JP2013111496A - 金属担持用担体、金属担持触媒、メタネーション反応装置及びこれらに関する方法 - Google Patents
金属担持用担体、金属担持触媒、メタネーション反応装置及びこれらに関する方法 Download PDFInfo
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- JP2013111496A JP2013111496A JP2011257842A JP2011257842A JP2013111496A JP 2013111496 A JP2013111496 A JP 2013111496A JP 2011257842 A JP2011257842 A JP 2011257842A JP 2011257842 A JP2011257842 A JP 2011257842A JP 2013111496 A JP2013111496 A JP 2013111496A
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- metal
- carbon monoxide
- methanation
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- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 145
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- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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Abstract
【解決手段】本発明に係る金属担持用担体は、有機物と金属とを含む原料の炭素化により得られる炭素化材料からなり、一酸化炭素のメタネーション反応触媒活性を示す金属を担持するための担体である。本発明に係る金属担持触媒は、有機物と金属とを含む原料の炭素化により得られる炭素化材料からなる担体と、前記担体に担持された、一酸化炭素のメタネーション反応触媒活性を示す金属と、を有する。
【選択図】図6
Description
まず、炭素化の対象となる原料を調製した。すなわち、フェノール樹脂(紡糸用、群栄化学工業株式会社製)と、コバルトフタロシアニン(純度90%、東京化成工業株式会社製)とを、当該フェノール樹脂に対するコバルト(Co)の重量割合が3wt%となるようにアセトン中で混合した。得られた混合物を超音波で30分撹拌し、エバポレーターを用いて溶媒を除去した。その後、混合物を70℃で 一晩減圧乾燥し、原料を得た。
硝酸ニッケル(Ni(NO3)2・6H2O)水溶液(特級試薬、和光純薬工業株式会社製)を用いた含浸法により、上述のようにして製造したNSCにニッケル(Ni)を担持した。
担持されたNiの状態の観察、及びNi粒子径の測定のために、透過型電子顕微鏡(JEM−2010、日本電子株式会社製)(TEM)を用い、金属担持触媒を観察した。すなわち、金属担持触媒1mgを、5mLのメタノールとともにバイアルに入れ、超音波で10分間撹拌することで、当該金属担持触媒をメタノール中に分散させた。その後、この金属担持触媒を含む溶液2μLを銅製のマイクログリッドに載せ、当該グリッドをTEM内に入れ、加速電圧200kVで観察した。
担持されたNiの状態の観察、及びNi結晶子径の測定のために、金属担持触媒のX線回折(XRD)を行った。すなわち、金属担持触媒をガラス製のホルダの上に均一に分散させて載せ、XRD装置(XRD−6100、株式会社島津製作所製)を用いて、CuKα、32kV、20mA、走査範囲5〜90°、走査ステップ0.01°の条件にてXRD測定を行った。Niの結晶子径は、52.0°付近のNi(220)のピークを用いて計算した。
昇温脱離スペクトル装置(マルチタスクTPD、日本ベル株式会社製)を用いて、金属担持触媒を使用した一酸化炭素のメタネーション反応を行い、当該金属担持触媒のメタネーション触媒活性を評価した。
金属担持触媒に担持されたNiの電子状態を把握するため、Ni/NSC、Ni/XC及びNi/LYについて、X線光電子分光(XPS)法を行った。すなわち、XPS装置(AXIS NOVA、株式会社島津製作所製)を用いて、金属担持触媒を、アルミ片に貼ったカーボンテープにのせ、当該装置内へ導入した。そして、X線源にAlKαを使用し、15kV、10mAの条件でXPS測定を行った。
