JP6078045B2 - 炭素酸化物を還元することによる固体炭素の製造方法 - Google Patents
炭素酸化物を還元することによる固体炭素の製造方法 Download PDFInfo
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- JP6078045B2 JP6078045B2 JP2014241250A JP2014241250A JP6078045B2 JP 6078045 B2 JP6078045 B2 JP 6078045B2 JP 2014241250 A JP2014241250 A JP 2014241250A JP 2014241250 A JP2014241250 A JP 2014241250A JP 6078045 B2 JP6078045 B2 JP 6078045B2
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Classifications
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- C01B32/00—Carbon; Compounds thereof
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Description
本件特許出願は、2009年4月17日付で出願された、「炭素酸化物を還元することによる固体炭素の製造方法(Method for Producing Solid Carbon by Reducing Carbon Oxides)」と題する、米国仮特許出願第61170199号に基く優先権を主張するものである。この米国仮特許出願の開示事項を、参照することによりここに組入れる。
この方法の改良によって生成されるはずの様々な形状の固体炭素に関する開示、又はこれら反応の主な望ましい生成物としての固体炭素に関する開示は、これまで全く見られない。
2CO(g) ←→ C(s) + CO2(g), ΔH = -169 kJ/モル(固体炭素)
本発明の方法は、少なくとも以下の3つの点において、該ブドゥアード反応とは異なっている:即ち、i) 一酸化炭素はこの方法にとって不要であるが、これは炭素源として利用することができる点;ii) 該一酸化炭素を還元して固体炭素及び水とするのに別の還元剤が使用される点;及びiii) 二酸化炭素が該反応の生成物ではない点。
・ボッシュ反応を利用する二酸化炭素還元装置(A carbon dioxide reduction unit using Bosch reaction);
・水の製造方法、ボッシュ及びサバティエ反応を含むISSに関して考慮さるべき方法の概観(Methods of Water Production a survey of methods considered for the ISS including Bosch and Sabatier reactions), オレゴン州立大学(Oregon State University);・CO2還元法の比較―ボッシュ及びサバティエ、SAEインターナショナル(Comparison of CO2 Reduction Process - Bosch and Sabatier, SAE International)、1985年7月、文書番号(Document Number) 851343;
・Bunnel, C.T. Boyda, R.B. & Lee, M.G., ボッシュのCO2還元法の最適化、SAE技術論文シリーズ(Optimization of the Bosch CO2 Reduction Process, SAE Technical Paper Series) No. 911451, 環境システムに関する第21回国際会議において提示された(presented 21st International Conference on Environmental Systems)、CA州、サンフランシスコ(San Francisco, CA), 1991年7月15-18;
・Davenport, R. J.; Schubert, F. H.; Shumar, J. W.; Steenson, T. S., メタン-二酸化炭素分解反応の評価及びキャラクタリゼーション(Evaluation and characterization of the methane-carbon dioxide decomposition reaction), 受入番号(Accession Number): 75N27071;
・Noyes, G.P., 宇宙船ECLSSに関する二酸化炭素の還元法:包括的論評(Carbon Dioxide Reduction Processes for Spacecraft ECLSS: A Comprehensive Review), SAE技術論文シリーズ(SAE Technical Paper Series)No. 881042, 自動車技術協会(Society of Automotive Engineers), PA州、ウォーレンダール(Warrendale, PA), 1988;
