JP2022550655A - 燃料電池膜用組成物、及びその調製方法 - Google Patents
燃料電池膜用組成物、及びその調製方法 Download PDFInfo
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- JP2022550655A JP2022550655A JP2021570137A JP2021570137A JP2022550655A JP 2022550655 A JP2022550655 A JP 2022550655A JP 2021570137 A JP2021570137 A JP 2021570137A JP 2021570137 A JP2021570137 A JP 2021570137A JP 2022550655 A JP2022550655 A JP 2022550655A
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- nafion
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- nanocellulose
- polydopamine
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Abstract
Description
本発明は、燃料電池膜用組成物、及びその調製方法に関する。特に、本発明は、熱機械的、及び化学的に安定な高分子電解質膜に関する。より具体的には、本発明は、多官能性ポリドーパミン、及び機械的に強靭なナノセルロースを使用することによる、高分子電解質膜の熱機械的、及び化学的安定性の向上に関する。本発明はさらに、前記高分子電解質膜の調製方法に関する。本発明で開発された膜は、燃料電池、電池、及び他の電気化学デバイス用の固体電解質膜の分野での用途を見出す。
高分子電解質膜であるナフィオンは、スルホン化テトラフルオロエチレンベースのフルオロポリマー-コポリマーである。テトラフルオロエチレン(テフロン(登録商標))骨格上にスルホン酸基で終端されたパーフルオロビニルエーテル基の存在は、クラスで最高のナフィオンのイオン特性をもたらす。ナフィオンは、プロトン交換膜(PEM)燃料電池のプロトン伝導体として知られている。ナフィオンは、さまざまなカチオン伝導性をもって製造できる。ナフィオンは、その特性により幅広い範囲の用途がある。ナフィオンは、燃料電池、電気化学デバイス、塩素アルカリ生成、金属イオン回収、水電解、めっき、金属の表面処理、電池、センサー、ドナン透析セル、薬物放出、ガス乾燥又は加湿、及びファインケミカル製造の超強酸触媒に使用される。ナフィオンはまた、多くの分野での理論的可能性(すなわち、これまで試されていない)がよく挙げられる。
したがって、本発明の主な目的は、これまでに報告された従来技術の欠点を取り除き、向上したプロトン伝導性を有する、化学的に及び熱機械的に安定な高分子電解質膜を提供することである。
本発明は、ポリドーパミン被覆ナノセルロースとナフィオンとの新規の複合膜、及びその調製方法に関する。
本発明の図、スキーム、及び説明は、本発明の明確な理解に関連する要素を説明するため、簡略化されていることを理解されたい。詳細な説明は、添付の図面、及びスキームを参照して、以下に提供される。
a)洗浄したコットンラグ片を10%水酸化ナトリウム溶液で、次いで脱イオン水[DI]で処理し、得られたコットンラグを酢酸緩衝液及び1.5重量%次亜塩素酸ナトリウムで漂白した後、精練、及び粉砕して、コットンラグナノセルロースを得ることによってコットンラグナノセルロース(CNF)を調製する工程;
b)ドーパミン塩酸塩モノマー0.5~2mg/mLを、70~90℃で、20~30時間の撹拌下にトリス緩衝液に分散させ、凍結乾燥してポリドーパミン(PDA)を得ることにより、ポリドーパミン(PDA)を調製する工程;
c)工程[a]で調製したナノセルロース(CNF)2mg/mLを、25℃で速度500rpmでの10~12時間の攪拌及び15~20分間の浴超音波処理の下で、pH 8.5のトリス緩衝液に分散させ、次いで、ドーパミン塩酸塩モノマーを、分散したNC溶液に、ドーパミン:NCの1:4~1:1の範囲内の比率で添加し、70~90℃で、20~30時間撹拌し、次いで得られた塊を凍結乾燥して、ポリドーパミン被覆ナノセルロース(PNC)を得ることにより、ポリドーパミン被覆ナノセルロース(PNC)を調製する工程;
