JP6463777B2 - 電気化学的装置 - Google Patents
電気化学的装置 Download PDFInfo
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- JP6463777B2 JP6463777B2 JP2016559881A JP2016559881A JP6463777B2 JP 6463777 B2 JP6463777 B2 JP 6463777B2 JP 2016559881 A JP2016559881 A JP 2016559881A JP 2016559881 A JP2016559881 A JP 2016559881A JP 6463777 B2 JP6463777 B2 JP 6463777B2
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Description
本発明は、少なくとも部分的に、米国政府の助成ではARPA−E契約第DE−AR−0000345号の下で、また、エネルギー省とは契約第DE−SC0004453号の下で、なされた。政府は、本発明に所定の権利を有する。
本出願は、2014年10月21日出願の米国仮特許出願第62/066,823号明細書に関連しかつその優先権の利益を主張し、また、2015年2月3日出願の国際特許出願第PCT/US2015/14328号明細書「電解装置及び膜(Electrolyzer and Membranes)」の優先権の利益を主張する。本出願はまた、2013年9月24日出願の米国特許出願第14/035,935号明細書「二酸化炭素を有用な燃料及び化学品に転換するための装置及び方法(Devices and Processes for Carbon Dioxide Conversion into Useful Fuels and Chemicals)」;2010年7月4日出願の米国特許出願第12/830,338号明細書「新規触媒混合物(Novel Catalyst Mixtures)」;2011年3月25日出願の国際出願第PCT/2011/030098号明細書「新規触媒混合物(Novel Catalyst Mixtures)」;2011年6月30日出願の米国特許出願第13/174,365号明細書「新規触媒混合物(Novel Catalyst Mixtures)」;2011年7月1日出願の国際特許出願第PCT/US2011/042809号明細書「新規触媒混合物(Novel Catalyst Mixtures)」;2012年6月21日出願の米国特許出願第13/530,058号明細書「二酸化炭素及び他の最終用途のためのセンサー(Sensors for Carbon Dioxide and Other End Uses)」;2012年6月22日出願の国際特許出願第PCT/US2012/043651号明細書「低コスト二酸化炭素センサー(Low Cost Carbon Dioxide Sensors)」;及び2012年4月12日出願の米国特許出願第13/445,887号明細書「二酸化炭素転換のための電解触媒(Electrocatalysts for Carbon Dioxide Conversion)」に関する。
本発明の分野は、電気化学である。記載される装置及びシステムは、有用な生成物への二酸化炭素の電気化学的転換、水の電気分解、燃料セル、及び電気化学的浄水に関する。
地球温暖化を低減し環境を保護する方法として、産業設備や発電所からの二酸化炭素(CO2)の排出を減らす要望がある。1つの解決方法は、炭素隔離として知られ、CO2の捕獲と貯蔵に関係する。しばしばCO2が単に埋蔵される。CO2を単に埋蔵したり貯蔵したりする代わりに、それを他の生成物に転換して有益な用途に供することができれば、有益であると考えられる。
1.カソードを以下のように作製する:
a. 30mgの銀ナノ粒子(20〜40nm、在庫番号45509、Alfa Aesar,Ward Hill,MA)を0.1mlの脱イオン水(18.2Mohm、EMD Millipore,Billerica,MA)及び0.2mlのイソプロパノール(在庫番号3032−16、Macron Fine Chemicals,Avantor Performance Materials,Center Valley,PA)と混合することによって、銀インクを作製する。次いで、混合物を1分間超音波処理する。