・Arlow, M. & Traxler, G., 将来の欧州宇宙計画のための、CO2処理及びO2再生利用システム選別法(CO2 Processing and O2 Reclamation System Selection Process for Future European Space Programmes), SAE技術論文シリーズ(SAE Technical Paper Series)No. 891548, 自動車技術協会(Society of Automotive Engineers), PA州、ウォーレンダール(Warrendale, PA), 1989;
・ボッシュのCO2還元法の最適化(Optimization of the Bosch CO2 Reduction Process), SAEインターナショナル(SAE International), 1991年7月, 文書番号(Document Number) 911451;
・Garmirian, J.E.,「コバルト及びニッケル触媒を用いた、ボッシュ法における炭素の堆積(Carbon Deposition in a Bosch Process Using a Cobalt and Nickel Catalyst)」, 学位論文, MIT, 1980年3月;
・Garmirian, J.E., Reid, R.C.,「鉄以外の触媒を用いた、ボッシュ法における炭素の堆積(Carbon Deposition in a Bosch Process Using Catalysts Other than Iron)」, 年報(Annual Report), NASA-AMES認可番号No. NGR22-009-723, 1978年7月1日;
・Garmirian, J.E., Manning, M.P., Reid, R.C.,「ボッシュ反応器におけるニッケル及びコバルト触媒の利用(The use of nickel and cobalt catalysts in a Bosch reactor)」, 1980;
・Heppner, D. B.; Hallick, T. M.; Clark, D. C.; Quattrone, P. D., ボッシュ―もう一つのCO2還元技術(Bosch - An alternate CO2 reduction technology), NTRS受入番号(Accession Number): 80A15256;
・Heppner, D. B.; Wynveen, R. A.; Schubert, F. H., RLSE実験のための原型ボッシュCO2還元サブシステム(Prototype Bosch CO2 reduction subsystem for the RLSE experiment), NTRS受入番号(Accession Number): 78N15693;
・Heppner, D. B.; Hallick, T. M.; Schubert, F. H., ボッシュCOサブ2還元サブシステムの性能のキャラクタリゼーション(Performance characterization of a Bosch CO sub 2 reduction subsystem), NTRS受入番号(Accession Number): 80N22987;
・Holmes, R. F.; King, C. D.; Keller, E. E., ボッシュCO2還元システムの開発(Bosch CO2 reduction system development), NTRS受入番号(Accession Number): 76N22910;
・Holmes, R. F.; Keller, E. E.; King, C. D., ボッシュ反応及び発泡性触媒カートリッジを用いた、二酸化炭素還元装置(A carbon dioxide reduction unit using Bosch reaction and expendable catalyst cartridges), ゼネラルダイナミック社(General Dynamics Corporation), 1970, NTRS受入番号(Accession Number): 71N12333;
・Holmes, R. F.,CO2還元のためのボッシュ反応の自動化(Automation of Bosch reaction for CO2 reduction), NTRS受入番号(Accession Number): 72B10666;
・Holmes, R. F.; Keller, E. E.; King, C. D., ボッシュCO2還元装置の研究並びに開発(Bosch CO2 reduction unit research and development), NTRS受入番号(Accession Number): 72A39167;