d)ナフィオン膜を小片に切断し、イソプロピルアルコールとエチルアルコールとの24:1(v/v)混合物に、25~30℃の範囲内の温度、500rpmの速度で攪拌することにより、溶解することにより、ナフィオン溶液を調製する工程;
e)25~30℃の範囲内の温度、500rpmの速度で、周期的な浴超音波処理を伴って、2~3時間攪拌することによって、イソプロピルアルコールとエチルアルコールとの24:1(v/v)混合物中で、撹拌、及び超音波処理することによって、上記の工程[a]、[b]、及び[c]から得られたCNF、又はPDA、又はPNCの均質な分散液を調製し、次いで、予め分散したCNF、又はPDA、又はPNC溶液を、工程[d]で得た予め溶解したナフィオン溶液に添加し、ボルテックスミキシングでよく混合し、30℃の温度、500rpmの速度で攪拌し、溶液を脱気し、ガラスペトリ皿にキャストして、3重量%CNF/ナフィオン、又は3重量%PDA/ナフィオン、又は3~7.5重量%PNC/ナフィオン膜を得る工程を含み、すべての膜の乾燥状態での厚さは、ランダムな5箇所で測定し、40~55μmであることが観測される。
図3bは、PNCの取り込みが、ナフィオンの熱機械的特性に対し非常に有意な効果を有し、その結果、高温での貯蔵弾性率が200%向上したことを示す。30℃における3重量%PNC/ナフィオン複合膜の貯蔵弾性率は、約540MPaであり、リキャストナフィオンの貯蔵弾性率よりもおおよそ50%高い。図3bは、さまざまな温度にわたる複合膜の弾性率の変化を示す。3重量%PNC/ナフィオン複合膜は、60℃及び90℃の高温において、リキャストナフィオンより70%、及び96%高い弾性率をそれぞれ示す。この向上は、PNCの濃度が高いほど、有意に高く、7.5重量%PNC/ナフィオン複合材料は、755MPa(30℃)、555MPa(60℃)、及び310(90℃)の弾性率を示し、これはリキャストナフィオンよりも、各温度において約150、170、及び200%高い。高温での膜の貯蔵弾性率の向上は、ホットプレスによる触媒層の組み立ての間の熱機械的安定性をもたらし、大量生産における膜電極接合体(MEA)の品質を維持するのに役立つことができる。
透過型電子顕微鏡分析:繊維の直径を決定するため、粉砕したセルロース懸濁液をDI水中で0.05mg/mLに希釈した。希釈分散液を30分間超音波処理し、カーボン被覆された銅グリッド上にドロップキャストした。グリッドをフード内で25~30℃で24~36時間乾燥させ、いかなるわずかな水をも除去した。乾燥したグリッドを200kVの加速電圧でTEM分析に供した。
以下の例は、説明のためにのみ与えられており、したがって、いかなる方法でも本発明の範囲を限定するものと解釈されるべきではない。
ナノセルロースは、化学的方法と機械的方法との組み合わせを用いて、コットンラグから抽出した。コットンラグを小片に切断し、脱イオン(DI)水で洗浄した。洗浄したコットンラグ片を60~80℃で、10%NaOHにより処理し、続いてDI水で洗浄した。NaOH処理後、同じ割合の酢酸緩衝液(27gのNaOH及び75mLの氷酢酸を、蒸留水を用いて1000mLに希釈)及び1.5重量%次亜塩素酸ナトリウムを使用することにより、コットンラグを漂白した。この方法は、繊維が白くなるまで(繊維の柔らかさに応じて)複数回繰り返し、その後DI水で洗浄した。漂白されたコットンラグは、バレービーターを使用して精練して細かいパルプにし、次にウルトラフリクションマイクログラインダー(スーパーマスコライダー、日本の増幸)によって粉砕した。静止した砥石車と回転する砥石車との間で高い剪断力を受けたマイクロファイバーパルプは、ナノファイバーに解繊された(TEMで確認した)。最後に、コットンラグナノセルロース(CNF)パルプを必要に応じて凍結乾燥し、多孔質エアロゲルを得た。