b. 銀ナノ粒子インクをガス拡散層(Sigracet 35 BC GDL、Ion Power Inc.,New Castle,DE)上に、2.5cm×2.5cmの面積を覆うように、手で塗布する。
2.アノードを以下のように作製する:
a. 15mgのRuO2(在庫番号11804、Alfa Aesar)を0.2mlの脱イオン水(18.2Mohm Millipore)、0.2mlのイソプロパノール(在庫番号3032−16、Macron)、及び0.1mlの5%ナフィオン溶液(1100EW、DuPont,Wilmington,DE)と混合することによってRuO2インクを作製する。
b. RuO2インクをガス拡散層(Sigracet 35 BC GDL、Ion Power)上に、2.5cm×2.5cmの面積を覆うように、手で塗布する。
3.「試験」材料の厚さ50〜300マイクロメートルの膜を、流し込み又は押出し成形など、従来の手法で作製する。
4.膜を、アノードとカソードの間に、銀触媒と酸化ルテニウム触媒が膜に対面するようにして、挟む。
5.アセンブリー全体を、サーペンタインフローフィールドを備えたFuel Cell Technologies(Albuquerque,NM)の5cm2の燃料セルハードウェアの中に取り付ける。
6.室温及び室内圧力下でセルを用い、50℃で加湿したCO2を5sccmの流量でカソードに供給し、室温及び室内圧力下でアノード側を大気に開放したままとし、セルに3.0Vを印加し、セルを室温で30分動作させた後、カソード放出物組成を分析する。
7.選択性を以下のように計算する:
(CO2転換電流)=(合計セル電流)×(選択性)。
本明細書に記載の特定の方法、プロトコル、及び試薬は、当業者が理解するように様々であってもよいため、本方法はこれらに限定されないことを理解されたい。また、本明細書で使用される用語は、具体的な実施形態のみを説明するために使用されるものであり、本方法の範囲を限定することを意図しないことも理解されたい。また本明細書及び添付の特許請求の範囲で使用される場合、単数形「a」、「an」、及び「the」は、文脈が明確に他に指定していなければ、複数形への言及を含むことも留意されたい。したがって、例えば「a linker」への言及は、当業者に公知の1つ又は複数のリンカー及びその同等物への言及である。同様に、語句「及び/又は」は、述べられた事柄の一方又は両方が起こり得ることを示すために使用され、例えば、A及び/又はBは、(A及びB)と(A又はB)を包含する。
本明細書で使用される用語「CO2の電気化学的転換」は、電気化学的プロセスのいずれかの工程において二酸化炭素、炭酸塩、又は炭酸水素塩が別の化学物質に転換されるいかなるプロセスをも指す。
P+(R12R13R14R15)
(式中、R12〜R15は、水素、ハライド、直鎖アルキル、分岐アルキル、環状アルキル、ヘテロアルキル、アリール、ヘテロアリール、アルキルアリール、ヘテロアルキルアリール、及びそれらのポリマーから選択される。)のリガンドが具体的に挙げられる。
概して、電気化学セルは、図1に示すように、アノード50、カソード51、及び電解質53を有する。膜52もまたセルに含まれることがある。所望の化学反応を促進するように、触媒を、アノード50上及び/又はカソード51上及び/又は電解質53中に配置してもよい。作動中に、反応物又は反応物を含む溶液をセルに供給する。そして、アノードとカソードの間に電圧を印加して、電気化学的反応を促進する。
具体例1は、補助膜を備えた電解装置を作出する手順を例示する。具体例1の実施形態は、CO2転換に用いられた従来の電気化学セルに比較して、改善された性能を例証する。
比較例1は、「有機生成物混合物の一部としてのメタノールの選択性を提供することができ、メタノールに対する二酸化炭素のファラデー収率が30%〜95%で、残りは水素を発生させる」システムを開示していると主張する‘583公開の教示に従って構成された電解装置の定常電流及びファラデー効率を測定した。しかしながら、‘583公開は、カソードが液体非接触である場合の、30%〜95%のファラデー収率を例証するデータを提供しない。比較例1では、セルを‘583公開の教示に従って組み立て、液体非接触カソードを用いて室温でファラデー効率を測定した。
