合プロトン伝導性膜と、を含む少なくとも1つの再充電可能セルであって、前記複合プロトン伝導性膜が前記正の電解質と前記負の電解質との間に配置されており、前記正の電解質が正極と接触し、前記負の電解質が負極と接触する、少なくとも1つの再充電可能セルを含む、レドックスフローバッテリシステム。 - 膜電極アセンブリであって、
請求項1に記載の複合プロトン伝導性膜と、
前記複合プロトン伝導性膜の一方の表面上にアノード触媒を含むアノードと、
アノードガス拡散層と、
前記複合プロトン伝導性膜の他方の表面上にカソード触媒を含むカソードと、
カソードガス拡散層と、を含み、
前記複合プロトン伝導性膜が、
共有結合した酸性官能基及び少なくとも150m2/gの高表面積を有する無機充填剤と、
水不溶性イオン伝導性ポリマーと、を含む、膜電極アセンブリ。 - 複合プロトン伝導性膜を作製する方法であって、
a.水、有機溶媒、又は水/有機溶媒混合物中の水不溶性イオン伝導性ポリマーの分散液を調製することと、
b.前記水不溶性イオン伝導性ポリマー及び無機充填剤を含む混合分散液を、前記無機充填剤、又は水、有機溶媒、若しくは水/有機溶媒混合物中の前記無機充填剤の分散液を、撹拌及び/又は超音波処理下で前記水不溶性イオン伝導性ポリマーの前記分散液に添加することによって調製することであって、前記無機充填剤が、共有結合した酸性官能基及び少なくとも150m2/gの高表面積を有する、調製することと、
前記混合分散液の層を無孔性基材上又は微孔性支持膜上に流延し、続いて乾燥させることによって、複合プロトン伝導性膜を調製することと、を含む、方法。
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