NC(2mg/mL)1.0gを、10mMトリス緩衝液500mLに25℃で12時間撹拌することによって分散させ、超音波処理を20分間行った。よく分散したNC溶液に、ドーパミン塩酸塩モノマー1.0g(2mg/mL)(NCとの重量比が1:1)を添加した。この反応混合物を80℃で24時間撹拌した。DI水を添加して反応をクエンチした。クエンチした反応混合物をろ過し、無色の上澄みが得られるまでDI水で洗浄した。濾液をDI水に再分散させ、さらなる使用のために凍結乾燥させた。同様の方法で、ドーパミン(2mg/mL)を水に分散させた後、トリス緩衝液を添加して10mMの溶液を作り、ポリドーパミン粒子を合成した。
ナフィオン膜を小片に切断し、IPAとEtOHとの24:1(v/v)混合物に溶解した。同様の溶媒混合物中で撹拌、及び超音波処理することにより、CNF又はPDA又はPNCの均一な分散液も得た。約51mgのPNC又はPDA又はCNFを含む分散液をナフィオン溶液(1.65gのナフィオンを含む)に添加して、3重量%ナフィオン複合材料を得た。同様に、7.5重量%PNC/ナフィオン複合材料は、予め分散したPNC127.5mgを、予め溶解したナフィオン1.57gに添加することによって調製した。対照サンプルとして、ナフィオン1.7gをIPA:EtOHの共溶媒混合物に溶解してナフィオン溶液も調製した。すべての溶液を真空下、40℃で脱気して、トラップされた空気を除去した。脱気した溶液を膜キャスト用ペトリ皿に注ぎ、周囲条件で36時間、次に真空下で24時間、溶媒を徐々に蒸発させて、残留溶媒をすべて除去した。すべての膜の乾燥状態での厚さは、5つのランダムな場所で測定し、約40~55μmであることがわかり、乾燥した膜はさらなるキャラクタリゼーションのために使用された。
・ポリドーパミン被覆ナノセルロース(PNC)を使用すると、プロトン伝導性を損なうことなく、ナフィオンの熱機械的及び化学的安定性が向上する。
・3重量%PNCは、ナフィオン膜の熱機械的安定性、化学的安定性を有意に向上させるだけでなく、プロトン伝導性も有意に向上する。
・向上した熱機械的特性は、バッテリー及びその他の電気化学デバイスでの使用を可能にする。
・ナフィオンインクは、燃料電池用の触媒インクの調製にも使用される。ナフィオンにPNCが存在すると、炭素担持Pt触媒とナフィオンとの間の良好な界面及びそれ故の触媒の効果的な利用をもたらす。
Claims (5)
- ナフィオン、及び3~7.5重量%のポリドーパミン被覆セルロースナノファイバーを含み、セルロースナノファイバー上のポリドーパミン被覆がセルロースナノファイバーの重量に対して10~12重量%である燃料電池膜用組成物。
- 前記組成物が、プロトン伝導性、熱安定性、機械的安定性及び化学的安定性において、15~76%の増加を示す、請求項1に記載の組成物。
- 前記組成物が、セルロースナノファイバー上に被覆されたポリドーパミンを3重量%含む、請求項1に記載の組成物。
- a) 洗浄されたコットンラグ片を10%水酸化ナトリウム溶液で、次いで脱イオン水[DI]で処理し、得られたコットンラグを酢酸緩衝液及び1.5重量%次亜塩素酸ナトリウムで漂白した後、バレービーターを用いて精練して細かいパルプにした後、ウルトラフリクションマイクログラインダーで粉砕してコットンラグナノセルロースを得ることにより、コットンラグナノセルロース(CNF)を調製する工程;
b) ドーパミン塩酸塩モノマー0.5~2mg/mLを、70~90℃で、20~30時間の攪拌の下にトリス緩衝液に分散させ、凍結乾燥してポリドーパミン(PDA)を得ることにより、ポリドーパミン(PDA)を調製する工程;
c) 工程[a]で調製したナノセルロース(CNF)2mg/mLを、25℃、500rpmの速度での10~12時間の攪拌及び15~20分間の浴超音波処理の下に、pH 8.5のトリス緩衝溶液に分散させ、次いで、ドーパミン塩酸塩モノマーを、分散したナノセルロース溶液に、ドーパミン:ナノセルロースの1:4~1:1の範囲内の比率で添加し、70~90℃で、20~30時間攪拌し、次いで得られた塊を凍結乾燥して、ポリドーパミン被覆ナノセルロース(PNC)を得ることにより、ポリドーパミン被覆ナノセルロース(PNC)を調製する工程;
d) ナフィオン膜を小片に切断し、イソプロピルアルコールとエチルアルコールとの24:1(v/v)混合物に、25~30℃の範囲内の温度、500rpmの速度で攪拌することにより溶解することにより、ナフィオン溶液を調製する工程;
