JP7176126B1 - 高分子重合体廃棄物から多層カーボンナノチューブを合成するためのプロセス及び装置 - Google Patents
高分子重合体廃棄物から多層カーボンナノチューブを合成するためのプロセス及び装置 Download PDFInfo
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- JP7176126B1 JP7176126B1 JP2021547034A JP2021547034A JP7176126B1 JP 7176126 B1 JP7176126 B1 JP 7176126B1 JP 2021547034 A JP2021547034 A JP 2021547034A JP 2021547034 A JP2021547034 A JP 2021547034A JP 7176126 B1 JP7176126 B1 JP 7176126B1
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Abstract
Description
本発明は、多層カーボンナノチューブを合成するためのプロセス及び装置に関する。特に、本発明は、高分子重合体廃棄物から多層カーボンナノチューブを合成するためのプロセス及び装置に関する。
カーボンナノチューブは、結晶構造又は黒鉛構造を示す炭素の同素体の1つである(Ajayan, P.M., Chem Rev 1999)。カーボンナノチューブは、グラフェンと同様にsp2混成炭素分子結合によって結合され、円筒形構造に巻かれている(Cumings et al., Science 2000)。カーボンナノチューブは、単層カーボンナノチューブ(SWCNT)又は多層カーボンナノチューブ(MWCNT)のいずれかとして存在する。独特な電気及び機械特性は、90年代初期に発見されて以来、非常に大きい研究的及び化学的関心を集めた(Iijima, S., Nature 1991;Frackowiak, E., et al., Applied Physics Letters 2000)。MWCNTは、構造的にも機能的にもSWCNTとは異なっていた。MWCNTは、同じ触媒分岐(catalyst branch)から生じた、互いに包み込まれた同心円状の単層カーボンナノチューブから構成され、SWCNTと比べてより大きい直径、剛性及び伝導性をMWCNTにもたらす。これらの特性は、ナノ多孔性膜、冷陰極電界放出、スーパーキャパシタ、低摩擦ナノベアリング、超高感度電位計などの応用、そしてさらに多くの応用におけるMWCNTの使用を可能にした(Ajayan, P.M., Chem Rev 1999;Cumings et al., Science 2000;Frackowiak, E., et al., Applied Physics Letters 2000;Dai, H, Accounts of Chemical Research 2002;de Heer, W.A. et al., Science 1995;Roschier, L. et al., 2001;Shiflett, M. B. et al., Science 1999)。
本発明の1つの態様によると、多層カーボンナノチューブを合成するためのプロセスが提供される。本プロセスは、高分子重合体廃棄物を脱重合させて、炭素含有原料を得ることと、ステンレス鋼からなる一連の触媒材料を含有する触媒反応器内に炭素含有原料を供給することであって、一連の触媒材料が、触媒材料の表面に多層カーボンナノチューブを成長及び堆積させるのに十分なスペースを、任意の2つの隣接する触媒材料間に有してスタックされた形で配置されることと、一連の触媒材料を炭素含有原料の存在下で誘導加熱により加熱して、触媒材料の表面に多層カーボンナノチューブを形成することと、多層カーボンナノチューブを一連の触媒材料の表面から除去することとを含む。
本発明に従うプロセス及び装置の上記の利点及び特徴は以下の詳細な説明に記載され、図面に示される。
本発明は、高分子重合体廃棄物から多層カーボンナノチューブを合成するためのプロセス及び装置に関する。本プロセスは、低価値の高分子重合体廃棄物から、より良好な収率及び純度で高価値のカーボンナノチューブ(CNT)を合成するために、修正された触媒化学蒸着(CVD)プロセスと組み合わせて誘導加熱を使用することを含む。
材料及び方法
ポリスチレン及びポリプロピレンなどのプラスチック廃棄物、ゴム油、並びに廃棄調理用油は、局所廃棄物コレクターから入手した。金属メッシュは、Wiremesh Industries, Singaporeから入手した。分析グレードのエタノール、イソプロパノール及びアセトンはSigma-Aldrich, Singaporeから入手し、受け取ったまま使用した。硫酸はMerck, Singaporeから入手し、塩酸(37%)はPanreac, Singaporeから入手し、受け取ったまま使用した。