・Holmes, R. F.; King, C. D.; Keller, E. E., ボッシュCO2還元システム開発(Bosch CO2 reduction system development), NTRS受入番号(Accession Number): 75N33726;
・King, C. D.; Holmes, R. F., 円熟したボッシュCO2還元技術(A mature Bosch CO2 reduction technology), NTRS受入番号(Accession Number): 77A19465;
・Kusner, R.E.,「鉄触媒を用いた逆水-ガスシフト反応の速度論(Kinetics of the Iron Catalyzed Reverse Water-Gas Shift Reaction)」, PhD論文, ケースインスティチュートオブテクノロジー(Case Institute of Technology), オハイオ州(Ohio)(1962);
・Isakson, W.E., Snacier, K.M., Wentrcek, P.R., Wise, H., Wood, B.J.「触媒の硫黄毒(Sulfur Poisoning of Catalysts)」, SRI, US ERDAに関連, 契約番号(Contract No.)E(36-2)-0060, SRIプロジェクト(Project)4387, 1977;
・Manning, M.P., Garmirian, J.E., Reid, R.C., 「ニッケル及びコバルト触媒を用いた、炭素堆積の研究(Carbon Deposition Studies Using Nickel and Cobalt Catalysts)」, Ind. Eng. Chem. Process Des. Dev., 1982, 21, 404-409;
・Manning, M. P.; Reid, R. C., ボッシュ法による二酸化炭素の還元(Carbon dioxide reduction by the Bosch process), NTRS受入番号(Accession Number): 75A40882;
・Manning, M.P., 「ボッシュ法の検討(An Investigation of the Bosch Process)」, MIT学位論文(Dissertation)(1976);
・Manning, M. P.; Reid, R. C.; Sophonpanich, C., ルテニウム及びルテニウム-鉄合金触媒を用いた、ボッシュ法における炭素の堆積(Carbon deposition in the Bosch process with ruthenium and ruthenium-iron alloy catalysts), NTRS受入番号(Accession Number): 83N28204;
・Meissner, H. P.; Reid, R. C., ボッシュ法(The Bosch process), NTRS受入番号(Accession Number): 72A39168;
・Minemoto, M., Etoh, T., Ida, H., Hatano, S., Kamishima, N., and Kita, Y., 宇宙ステーション用の空気再生システムに関する研究(Study of Air Revitalization System for Space Station), SAE技術論文シリーズ(SAE Technical Paper Series) No. 891576, 自動車技術協会(Society of Automotive Engineers), PA州、ウォーレンダール(Warrendale, PA), 1989;
・Otsuji, K., Hanabusa, O., Sawada, T., Satoh, S., and Minemoto, M., 「ボッシュ及びサバチエCO2還元法の実験的研究(An Experimental Study of the Bosch and the Sabatier CO2 Reduction Processes)」, SAE技術論文シリーズ(SAE Technical Paper Series) No. 871517, 環境システムに関する第17回学会間会議で提示された(presented 17th Intersociety Conference on Environmental Systems), WA州、シアトル(Seattle, WA), 1987年7月;
・Ruston, W.R., Warzee, M., Hennaut, J. Waty, J., 「550℃における鉄触媒上での一酸化炭素の接触的分解の固体反応生成物(The Solid Reaction Products of the Catalytic Decomposition of Carbon Monoxide on Iron at 550C)」, Carbon, 7, 47 (1969);
