JP2018524150A - 酸素を除去するためのナノ構造化した鉄/炭素 - Google Patents
酸素を除去するためのナノ構造化した鉄/炭素 Download PDFInfo
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- JP2018524150A JP2018524150A JP2017560586A JP2017560586A JP2018524150A JP 2018524150 A JP2018524150 A JP 2018524150A JP 2017560586 A JP2017560586 A JP 2017560586A JP 2017560586 A JP2017560586 A JP 2017560586A JP 2018524150 A JP2018524150 A JP 2018524150A
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- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 82
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 239000001301 oxygen Substances 0.000 title claims abstract description 79
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 76
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 28
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- 229930182830 galactose Natural products 0.000 claims description 2
- GDSRMADSINPKSL-HSEONFRVSA-N gamma-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO GDSRMADSINPKSL-HSEONFRVSA-N 0.000 claims description 2
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Images
Classifications
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Abstract
【選択図】なし
Description
i.多孔質構造を有する少なくとも1つの炭素粒子を金属イオンの溶液中に浸漬して、前記金属イオンを前記炭素粒子の細孔内に含浸させる工程と、
ii.含侵された炭素粒子を乾燥させる工程と、
iii.前記含侵された炭素粒子を、前記複合材料を合成するための条件で、炭素熱還元過程に供する工程とを含む。
本願に用いられる以下の単語および用語は以下に示す意味を有するものとする。
ここで複合材料の例示的かつ非限定的な実施形態を開示する。
i.多孔質構造を有する少なくとも1つの炭素粒子を金属イオンの溶液中に浸漬して、前記金属イオンを前記炭素粒子の細孔内に含浸させる工程と、
ii.含侵された炭素粒子を乾燥させる工程と、
iii.前記含侵された炭素粒子を、複合材料を合成するための条件で、炭素熱還元過程に供する工程とを含む。
F−127ブロックコポリマーによってテンプレートされたα−シクロデキストリンに由来する炭素粒子(C1)の調製
シグマ オールドリッチ(Sigma Aldrich)(アメリカ合衆国ミズーリ州セントルイス)から入手した22.5mgのF−127ブロックコポリマーを15mLの脱イオン水中に溶解して、室温で一晩撹拌した。合計で45mgのα−シクロデキストリン(日本の東京化成工業株式会社から入手したTCI−GR)を15mLの脱イオン水中に溶解して、室温で一晩撹拌した。次に、調製したα−シクロデキストリン溶液をF−127の溶液中に700rpmで撹拌しながら注入した。前記F−127ブロックコポリマーは、炭素粒子の大きさを制御し、かつ2)炭素粒子内に細孔を生成するように機能する。
D−(+)−グルコサミン塩酸塩に由来する炭素粒子(C2)の調製
160mgのD−(+)−グルコサミン塩酸塩(≧99%、シグマ オールドリッチ)を30mLの脱イオン水中に溶解して、清澄溶液を形成した。次に前記溶液をテフロン(登録商標)加工のステンレス鋼オートクレーブ(容量125mL)に移した。前記オートクレーブを200℃で12時間にわたって加熱し、次いで室温に冷ました。9000rpmで30分間にわたって遠心分離することによりC2粒子を得た。次に、前記粒子を脱イオン水で、それぞれ9000rpmで15分間にわたる遠心分離によって、3回洗浄した。得られたC2粒子を風乾し、次いでさらなる使用のために室温で真空乾燥した。
D−(+)−グルコースに由来する炭素粒子(C3)の調製
3.0〜4.5gのD−(+)−グルコース(≧99.5%、東京化成工業株式会社、日本)を30mLの脱イオン水中に溶解して、清澄溶液を形成した。次に前記溶液をテフロン(登録商標)加工のステンレス鋼オートクレーブ(容量125mL)に移した。前記オートクレーブを180℃で3時間にわたって加熱し、次いで室温に冷ました。9000rpmで30分間にわたって遠心分離することによりC3粒子を得た。次に、前記粒子を脱イオン水で、それぞれ9000rpmで15分間にわたる遠心分離によって、3回洗浄した。得られたC3粒子を風乾し、次いでさらなる使用のために室温で真空乾燥した。