窒素雰囲気中でMettler-Toledo TGA DSC 1システムからの熱重量分析(TGA)を用いて、プラスチック廃棄物及び調理用油の分解温度を分析した。5℃/分の加熱温度で室温から500℃まで分析を実行した。質量分析(GC-MS)と連結したガスクロマトグラフィ(PerkinElmer, Clarus 6000)を用いて、プラスチック、ゴム及び調理用油の化学組成を同定及び定量した。多層MWCNTのラマンスペクトルは、室温でBruker SENTERRAラマン顕微鏡(λ=534nm、5mW)により測定した。エネルギー分散型X線分光法(EDX)(Oxford Instruments)と連結した電界放射型走査電子顕微鏡法(FESEM)(JEOL, JSM 7600F)を使用して、カーボンナノチューブのモルホロジーと、カーボンナノチューブ及び触媒表面の化学組成とを研究した。MWCNTのモルホロジーの確認のために透過電子顕微鏡法(TEM)(JEOL 2100F)を使用した。
触媒CVDプロセスの前に、プロセスパラメータ及び炭素源の化学組成を研究した。プラスチックの脱重合温度及び真空オーブン内の小鎖炭化水素蒸気の発生を特定するために、プラスチックの分解温度をまずTGA曲線から特定した。TGAスペクトルから炭化水素蒸気の最大発生が選択された温度は、プラスチックの性質及び化学組成に依存する。この実施例では、ポリプロピレン、ポリスチレン、並びに1:1、1:2及び2:1wt%/wt%のポリプロピレン及びポリスチレンの混合物などの熱可塑性樹脂を、多層カーボンナノチューブを合成するための炭素含有原料として研究した。
CxHy → xC+1/2yH2
触媒CVDにおける触媒材料として使用する前に、ステンレス鋼メッシュ/プレート/ロッドを化学的に前処理した。ステンレス鋼中のクロム含量は、より良好なカーボンナノチューブの成長のために12%未満でなければならない。ステンレス鋼メッシュ/プレート/ロッドをまずアセトン、エタノール又はイソプロパノール混合物中で洗浄して、微粒子及び有機残留汚染物質を除去した。次に、ステンレス鋼メッシュ/プレート/ロッドを3~10%の硫酸又は塩酸中で穏やかに前処理した。触媒CVDプロセスのための触媒材料として使用する前に、不活性窒素雰囲気において、酸処理したステンレス鋼メッシュ/プレート/ロッドを触媒反応器内で還元した。
ポリプロピレンを真空オーブン中400℃~480℃で脱重合させた。脱重合した油の中に、約100~120SCCMの窒素ガス流をバブリングした。小鎖炭化水素分子を触媒反応器内に移送及び供給し、約1:6の水素対窒素ガス流量比を用いてステンレス鋼メッシュ触媒材料の存在下において700℃~800℃の温度で加熱した。400トル(又は5.33x104Pa)よりも低い真空圧を反応器内で維持した。
ポリスチレンを真空オーブン中400℃~450℃の温度で脱重合させた。脱重合した油の中に、約120SCCMの窒素ガス流をバブリングした。小鎖炭化水素分子を触媒反応器内に移送及び供給し、約1:10の水素対窒素ガス流量比を用いてステンレス鋼メッシュ触媒材料の存在下において700℃~800℃の温度で加熱した。400トル(又は5.33x104Pa)よりも低い真空圧を反応器内で維持した。
1:2、1:1及び2:1wt%/wt%の重量比のポリプロピレン及びポリスチレンの混合物を考えた。約420℃~480℃の脱重合温度を真空オーブン内で維持して、小鎖炭化水素分子を得た。次に、小鎖炭化水素分子を触媒反応器内に移送及び供給し、約1:6の水素対窒素ガス流量比を用いてステンレス鋼メッシュ触媒材料の存在下において700℃~900℃の温度で加熱した。プロセスにおいて400トル(又は5.33x104Pa)よりも低い真空圧を維持した。カーボンナノチューブの品質をさらに改善するために、100:1の比率で水と混合したエタノール添加剤を100SCCMの窒素ガス炭化水素キャリアと共に導入した。MWCNTの長さの著しい増大が観察された。これは、触媒CVDプロセスにおける少量の水の酸化による触媒材料の再生に起因するものである。さらに、このプロセスは、より長く且つ垂直に整列したMWCNTをもたらした。
ゴム油は液体形態なので、真空オーブン中で加工するのではなく、バブラー内に直接供給した。120SCCMの窒素ガス流にバブラーを通過させる前に、バブラー内でゴム油をまず180℃~250℃の脱重合温度まで加熱した。小鎖炭化水素分子を触媒反応器内に移送及び供給し、約1:10の水素対窒素ガス流量比を用いてステンレス鋼メッシュ触媒材料の存在下において600℃~700℃で加熱した。400トル(又は5.33x104Pa)よりも低い真空圧を触媒反応器内で維持した。炭化水素ガスについては、触媒反応器へ通す前にバブラー内で窒素ガス流と均一に混合した。