e) 25~30℃の範囲内の温度、500rpmの速度で、周期的な浴超音波処理を伴って、2~3時間攪拌することによって、イソプロピルアルコールとエチルアルコールとの24:1(v/v)混合物中で攪拌、及び超音波処理して、上記の工程[a]、[b]及び[c]から得られたCNF又はPDA又はPNCの均質な分散液を調製し、次いで予め分散したCNF又はPDA又はPNC溶液を、工程[d]で得た予め溶解したナフィオン溶液に添加し、ボルテックスミキシングでよく混合し、30℃の温度、500rpmの速度で攪拌し、その溶液を脱気し、ガラスペトリ皿にキャストして、3重量%CNF/ナフィオン又は3重量%PDA/ナフィオン又は3~7.5重量%PNC/ナフィオン膜を得る工程を含み、すべての膜の乾燥状態での厚さは5箇所のランダムな位置で測定し、40~55μmであることが観測される、請求項1に記載の組成物の調製方法。 - 前記燃料電池膜の厚さが40~55μmである、請求項1に記載の組成物。
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CN101842931B (zh) * | 2007-08-29 | 2013-09-25 | 科学与工业研究委员会 | 可用于聚合物电解质燃料电池的质子传导聚合物电解质膜 |
US9385388B2 (en) * | 2011-06-16 | 2016-07-05 | Lg Chem, Ltd. | Polymer electrolyte membrane for fuel cell, membrane electrode assembly and fuel cell including the same |
CN102738494B (zh) * | 2012-05-18 | 2016-02-17 | 东华大学 | 细菌纤维素/Nafion质子交换混合膜及制备和应用 |
CN103715438B (zh) * | 2013-12-27 | 2015-09-30 | 郑州大学 | 一种纳米复合质子交换膜及其制备方法和应用 |
CN104530682B (zh) * | 2015-01-16 | 2017-01-25 | 长春工业大学 | 纳米纤维素/磺化聚芳醚酮复合膜及其制备方法与应用 |
KR102339036B1 (ko) * | 2017-09-29 | 2021-12-13 | 코오롱인더스트리 주식회사 | 라디칼 분해 촉매, 이의 제조 방법, 이를 포함하는 막-전극 어셈블리, 그리고 이를 포함하는 연료 전지 |
CN108285643A (zh) * | 2017-10-19 | 2018-07-17 | 天津工业大学 | 一种纤维素纳米纤维/磺化聚醚砜质子交换膜及制备方法 |
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2020
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- 2020-05-26 JP JP2021570137A patent/JP2022550655A/ja active Pending
- 2020-05-26 CN CN202080039443.5A patent/CN113906087B/zh active Active
- 2020-05-26 EP EP20814058.2A patent/EP3976695A1/en active Pending
- 2020-05-26 WO PCT/IN2020/050470 patent/WO2020240585A1/en unknown
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EP3976695A1 (en) | 2022-04-06 |
CA3141780A1 (en) | 2020-12-03 |
CN113906087A (zh) | 2022-01-07 |
US20220311037A1 (en) | 2022-09-29 |
WO2020240585A1 (en) | 2020-12-03 |
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