ナフィオン、スルホン化ポリ(エーテルエーテルケトン)「SPEEK」、ポリビニルアルコール(PVA)、ポリエチレンイミン(PEI)、CMI−7000、AMI7001、リン酸ドープしたPBI、又はネオセプタの各膜が、表1に記載する先行文献に記載された通りに前処理された場合に補助膜として作用するかどうかを判定するために、比較例2を行った。
この例の目的は、膜ドーピングにおける変更が膜を活性化させてCO2を転換することができるかどうかを判定することであった。AMI−7001とCMI−7000は、PSMMIMとPSDMIMにおけるのと同じポリスチレン主鎖を有するが異なるアミン基を有し、そのため活性化させることが可能であり得るので、それらを試験例として選んだ。
具体例3の目的は、補助膜の他の一例を提供することである。
具体例4の目的は、ピリジニウム基をもった補助膜の一例を提供することである。
この例の目的は、ポリマーにおけるアミン部分の、性能に対する影響を調べることであった。補助膜を種々の組成のメチルイミダゾリウム−ポリ(4−ビニルベンジルクロリド−コ−スチレン)クロリド(PSMIM−Cl)ポリマー溶液から作製した。
この例の目的は、補強した補助膜の例を提供することである。特に、メチルイミダゾリウム−ポリ(4−ビニルベンジルクロリド−コ−スチレン)クロリド(PSMIM−Cl)と、ポリマーマトリクス、例えばポリベンゾイミダゾール(PBI)、ポリ(2,6−ジメチル−1,2−フェニレンオキシド)(PPO)、ナイロン6/6、又はポリエチレン(PE)との混合物から作製される補助膜が提供される。
この例の目的は、スチレンを含有しない補助膜を同定することである。特に、メチルイミダゾリウム−ポリ(ビニルベンジルクロリド−コ−メチルメタクリラート−コ−ブチルアクリラート)クロリド(PVMBMIM−Cl)と言われる、メチルメタクリラート(MMA)とブチルアクリラート(BA)とVBCの1−メチルイミダゾール付加物とのターポリマーが補助膜であることが示されることになる。
この例の目的は、水分保持を改善するために親水性材料を膜に加えることができることを例証することである。この例では、膜中の水分吸収と水分保持を改善するために、吸湿性酸化物材料を膜の作製中に導入した。吸湿性酸化物材料としては、シリカ(SiO2)、ジルコニア(ZrO2)、及びチタニア(TiO2)が挙げられる。この例ででは、ジルコニアを試験した。
この例の目的は、水分保持を改善するために潮解性材料ZnBrを膜に加えることができることを例証することである。
最初に、50mgの銀ナノ粒子(20〜40nm、45509、Alfa Aesar)を0.8mlの脱イオン水(18.2Mohm Millipore)及び0.4mLのイソプロパノール(3032−16、Macron)に加えることによって銀ナノ粒子インクを作製した。次いで、混合物を1分間超音波処理した。得られた銀インクを、炭素繊維紙(Toray Paper 120、40%防湿性、東レ株式会社、日本東京)の上に、5cm×5cmの面積を覆うように、エアブラシした。次いで、この四角形を、それぞれ2.5cmx2.5cmの等しいサイズの4つの四角形に切り分けた。
この実験の目的は、補助膜が水電解装置に有用であることを例証することである。
この例は、補助膜がまた、アルカリ膜燃料セルに有用であることを示す。
この例の目的は、メチルイミダゾリウム−ポリ(2,6−ジメチル−1,4−フェニレンオキシド)ブロミド(PPOMIM−Br)ポリマー溶液から作製された補助膜を提供することである。
この例の目的は、スチレンをもたないメチルイミダゾリウム−ポリ(4−ビニルベンジルクロリド膜もまた補助膜であるかどうかを判定することである。
この例の目的は、ポリ(ビニルベンジルクロリド)(PVBC)とポリベンゾイミダゾール(PBI)との混合物から作製される補助膜を提供することである。
この例の目的は、スズのカソード触媒と上の表4のPBI/PSMIM−Clアニオン交換膜番号6とを用いることによって電気化学的装置中でCO2をギ酸に転換する手順を例示することである。
この例の目的は、(2−ヒドロキシエチル)リミダゾリウム(limidazolium)−ポリ(4−ビニルベンジルクロリド−コ−スチレン)クロリド(PSIMOH−Cl)ポリマー溶液から作製される膜が補助膜であることを示すことである。
Claims (9)
- (a)アノードと、
(b)カソードと、
(c)前記アノードと前記カソードの間に挿入されたポリマー電解質膜であって、前記ポリマー電解質膜の少なくとも一部は、
(1)カーボンペーパー製ガス拡散層上に6mg/cm2の銀ナノ粒子を含むカソードを作製することと、