・Ruston, W.R., Warzee, M., Hennaut, J., Waty, J., 「金属触媒上での一酸化炭素からの炭素堆積物の成長に係る基本的研究(Basic Studies on the Growth of Carbon Deposition from Carbon Monoxide on a Metal Catalyst)」, D.P.報告(D.P. Report) 394, 原子エネルギーの確立(Atomic Energy Establishment), ウインフリス(Winfrith)(1966);・Sacco, A., 「鉄、炭化鉄、及び酸化鉄上での、二酸化炭素、一酸化炭素、メタン、水素、及び水の反応に関する検討(An Investigation of the Reactions of Carbon Dioxide, Carbon Monoxide, Methane, Hydrogen, and Water Over Iron, Iron Carbides, and Iron Oxide)」, PhD論文(PhD Thesis), MIT (1977);
・Sacco, A., 「鉄、炭化鉄、及び酸化鉄上での、二酸化炭素、一酸化炭素、メタン、水素、及び水の反応に関する検討(An Investigation of the Reactions of Carbon Dioxide, Carbon Monoxide, Methane, Hydrogen, and Water over Iron, Iron Carbides, and Iron Oxide)」, PhD論文(PhD Thesis), MIT (1977)
・Sophonpanich, C., Manning, M.P., and Reid, R.C., 「ルテニウム及びルテニウム-テル合金触媒の、ボッシュ法触媒としての利用(Utilization of Ruthenium and Ruthenium-Iron Alloys as Bosch Process Catalysts)」, SAE技術論文シリーズ(SAE Technical Paper Series) No. 820875, 自動車技術協会(Society of Automotive Engineers), PA州、ウォーレンダール(Warrendale, PA), 1982;
・Schubert, F. H.; Clark, D. C.; Quattrone, P. D., 電気化学的に減極されたCO2濃縮機/EDC及びボッシュCO2還元サブシステム/BRS/の包括的テスト(Integrated testing of an electrochemical depolarized CO2 concentrator /EDC/ and a Bosch CO2 reduction subsystem /BRS/), NTRS受入番号(Accession Number): 77A19483;
・Schubert, F. H.; Wynveen, R. A.; Hallick, T. M., 電気化学的に減極されたCO2濃縮機とボッシュCO2還元サブシステムの一体化(Integration of the electrochemical depolorized CO2 concentrator with the Bosch CO2 reduction subsystem), NTRS受入番号(Accession Number): 76N22907;
・Wagner, Robert C.; Carrasquillo, Robyn; Edwards, James; Holmes, Roy,宇宙ステーション用途用のボッシュCO2還元技術の円熟(Maturity of the Bosch CO2 reduction technology for Space Station application), NTRS受入番号(Accession Number): 89A27804, SAE技術論文シリーズ(SAE Technical Paper Series) No. 88099;
・地球温暖化及び温室ガス:温室ガス効果の改善のための一体化された技術(Global Warming & Greenhouse Gases: Integrated-Technologies Remediation of Greenhouse Gas Effects)
・Walker, P.L., Rakszawski, J.F.及びImperial, G.R.,「鉄触媒上での一酸化炭素-水素混合物からの炭素生成、生成された炭素の諸特性(Carbon Formation from Carbon Monoxide-Hydrogen Mixtures over Iron Catalysts. Properties of Carbon Formed)」, J. Phys. Chem., 73, 133, (1959)。