ゴム油と同様の方法で植物油を加工した。まずバブラー内で植物油を400℃~480℃の温度で脱重合させた。油の中に120SCCMの窒素ガス流をバブリングした。小鎖炭化水素分子を触媒反応器内に移送及び供給し、約1:10の水素対窒素ガス流量比を用いてステンレス鋼メッシュ触媒材料の存在下において700℃~800℃で加熱した。400トル(又は5.33x104Pa)よりも低い真空圧を触媒反応器内で維持した。
バブラーを約90℃に維持したことを除いてゴム油と同様の方法で、エタノールを加工した。エタノールの中に120SCCMの窒素ガス流をバブリングした。次に、ガス状エタノールを触媒反応器内に移送及び供給し、約1:10の水素対窒素ガス流量比を用いてステンレス鋼メッシュ触媒材料の存在下において700℃~800℃で加熱した。400トル(又は5.33x104Pa)よりも低い真空圧を触媒反応器内で維持した。
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Claims (31)
- 多層カーボンナノチューブを合成するためのプロセスであって、
高分子重合体廃棄物を脱重合させて、炭素含有原料を得ることと、
タイプ304のステンレス鋼からなる一連の触媒材料内のクロム含量を12%未満まで低減させるために前記一連の触媒材料を酸で前処理することと、
前記一連の触媒材料を含有する触媒反応器内に還元ガスを導入することと、
前記一連の触媒材料の表面の活性部位を活性化するために前記還元ガスの存在下で誘導加熱により前記触媒反応器内で前記一連の触媒材料を加熱することと、
前記一連の触媒材料を含有する前記触媒反応器内に前記炭素含有原料を供給することであって、前記一連の触媒材料が、前記触媒材料の表面に多層カーボンナノチューブを成長及び堆積させるのに十分なスペースを、任意の2つの隣接する触媒材料間に有して水平にスタックされた形で配置される、供給することと、
前記一連の触媒材料を前記炭素含有原料の存在下で誘導加熱により加熱して、前記触媒材料の表面に多層カーボンナノチューブを形成することと、
前記多層カーボンナノチューブを前記一連の触媒材料の表面から除去することと、を含むプロセス。 - 前記高分子重合体廃棄物を脱重合させるステップが、不活性雰囲気中400℃~480℃の温度で前記高分子重合体廃棄物を加熱することを含む、請求項1に記載のプロセス。
- 前記高分子重合体廃棄物が30~120分間にわたって加熱される、請求項2に記載のプロセス。
- 前記炭素含有原料をバブラー内に供給することと、
前記炭素含有原料を前記反応器内に供給する前に、前記バブラー内の前記炭素含有原料の中に不活性ガスをバブリングすることと、をさらに含む、請求項1に記載のプロセス。 - 前記不活性ガスの前記バブラー内へのバブリングが、0.833x10-3~3x10-3m3/sの流速に維持される、請求項4に記載のプロセス。
- 前記炭素含有原料が、不活性キャリアガスと一緒に前記触媒反応器内に供給される、請求項1に記載のプロセス。
- 前記一連の触媒材料は、前記還元ガスの存在下で、および、前記炭素含有原料の存在下で同時に加熱される、請求項6に記載のプロセス。
- 前記還元ガスが水素を含む、請求項7に記載のプロセス。
- 前記炭素含有原料を前記触媒反応器内に供給する前に、前記炭素含有原料及び前記不活性キャリアガスを前記還元ガスと混合することをさらに含む、請求項7に記載のプロセス。
- 前記不活性キャリアガスが窒素であり、前記還元ガスが水素であり、窒素対水素ガス流量比が1:4~1:10に維持される、請求項9に記載のプロセス。
- 前記一連の触媒材料が、ステンレス鋼のシートの層からなる、プレート、メッシュ又はシートの形態の触媒材料からなる、請求項1に記載のプロセス。
- 前記一連の触媒材料が金属ロッドの形態の触媒材料からなり、前記触媒材料のそれぞれが、プレートを形成するように隣り合わせに配置された複数の金属ロッドを含み、複数の前記プレートが、前記一連の触媒材料を形成するように提供される、請求項11に記載のプロセス。
- 前記高分子重合体廃棄物が、廃棄有機溶媒、使用済み植物油及び調理用油、並びにポリプロピレン、ポリエチレン、ポリスチレン、ゴムからなる群から選択される1つ又は複数の長鎖熱可塑性ポリマーからなる群から選択される1つ又は複数である、請求項1に記載のプロセス。
- 前記誘導加熱が、前記反応器の外壁に近接してその周囲に巻き付けられた誘導コイルを用いて実行される、請求項1に記載のプロセス。
- 前記誘導加熱が、1kHz~60kHzの範囲の周波数を有するAC出力を前記誘導コイルに適用することによって実行される、請求項14に記載のプロセス。