(2)カーボンペーパー製ガス拡散層上に3mg/cm2のRuO2を含むアノードを作製することと、
(3)ポリマー電解質膜試験材料を作製することと、
(4)前記アノードと前記カソードの間に前記膜試験材料を挿入し、カソードの前記銀ナノ粒子を上に配置した側を前記膜の一方の側に対面させ、前記アノードのRuO2を上に配置した側を前記膜の他方の側に対面させ、それによって膜電極アセンブリーを形成することと、
(5)前記膜電極アセンブリーを、カソード反応物流体フローチャネル及びアノード反応物流体フローチャネルを有する燃料セル構造体の中に取り付けることと、
(6)前記燃料セル構造体が室温及び大気圧下にあり、前記アノード反応物流体フローチャネルを室温及び室内圧力下で大気に開放したままの状態で、50℃で加湿したCO2の流れを、前記カソードに対面している前記カソード反応物流体フローチャネルの中に送ることと、
(7)前記アノードと前記カソードの間の電気的接続によって3.0Vのセル電位を印加することと、
(8)前記カソードのフローチャネルの出口で、前記セルを通る電流とCO及びH2の濃度とを測定することと、
(9)CO選択性を
(10)前記膜での平均電流密度が少なくとも20mA/cm2であり、前記選択性が3.0Vのセル電位で少なくとも50%であれば、前記膜を補助膜として同定することと、
を含む試験を適用することによって特定できる補助膜である、ポリマー電解質膜と、
を含むCO2を反応生成物に転換する電気化学的装置。 - 前記ポリマー電解質膜が完全に補助膜である、請求項1に記載の電気化学的装置。
- 電気分解の間にバルク液体が前記カソードに直接接触しないように前記カソードが本質的に液体非接触の状態で作動されるとき、所望の前記反応生成物のためのファラデー効率が50%超である、請求項1に記載の電気化学的装置。
- 前記補助膜は、イミダゾリウムリガンド、ピリジニウムリガンド、及びホスホニウムリガンドのうち少なくとも1つを含有するポリマーを含む、請求項1に記載の電気化学的装置。
- 前記アノードは前記膜に対面する触媒被覆を有し、前記カソードは前記膜に対面する触媒被覆を有する、請求項1に記載の電気化学的装置。
- 前記ポリマー電解質膜が本質的に水に不混和性である、請求項1に記載の電気化学的装置。
- 前記反応生成物は、CO、HCO-、H2CO、(HCO2)-、H2CO2、CH3OH、CH4、C2H4、CH3CH2OH、CH3COO-、CH3COOH、C2H6、(COOH)2、(COO-)2、H2C=CHCOOH、及びCF3COOHからなる群より選択される、請求項1に記載の電気化学的装置。
- 触媒活性元素をさらに含む、請求項1に記載の電気化学的装置。
- 前記触媒活性元素はAu、Ag、Cu、Sn、Sb、Bi、Zn、及びInからなる群より選択される、請求項8に記載の電気化学的装置。
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JP6721637B2 (ja) | 2020-07-15 |
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KR20170140423A (ko) | 2017-12-20 |
EP3209816B1 (en) | 2021-03-03 |
AU2018204762A1 (en) | 2018-07-19 |
KR20160105909A (ko) | 2016-09-07 |
EP3209816A1 (en) | 2017-08-30 |
CN106170339A (zh) | 2016-11-30 |
WO2016064447A1 (en) | 2016-04-28 |
CA2941423C (en) | 2020-05-26 |
WO2016064440A1 (en) | 2016-04-28 |
JP2018204021A (ja) | 2018-12-27 |
AU2015337093A1 (en) | 2016-08-18 |
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CA2941423A1 (en) | 2016-04-28 |
KR101809161B1 (ko) | 2017-12-14 |
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