見掛け上は、該所望のカーボンナノチューブ径の約1.2〜1.6倍の寸法を持つ触媒の使用が、単一壁カーボンナノチューブの生成を結果する。該触媒は、所望の寸法を持つ触媒ナノ粒子の形状、又は固体触媒、例えばステンレススチール処方の領域内の形状であってもよく、後者において該スチールの粒径は、所望のCNTの径に対して特徴的な寸法にある。触媒ナノ粒子は、エアゾール溶液の注入により該反応ゾーン中又はその近傍にて生成することができ、ここで各エアゾール液滴中の触媒プリカーサの濃度は、(存在する場合には)溶質が蒸発し、かつ該触媒プリカーサが分解して、触媒ナノ粒子を生成する際に、所望のナノ粒子サイズを与えるのに必要とされるような値である。典型的には、該温度を、該触媒粒子のサイズの減少に応じて下げる必要がある。該触媒及び該反応条件を選択することにより、比較的特定された形状を持つ炭素を与えるように、該工程を調節することができる。
CO2 + 2H2 ←→ C(s) + H2O
その際に、固体炭素(C(s))1gにつき約2.3×103Jなる熱を放出する。この反応は、該固体炭素が水及び二酸化炭素により酸化される反応(酸素シフト反応)と可逆的であり、従って固体炭素を製造するためには約450℃を越える反応温度が必要とされるが、この温度が高過ぎると、逆反応が進み、また全体としての反応速度は、遅くなる(該反応の平衡が左側にシフトする)。
・熱分解グラファイトを含むグラファイト;
・グラフェン;
・カーボンブラック;
・繊維状炭素;
・バッキーボール、単一壁カーボンナノチューブ、及び多重壁カーボンナノチューブを含むバックミンスターフラーレン。
CO2 + CH4 ←→ 2C(s) + 2H2O
ここで、該発熱反応中に、決定されていない量の熱の放出を伴う。
本発明の方法によれば、該固体炭素製品の形態は、該反応条件により、また該触媒を変更することにより、さらには該触媒を該水素及び炭素酸化物と接触させる方法によって調節することができる。一態様において、該触媒は以下のようにして製造することができる。
即ち、触媒プリカーサ化合物、例えばフェロセン又は幾つかの他のメタロセン、あるいは幾つかの他の金属-含有プリカーサ、例えばペンタカルボニル鉄の化学的な反応及び該反応生成物の凝集を通して、該反応ガス中に同伴させ、あるいは該反応ゾーン内の表面上に堆積されたナノ粒子として該触媒を生成することによって、該反応ゾーン内で製造することができる。
例えば、スチールウール、スチールプレート、及びスチールショット(サンドブラスチングにおいて使用されている如きもの)は、満足な成長速度及び均一な品質を与えた。スチール上で成長したカーボンナノチューブの形態は、該スチールの化学的性質及び該スチールを処理した方法に依存する。これは、現時点において完全に理解されていない多くのファクタの何れかによるものと思われるが、これは該スチールの粒度及び該金属内の境界の形状と関連しているものと考えられ、ここでこれら特徴の中の該特性サイズは、このようなスチールサンプルの表面上で成長したカーボンナノチューブ群の特徴的な径を制御する。当業者は、該スチールに関する正確な化学的性質を決定するための適当な実験及び所望のカーボンナノチューブの形態及び制御された径を実現するための該スチールに対する処理方法を、容易に見出すであろう。
・エアゾール反応器:ここでは、該触媒は、触媒プリカーサから気相中で生成され、あるいは該触媒は予備成形され、かつ特定のサイズ分布につき選別され、液体又はキャリヤ溶液と混合され、次いで該反応器に、(例えば、静電噴霧により)噴霧される。次いで、該炭素製品の成長段階及びその後の該製品の該反応ゾーンからの搬送段階に対して、該触媒は、該気相中に分散された状態を維持し、あるいは該反応ゾーン内の固体表面上に堆積された状態を維持することができる;
・流動床反応器:ここでは、該触媒又は触媒-被覆粒子は、該反応器に導入され、また該固体炭素は、該粒子の表面上で成長する。次いで、該固体炭素は、該反応機内で洗い分けされ、該反応ガス中に同伴された状態で該反応器から運び出されるか、あるいは該触媒粒子は回収され、また該固体炭素は該触媒粒子表面から取出される;
・バッチ反応器:ここでは、該触媒は固定された固体表面(例えば、スチールシート、又はスチールウール)であるか、あるいは固定された固体表面上に配置(例えば、不活性基板上に堆積された触媒ナノ粒子)されており、該触媒上で該固体炭素が成長し、また該触媒及び固体炭素は、定期的に該反応器から取出される;
・連続反応器:ここでは、固体触媒又は固体基板上に配置された触媒は、該流動するガス流を介して移動し、生成する固体炭素製品は回収され、該基板の固体表面が調製され、また該反応器に再度導入される。該固体基板は、該触媒物質(例えば、ステンレススチール形状にある)、又は該触媒が配置されている表面であり得る。該固体表面の適当な形状は、ウエハ、シート、シリンダー、又は球を含む。
また、1又はそれ以上の物質を、該反応ゾーンに導入して、該固体炭素製品への組込みを通して、あるいは該固体炭素製品上での表面堆積によって、該所望の固体炭素製品の物性を改善することができる。