ナノ構造化したFe0/C1粒子(nanostructured Fe0/C1 particles)(Fe0/C1)の調製
0.15gの実施例1から得たC1粒子を脱イオン水中に分散させた。適当な量の硝酸鉄(III)九水和物(≧98%、シグマ オールドリッチ(Sigma Aldrich))(炭素に対して〜50wt%のFe)を脱イオン水中に溶解した。次に、硝酸鉄(III)九水和物溶液をC1溶液に添加し、10分間にわたって超音波処理し、数時間にわたって間欠的に振動させた。前記C1粒子を鉄(III)溶液中に一晩浸漬した。室温の真空炉中において水を蒸発させて乾燥させた。集めたC1粒子粉末を次に管状炉の内部の石英管内に配置し、200 sccmのアルゴン流量下において、5℃/分のランプレートで800℃に加熱した。前記試料を800℃で3時間にわたって維持した。その後、前記試料を管状炉から取り出す前にアルゴン下で周囲温度まで冷ました。その合成したままのナノ構造化したFe0/C1粒子は特性評価を行える状態であった。
ナノ構造化したFe0/C2粒子(Fe0/C2)の調製
0.15gの実施例2から得たC2粒子を脱イオン水中に分散させた。適当な量の硝酸鉄(III)九水和物(≧98%、シグマ オールドリッチ)(炭素に対して〜50wt%のFe)を脱イオン水中に溶解した。次に、硝酸鉄(III)九水和物溶液をC2溶液に添加し、10分間にわたって超音波処理し、数時間にわたって間欠的に振動させた。前記C2粒子を鉄(III)溶液中に一晩浸漬した。室温の真空炉中において水を蒸発させて乾燥させた。集めたC2粒子粉末を次に管状炉の内部の石英管内に配置し、200 sccmのアルゴン流量下において、5℃/分のランプレートで800℃に加熱した。前記試料を800℃で3時間にわたって維持した。その後、前記試料を管状炉から取り出す前にアルゴン下で周囲温度まで冷ました。その合成したままのナノ構造化したFe0/C2粒子は特性評価を行える状態であった。
ナノ構造化したFe0/C3粒子(Fe0/C3)の調製
0.15gの実施例3から得たC3粒子を脱イオン水中に分散させた。適当な量の硝酸鉄(III)九水和物(≧98%、シグマ オールドリッチ)(炭素に対して〜50wt%のFe)を脱イオン水中に溶解した。次に、硝酸鉄(III)九水和物溶液をC3溶液に添加し、10分間にわたって超音波処理し、数時間にわたって間欠的に振動させた。前記C3粒子を鉄(III)溶液中に一晩浸漬した。室温の真空炉中において水を蒸発させて乾燥させた。集めたC3粒子粉末を次に管状炉の内部の石英管内に配置し、200 sccmのアルゴン流量下において、5℃/分のランプレートで800℃に加熱した。前記試料を800℃で3時間にわたって維持した。その後、前記試料を管状炉から取り出す前にアルゴン下で周囲温度まで冷ました。その合成したままのナノ構造化したFe0/C3粒子は特性評価を行える状態であった。
透過型電子顕微鏡(TEM)およびエネルギー分散型X線(EDX)
TEMおよびEDX分析は、透過型電子顕微鏡(JEOL 2100 TEM)によって200kVの加速電圧下で実施した。すべての試料を最初にエタノールで分散させて希釈し、次いで観察の前に200メッシュの炭素被覆銅グリッド(200−mesh carbon coated copper grid)上に滴下して室温で乾燥させた。
試料の構造特性および結晶相をXRD分析によって評価した。XRD分析は、20〜86°に及ぶ走査角度でCukα放射線(k=0.154nm)を使用したブルカー D8−ジェネラル エリア ディテクター ディフラクション システム(Bruker D8−General Area Detector Diffraction System)(GADDS) XRDを用いることによって実施した。ここで試料Fe0/C1粒子を分析し、異なる条件において試験したFe0/C1粒子のXRDパターンを図4および図5に示す。
25mLのガラス三角フラスコを試料容器(モデル包装)として用いて、前記試料のO2除去特性を特徴付けた。フラスコの全容量を最初に周囲条件において空気(20.90%のO2)で充填した。1mLの水を収容した1つの2mLのバイアルを前記フラスコの内側に配置して、室内湿度(RH)を100%に調節した。約0.03〜0.05gの試料(Fe0/C1、Fe0/C2およびFe0/C3)を塩化ナトリウム(乾燥物または50μL溶液)とともに、または塩化ナトリウムなしで、前記フラスコの内部に配置した。次に、前記フラスコを気密性ゴムセプタムストッパー(シュバシール(Suba−Seal)、ダブリュ.フリーマン アンド カンパニー リミテッド(W. Freeman & Co. Ltd)、英国)によって密閉し、酸素除去実験の期間中、室温に配置した。前記フラスコのヘッドスペース中の酸素含有量(% O2)をヘッドスペース酸素/二酸化炭素アナライザ(モデル GS3、システック イリノイ(Systec Illinois)、米国、0.005% O2までの精度)によって、ヘッドスペースガスのアリコートを採取してジルコニウムに基づくセンサーを用いて分析する手順にて分析した。0.45μmのPTFEフィルタを備えた試料採取針を前記ストッパーを介して挿入して、〜0.875mLのヘッドスペースガスを試料採取した。ヘッドスペースアナライザの較正は、各試料測定の後に周囲空気を用いて行われた。酸素吸収量(Oxygen uptake)(消費された酸素の質量/試料の質量)は、前記フラスコのヘッドスペース内における酸素含有量の(約96時間の)経時的な減少から間接的に計算した。