- 前記誘導加熱が600℃~1000℃の温度で実行される、請求項14に記載のプロセス。
- 前記多層カーボンナノチューブが2μm~30μmの長さを有する、請求項1に記載のプロセス。
- 前記多層カーボンナノチューブが30nm~150nmの直径を有する、請求項1に記載のプロセス。
- 前記多層カーボンナノチューブが、機械的攪拌によって前記触媒材料から除去される、請求項1に記載のプロセス。
- 前記多層カーボンナノチューブが、前記複数の触媒材料を溶媒中で超音波処理し、前記溶媒中の多層カーボンナノチューブを熱乾燥にさらすことによって前記触媒材料から除去され、前記多層カーボンナノチューブが得られる、請求項1に記載のプロセス。
- 500℃~900℃の温度の空気中で前記複数の触媒材料を熱活性化することによって、前記複数の触媒材料を再使用のために再活性化することをさらに含む、請求項1に記載のプロセス。
- 前記熱活性化が超音波処理と組み合わせて実行される、請求項21に記載のプロセス。
- 高分子重合体廃棄物を脱重合させるためのチャンバと、
前記チャンバと流体連通する触媒反応器と
を含む、多層カーボンナノチューブを合成するための装置であって、前記触媒反応器が、
円筒形アウターケーシングと、
12%未満のクロム含量を有する前処理された304タイプのステンレス鋼からなる一連の触媒材料と、
前記一連の触媒材料を保持及び支持するように構成されたホルダセンブリであって、前記ホルダセンブリが、入口、出口、及び前記ホルダセンブリの長手方向表面に沿って提供された複数の開口を有し、
前記一連の触媒材料が、触媒材料の表面に多層カーボンナノチューブが成長できるようにするのに十分なスペースを、任意の2つの隣接する触媒材料間に有して水平にスタックされた形で配置された、ホルダセンブリと、
前記ホルダセンブリに接続されたガス分配チャネルと、
前記触媒反応器内の前記一連の触媒材料に均一な誘導加熱を提供することができる、前記アウターケーシングの外壁の周囲に巻き付けられた加熱素子と、を含む装置。 - 前記一連の触媒材料が、ステンレス鋼のシートの層からなる、プレート、メッシュ又はシートの形態の触媒材料からなる、請求項23に記載の装置。
- 前記一連の触媒材料が金属ロッドの形態の触媒材料からなり、前記触媒材料のそれぞれが、プレートを形成するように隣り合わせに配置された複数の金属ロッドを含み、複数の前記プレートが、前記一連の触媒材料を形成するように提供される、請求項23に記載の装置。
- 前記装置がさらに、
前記チャンバからの脱重合された原料を加工すると共に、前記脱重合された原料を前記触媒反応器に供給するように構成された、前記チャンバ及び前記触媒反応器と流体連通する第1のバブラーを含む、請求項23に記載の装置。 - 前記装置がさらに、前記触媒反応器と流体連通する第2のバブラーを含む、請求項26に記載の装置。
- 円筒形アウターケーシングと、
12%未満のクロム含量を有する前処理された304タイプのステンレス鋼からなる一連の触媒材料と、
前記一連の触媒材料を前記円筒形アウターケーシング内に保持及び支持するように構成されたホルダセンブリであって、入口、出口、及び前記ホルダセンブリ内から触媒反応器内へガスを分配するために前記ホルダセンブリの長手方向表面に沿って提供された複数の開口を有するホルダセンブリと、
ガス入口及びガス出口を有するガス分配チャネルであって、前記ガス出口が前記ホルダセンブリの入口に接続された、ガス分配チャネルと、
前記触媒反応器内の前記一連の触媒材料に均一な誘導加熱を提供することができる、前記アウターケーシングの外壁の周囲に巻き付けられた加熱素子と、を含む、多層カーボンナノチューブを合成するための触媒反応器であって、
前記一連の触媒材料が、触媒材料の表面に多層カーボンナノチューブを形成させるのに十分なスペースを、任意の2つの隣接する触媒材料間に有して水平にスタックされた形で配置される、触媒反応器。 - 前記ガス分配チャネルがさらに、前記ガス分配チャネルのガス出口に近接して提供された円板を含み、前記円板が、前記ガス分配チャネルを前記触媒反応器の前記円筒形アウターケーシングに固定するための固定手段を有する、請求項28に記載の触媒反応器。
- 前記一連の触媒材料が、ステンレス鋼のシートの層からなる、プレート、メッシュ又はシートの形態の触媒材料からなる、請求項28に記載の触媒反応器。
- 前記一連の触媒材料が金属ロッドの形態の触媒材料からなり、前記触媒材料のそれぞれが、プレートを形成するように隣り合わせに配置された複数の金属ロッドを含み、複数の前記プレートが、前記一連の触媒材料を形成するように提供される、請求項28に記載の触媒反応器。
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