これは、該触媒を取巻く炭素シェルによるものと考えられ、あるいはこれは、該触媒粒度と、該触媒から成長した該カーボンナノチューブの粒度との間の基本的な関係を示すものであると考えることができ、あるいはこれは、ある他のファクタ又はさらには偶然によるものと考えることができる。何れにしろ、該カーボンナノチューブのサイズを制御するための一つの方法は、触媒粒度の制御を通して行うものであると思われ、該触媒の粒度は、該所望のナノチューブの粒度よりも幾分大きい。
・二酸化炭素(CO2)、研究グレードのもの、プラックスエアー(PraxAir)社製;
・メタン(CH4)、研究グレードのもの、プラックスエアー(PraxAir)社製;
・窒素ガス(N2)、標準グレードのもの、プラックスエアー(PraxAir)社製;
・ヘリウム(He)、研究グレードのもの、エアーリキッド(Air Liquide)社製;
・水素ガス(H2)、研究グレードのもの、プラックスエアー(PraxAir)社製。
図1に示した如く、これらのガスを、ガス供給源6から混合バルブ7までパイプ輸送し、該バルブにおいて、該ガスを計量し、かつ管状炉1及び2に分配した。これらのガスは、該管状炉1及び2を介して冷却されたコンデンサ4(露点=約3.33℃(38゜F))まで流動し、次いで圧縮器3を通り、また該管状炉1のヘッド端部に戻された。特定の実験が、不活性ガスによる該炉のパージを要する場合には、真空ポンプ5を使用して、該実験装置の排気を行った。
流量は、製造設備の最適な設計及び動作において重要であるが、ここに報告したテストにおいては格別重要である訳ではない。というのは、該実験装置の容積が、該触媒及び生成する固体炭素製品の容積よりも著しく大きかったからである。当業者は、具体的な製造計画に対する最適な流量を決定するための適当なテストに、容易に思い至るであろう。
実施例1:
該真空ポンプ5を始動させ、該実験装置を5分間に渡りパージするのに、ヘリウムを使用した。5分後に、該真空ポンプ5を停止させ、上記圧縮器3を稼働させ、上記冷却したコンデンサ4を始動させ、またヘリウムガスを、該装置内の圧力が680トールをなるまで流し続けた。この時点において、該ガスの流動を停止させた。次いで、該炉1を始動させた。
図5は、図4に示したCNTの元素分析結果を示すものであり、この図は、該CNTが少量の鉄及び酸素を構成成分として含む炭素であることを示しており、これは、恐らく該CNTの成長先端部に包埋されている該触媒粒子のよるものである。
実施例2:
実施例3:
実施例4:
実施例5:
該316ステンレススチールワイヤを、炉1の出口近傍に配置した。該炉1を作動させ、かつ冷却されたコンデンサ4を始動させた。真空ポンプ5を始動させ、また混合バルブ7によって制御されるガス供給源6からの、二酸化炭素と水素との化学量論的な混合物を含む反応ガスを、該実験装置を5分間に渡りパージするのに使用した。5分後、該真空ポンプ5を停止させ、圧縮器3を始動させ、かつ該反応ガス混合物を、該実験装置のゲージ圧が589トールとなるまで流し続け、該所定圧力に達した時点において、該反応ガスの供給を止めた。
該実験装置を2時間に渡り稼働させ、その後該炉1を停止させ、該真空ポンプ5を始動させ、かつ該実験装置を、5分間に渡り、混合バルブ7によって制御されるガス供給源6からのヘリウムガスでパージした。次いで、該真空ポンプ5を停止させ、かつ該ヘリウムガスを、該実験装置におけるゲージ圧が700トールとなるまで流し続けた。次いで、該炉1を放冷させた。
実施例6:
[1] 固体炭素製品の製造方法であって、以下の諸工程:
炭素酸化物ガス流を供給する工程;
還元剤ガス流を供給する工程;
触媒を準備する工程;
該炭素酸化物と還元剤ガス流とを混合して、反応ガス混合物を生成する工程;
該反応ガス混合物を、触媒の存在下にて、所定の反応条件下で、反応ゾーンに導入する
工程;及び
該固体触媒の存在下にて、該反応混合物を反応させて、所望の形態を持つ固体炭素製品
を得る工程、
を含むことを特徴とする、前記固体炭素製品の製造方法。
[2] さらに、前記得られる反応ガスを、制御された冷却処理に付して、さらに反応時間、二次的な堆積物の生成、アニール及びランプダウンを制御する工程をも含む、[1]記載の方法。
[3] さらに、前記分離されたガス混合物を、凝縮ゾーンに通して、該ガス混合物から水分を除去する工程、及び得られる任意の非-凝縮性ガスの一部を、前記反応ガス又は前記触媒プリカーサ流に再循環する工程をも含む、[1] 記載の方法。
[4] 前記反応が、約450℃〜1,500℃なる範囲の温度にて起る、[1]記載の方法。
[5] さらに、前記炭素酸化物及び前記還元ガス流を、第一の予め定められた温度まで予備加熱する工程をも含む、[1]記載の方法。
[6] さらに、反応ゾーンを、第二の予め定められた温度まで予備加熱する工程をも含む、[1]記載の方法。