前記複合材料は、酸素除去ナノ構造複合物として用いられ得る。酸素除去ナノ構造複合物は、食品包装に用いられてもよく、小袋(sachets)、透過性バッグ、シート状マットおよび積層シートのような様々な容器内に配置されて、そのような容器の内容物を酸素による劣化または酸素との反応から保護する。
Claims (27)
- 少なくとも1つの金属粒子と炭素材料との混合物を含有する複合材料。
- 前記炭素材料はバイオマス材料に由来する、請求項1に記載の複合材料。
- 前記バイオマス材料は、リグニン、糖、脂肪酸、タンパク質、およびそれらの組み合わせからなる群から選択される、請求項2に記載の複合材料。
- 前記バイオマス材料は、単糖、二糖、オリゴ糖または多糖から選択された糖である、請求項3に記載の複合材料。
- 前記単糖は、グルコース、フルクトースおよびガラクトースからなる群から選択される、請求項4に記載の複合材料。
- 前記オリゴ糖は、砂糖またはアミノ糖からなる群から選択される、請求項4に記載の複合材料。
- 前記多糖は、シクロデキストリン、セルロース、デンプン、グリコーゲン、キチンおよびヘミセルロースからなる群から選択される、請求項4に記載の複合材料。
- 前記糖は、α−シクロデキストリン、β−シクロデキストリン、γ−シクロデキストリン、D−グルコサミン塩酸塩、L−グルコサミン塩酸塩、α−D−グルコース、β−D−グルコース、α−L−グルコース、およびβ−L−グルコースからなる群から選択される、請求項4乃至7のいずれか1項に記載の複合材料。
- 前記炭素材料は、炭素粒子またはシート状材料である、請求項1乃至8のいずれか1項に記載の複合材料。
- 前記炭素材料は、10〜700nmの範囲である細孔サイズを有した多孔質構造を有する、請求項1乃至9のいずれか1項に記載の複合材料。
- 前記炭素材料は、50m2/g〜約1000m2/gの範囲である表面積を有する、請求項1乃至10のいずれか1項に記載の複合材料。
- 前記炭素材料は前記金属粒子の支持体として作用する、請求項1乃至11のいずれか1項に記載の複合材料。
- 前記金属粒子は遷移金属粒子である、請求項1乃至12のいずれか1項に記載の複合材料。
- 前記遷移金属粒子の遷移金属は、鉄粒子、ルテニウム粒子、オスミウム粒子、コバルト粒子、ロジウム粒子、イリジウム粒子、マンガン粒子、およびそれらの組み合わせからなる群から選択される、請求項13に記載の複合材料。
- 前記金属粒子は500nm未満の粒径を有する、請求項1乃至14のいずれか1項に記載の複合材料。
- 前記複合材料中の前記金属粒子の濃度は、前記炭素材料の乾燥重量%に基づいて、1〜80重量%の範囲であり得る、請求項1乃至15のいずれか1項に記載の複合材料。
- i.少なくとも1つの金属粒子と炭素材料との混合物を含有する複合材料と、
ii.無機塩類と、
iii.任意で水性媒体とを含む、組成物。 - 前記無機塩類は電解質または酸性化剤である、請求項18に記載の組成物。
- 前記電解質は、ハロゲン化アルカリ金属、ハロゲン化アルカリ土類金属、およびハロゲン化金属からなる群から選択されたハロゲン化物化合物である、請求項17または18のいずれか1項に記載の組成物。
- 前記無機塩類の濃度は、前記複合材料の乾燥重量に基づいて、0.1〜20wt%の範囲である、請求項17乃至19のいずれか1項に記載の組成物。
- 前記無機塩類は、ポリアクリル酸、ポリメタクリル酸、ポリエチルアクリル酸およびポリマレイン酸からなる群から選択されたポリ酸である、請求項17または18のいずれか1項に記載の組成物。
- 少なくとも1つの金属粒子と炭素材料との混合物を含有する複合材料を合成する方法であって、前記方法は、
i.多孔質構造を有する少なくとも1つの炭素粒子を金属イオンの溶液中に浸漬して、前記金属イオンを前記炭素粒子の細孔内に含浸させる工程と、
ii.含侵された炭素粒子を乾燥させる工程と、
iii.前記含侵された炭素粒子を、前記複合材料を合成するための条件で、炭素熱還元過程に供する工程とを含む、方法。 - 前記金属イオンの溶液は、金属硝酸塩、金属塩化物、金属硫酸塩、金属グルコン酸塩、金属クエン酸塩および金属シュウ酸塩からなる群から選択された金属塩に由来する、請求項22に記載の方法。
- 前記浸漬工程は、30分間〜24時間の範囲の期間にわたって行われる、請求項22または23のいずれか1項に記載の方法。
- 前記供する工程は、700〜1000℃の範囲の温度で行われる、請求項22乃至24のいずれか1項に記載の方法。
- 前記供する工程は、不活性ガス環境において行われる、請求項22乃至25のいずれか1項に記載の方法。
- 多層フィルムであって、
i.外的環境から前記多層フィルム内への酸素の透過を妨げる酸素バリア層と、
ii.少なくとも1つの金属粒子と炭素材料との混合物を有する複合材料を含む酸素除去層とを備えた、多層フィルム。
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