[7] さらに、前記反応ゾーンにおける、温度、圧力及び前記反応ガスの滞留時間を含む前記反応条件を維持する工程及び反応ガス流を、予め定められた期間に渡り、該反応ゾーンを介して流し続けて、所望の形態を持つ固体炭素製品を生成する工程をも含む、[1]記載の方法。
[8] さらに、前記ガス混合物及び固体炭素製品を、前記反応ゾーンから冷却ゾーンに移送する工程、次いで該冷却ゾーンから分離工程に移送して、該ガス混合物から該固体炭素製品を分離する工程をも含む、[1]記載の方法。
[9] 前記触媒が、所定の組成及び形状を持つ鋼を含み、あるいは該所定の組成及び形状を持つ該鋼の酸化物を還元することにより製造される、[1]記載の方法。
[10] 前記還元剤ガス流が、水素又は炭化水素又はこれらの混合物を含む、[1]記載の方法。
[11] 前記触媒が、周期律表の第VI族金属、第VIII族金属、及びこれらの混合物からなる群から選択される金属である、[1]記載の方法。
[12] 前記炭素酸化物ガス流が二酸化炭素を主成分とするものである、[1]記載の方法。
[13] 前記炭素酸化物ガス流が一酸化炭素を主成分とするものである、[1]記載の方法。
[14] 前記炭素酸化物ガス流が、ガス混合物、例えば大気ガス、燃焼ガス、プロセス排ガス、ポルトランドセメント製造過程由来の排ガス、及び油井ガスから分離される、[1]記載の方法。
[15] 前記炭素酸化物ガス流が、ガス混合物、例えば燃焼ガス、プロセス排ガス、ポルトランドセメント製造過程由来の排ガス、及び油井ガス又はその分離画分の形状にある、[1]記載の方法。
[16] 前記還元剤ガス流が、水素ガスを含む、[1]記載の方法。
[17] 前記還元剤ガス流が、炭化水素ガスを含む、[1]記載の方法。
[18] 前記炭化水素が、天然ガスを含む、[17]記載の方法。
[19] 前記炭化水素が、合成ガスを含む、[17]記載の方法。
[20] 前記炭化水素が、メタンを含む、[17]記載の方法。
[21] 前記還元剤ガス流が、任意の利用可能な炭素酸化物の還元に必要とされる化学量論比を大幅に越える量で供給される、[1]記載の方法。
[22] 前記還元剤ガス流が、任意の利用可能な炭素酸化物の還元に必要とされる化学量論比にほぼ等しい比にて存在する、[1]記載の方法。
[23] 前記還元剤ガス流が、任意の利用可能な炭素酸化物の還元に必要とされる化学量論比よりも著しく低い量で存在する、[1]記載の方法。
[24] 前記触媒が、予め決められたキャリヤガスと共に前記反応ゾーンに供給される、[1]記載の方法。
[25] 前記触媒が触媒プリカーサとして前記反応ゾーンに供給される、[1]記載の方法。
[26] 前記触媒が、周期律表の第VI族金属、第VII族金属、及びこれらの混合物からなる群から選択される遷移金属原子を含む、[1]記載の方法。
[27] 前記触媒が、酸化ベリリウム、酸化マグネシウム、酸化カルシウム、酸化ストロンチウム及び酸化バリウムからなる群から選択される、酸化金属化合物を含む、[1]記載の方法。
[28] 前記触媒が、酸化鉄を含む、[1]記載の方法。
[29] 前記触媒プリカーサが、周期律表の第VI族金属、第VII族金属、及びこれらの混合物からなる群から選択される金属の化合物である、[25]記載の方法。
[30] 前記化合物が、金属カルボニルである、[29]記載の方法。
[31] 前記化合物が、金属酸化物である、[29]記載の方法。
[32] 前記化合物が、メタロセンである、[29]記載の方法。
[33] 前記反応ゾーンが、流動床反応器である、[1]記載の方法。
[34] 前記キャリヤガスが、1種又はそれ以上の、不活性ガス及び炭素酸化物との混合物を含む、[24]記載の方法。
[35] 前記反応混合物における前記触媒プリカーサの濃度が、約1ppm〜約100ppmなる範囲内にある、[25]記載の方法。
[36] 前記触媒プリカーサが、該触媒プリカーサの分解温度以下の温度にて供給される、[1]記載の方法。
[37] 前記反応混合物に、触媒促進剤を添加する、[1]記載の方法。
[38] 前記触媒促進剤が、チオフェン、H2S、複素環式スルフィド、無機スルフィド、揮発性鉛、ビスマス化合物及びこれらの混合物からなる群から選択される、[37]記載の方法。
[39] さらに、核形成剤を供給して、前記触媒プリカーサからの前記触媒の形成を容易にする工程をも含む、[25]記載の方法。
[40] 前記核形成剤が、ガス状金属-含有化合物である、[39]記載の方法。
[41] 前記ガス状金属-含有化合物が、Ni(CO)4、W(CO)6、Mo(CO)6及びこれらの混合物からなる群から選択される、[40]記載の方法。
[42] 前記核形成剤が、レーザー光フォトンである、[39]記載の方法。
[43] さらに、前記反応ゾーンにおいて生成されたカーボンナノチューブを、これに引続く成長及びアニールゾーンに通す工程をも含む、[1]記載の方法。
[44] 前記反応ゾーンが、エアゾール反応器であり、そこには前記触媒をエアゾールスプレーとして導入することができる、[1]記載の方法。
[45] 前記触媒が、前記成長したカーボンナノチューブの径を制御するように選択される粒径を持つ、予備成形された粒子の形状にある、[44]記載の方法。
[46] 前記触媒が、1又はそれ以上の触媒プリカーサの形状にあり、該触媒プリカーサが、予め定められた反応温度に暴露された場合に、分解して該触媒を生成する、[44]記載の方法。
[47] 前記触媒が、前記エアゾール内に留まっており、かつ前記固体炭素製品が、前記反応ゾーンを通過する触媒粒子上で成長する、[44]記載の方法。
[48] 前記触媒が、前記エアゾールから、前記反応ゾーン内の1又はそれ以上の表面上に堆積される、[44]記載の方法。
[49] 前記反応ガス、触媒、及び反応条件の組合せが、ピローの形態を持つカーボンナノチューブクラスターの生成をもたらす、[1]記載の方法。
Claims (17)
- 固体炭素の製造方法であって、
炭素酸化物を含む第一のガス流と還元剤を含む第二のガス流とを混合して、反応ガス混合物を生成する工程;
該反応ガス混合物を反応ゾーンに供給する工程;
該反応ゾーンにおいて、炭素酸化物と還元剤を触媒の存在下で反応させて、水と固体炭素を生成する工程;
金属イオンを含む水を反応ゾーンに注入する工程;及び
該水を凝縮し、該水から潜熱を回収する工程
を含むことを特徴とする、前記固体炭素の製造方法。 - 反応ゾーンにおいて、炭素酸化物と還元剤を触媒の存在下で反応させて、水と固体炭素を生成する工程が、カーボンナノチューブの直径の1.3〜1.6倍大きい粒径を有する触媒から、カーボンナノチューブを形成する工程を含む、請求項1記載の方法。
- 水を凝縮する工程が、反応ガス混合物を反応ゾーンから凝縮ゾーンに循環して、該反応ガス混合物から水を除去し、乾燥再循環ガス混合物を生成する工程、及び該乾燥再循環ガス混合物を反応ゾーンに再循環する工程をも含む、請求項1又は2記載の方法。
- さらに、乾燥再循環ガス混合物と反応ガス混合物とを混合する工程を含む、請求項3記載の方法。
- さらに、固体炭素をエタノール中に分散し、相互に噛み合った固体炭素材料を生成する工程を含む、請求項1〜4のいずれか1項に記載の方法。
- 炭素酸化物を含む第一のガス流と還元剤を含む第二のガス流とを混合する工程が、炭素酸化物を含有する燃焼ガスを含む第一のガス流と第二のガス流とを混合する工程を含む、請求項1〜5のいずれか1項に記載の方法。
- 反応ゾーンにおいて、炭素酸化物と還元剤を触媒の存在下で反応させて、水と固体炭素を生成する工程が、
反応ガス混合物を流動する工程;
該流動している反応ガス混合物を介して固体触媒を移動する工程;
固体炭素を採取する工程;及び
前記固体触媒を反応ゾーンに再導入する工程
を含む、請求項1〜6のいずれか1項に記載の方法。 - さらに、
反応ゾーンへの反応ガス混合物の流入を停止する工程、
反応ゾーンから反応ガス混合物を取り出す工程、
反応ゾーンに不活性ガスを供給する工程、
内部に固体炭素を含む反応ゾーンを冷却する工程、及び
反応ゾーンから固体炭素を取り出す工程
を含む、請求項2〜7のいずれか1項に記載の方法。 - さらに、
固体炭素の少なくとも一部を反応ガスゾーンから取り出す工程;
ヘリウムのパージにより、該固体炭素の少なくとも一部との接触から、反応ガス混合物を分離する工程;及び
前記固体炭素の少なくとも一部を冷却する工程
を含む、請求項1〜7のいずれか1項に記載の方法。 - 反応ゾーンにおいて、炭素酸化物と還元剤を触媒の存在下で反応させて、水と固体炭素を生成する工程が、炭素酸化物と還元剤を、軟鋼を含む触媒の存在下で反応させて、少なくとも100 nmの直径を示す固体炭素を生成する工程を含む、請求項1〜9のいずれか1項に記載の方法。
- 反応ゾーンにおいて、炭素酸化物と還元剤を触媒の存在下で反応させて、水と固体炭素を生成する工程が、炭素酸化物と還元剤を、ステンレススチールを含む触媒の存在下で反応させて、少なくとも20 nmの直径を示す固体炭素を生成する工程を含む、請求項1〜9のいずれか1項に記載の方法。
- 反応ゾーンにおいて、炭素酸化物と還元剤を反応させる工程に先立って、ヘリウムの存在下で触媒を加熱する工程を更に含む、請求項1〜11のいずれか1項に記載の方法。
- さらに、金属カルボニル、金属酸化物、及びメタロセンの少なくとも一種を含む触媒プリカーサを反応ゾーンに供給する工程を含む、請求項1〜12のいずれか1項に記載の方法。
- 固体炭素の少なくとも一部を形成した後、触媒プリカーサを反応ゾーンに導入する工程を含む、請求項13記載の方法。
- 反応ガス混合物を含む反応ゾーンの触媒プリカーサの濃度が、1〜100 ppmの範囲にある、請求項13記載の方法。
- さらに、触媒の領域をマスクする工程を含む、請求項1〜15のいずれか1項に記載の方法。
- さらに、チオフェン、硫化水素、複素環式スルフィド、無機スルフィド、揮発性鉛、ビスマス、アンモニア、窒素、及び余分の水素から選択される少なくとも一種を添加する工程を含む、請求項1〜16のいずれか1項に記載の方法。
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