昇温脱離スペクトル装置(マルチタスクTPD、日本ベル株式会社製)を用いて、Ni/NSC及びNi/XCについて、CO及びH2の昇温脱離法(TPD)を実施した。なお、Ni/LYは、LYの熱分解温度が約600℃であるため、正確なスペクトルを得ることが困難であった。
上述のようにして得られた結果に基づき、金属担持触媒からのH2の脱離量及びCOの脱離量をそれぞれ求めた。すなわち、H2又はCOの脱離量が理論的に求められる標準物質(MgH2又はCaC2O4・H2O)を使用したH2昇温脱離法又はCO昇温脱離法により、H2又はCOのピーク面積と、H2又はCOの脱離量との相関関係を示す検量線を作成した。
Claims (17)
- 有機物と金属とを含む原料の炭素化により得られる炭素化材料からなり、
一酸化炭素のメタネーション反応触媒活性を示す金属を担持するための担体である
ことを特徴とする金属担持用担体。 - 前記金属は、Ni、Ru、Rh、Pd、Pt、Ir、Cu、W、Cs、K、Na、Co、Fe、Ca、Mg、Ba、Sr及びLiからなる群より選択される1種以上である
ことを特徴とする請求項1に記載の金属担持用担体。 - 前記金属は、Niである
ことを特徴とする請求項2に記載の金属担持用担体。 - Niを担持した状態において、
Niの2p軌道の電子状態をXPS測定して得られる、850eV以上、860eV以下のピーク面積に対する、853.5eV超、860eV以下のピーク面積の比率が0.5以上であり、
CO昇温脱離法による40℃〜800℃でのCO脱離量に対する、H2昇温脱離法による40℃〜800℃でのH2脱離量のモル比率が0.3以上である
ことを特徴とする請求項1乃至3のいずれかに記載の金属担持用担体。 - 有機物と金属とを含む原料の炭素化により得られる炭素化材料からなる担体と、
前記担体に担持された、一酸化炭素のメタネーション反応触媒活性を示す金属と、
を有する
ことを特徴とする金属担持触媒。 - 前記金属は、Ni、Ru、Rh、Pd、Pt、Ir、Cu、W、Cs、K、Na、Co、Fe、Ca、Mg、Ba、Sr及びLiからなる群より選択される1種以上である
ことを特徴とする請求項5に記載の金属担持触媒。 - 前記金属は、Niである
ことを特徴とする請求項6に記載の金属担持触媒。 - Niの2p軌道の電子状態をXPS測定して得られる、850eV以上、860eV以下のピーク面積に対する、853.5eV超、860eV以下のピーク面積の比率が0.5以上であり、
CO昇温脱離法による40℃〜800℃でのCO脱離量に対する、H2昇温脱離法による40℃〜800℃でのH2脱離量のモル比率が0.3以上である
ことを特徴とする請求項7に記載の金属担持触媒。 - 請求項5乃至8のいずれかに記載の金属担持触媒を有し、
一酸化炭素のメタネーション反応に使用される
ことを特徴とするメタネーション反応装置。 - 有機物と金属とを含む原料の炭素化により得られる炭素化材料を、一酸化炭素のメタネーション反応触媒活性を示す金属を担持するための担体として使用する
ことを特徴とする方法。 - 前記金属は、Ni、Ru、Rh、Pd、Pt、Ir、Cu、W、Cs、K、Na、Co、Fe、Ca、Mg、Ba、Sr及びLiからなる群より選択される1種以上である
ことを特徴とする請求項10に記載の方法。 - 前記金属は、Niである
ことを特徴とする請求項11に記載の方法。 - 請求項5乃至8のいずれかに記載の金属担持触媒を使用して、一酸化炭素のメタネーション反応を行う
ことを特徴とする方法。 - 一酸化炭素を含む第一のガスを処理することにより、前記第一のガスに比べて一酸化炭素の濃度が低減された第二のガスを製造する
ことを特徴とする請求項13に記載の方法。 - 前記第一のガス及び前記第二のガスは、水素をさらに含む
ことを特徴とする請求項14に記載の方法。 - 前記金属担持触媒を有するメタネーション反応装置を使用する
ことを特徴とする請求項13乃至15のいずれかに記載の方法。 - 複数の候補担体から、一酸化炭素のメタネーション反応触媒活性を示す金属を担持するための担体を選択する方法であって、
Niを担持した状態の前記複数の候補担体の各々について、
Niの2p軌道の電子状態をXPS測定して得られる、850eV以上、860eV以下のピーク面積に対する、853.5eV超、860eV以下のピーク面積の比率が、0.5以上の予め定められた閾値以上であるか否かを判断すること、
CO昇温脱離法による40℃〜800℃でのCO脱離量に対する、H2昇温脱離法による40℃〜800℃でのH2脱離量のモル比率が、0.3以上の予め定められた閾値以上であるか否かを判断すること、及び
前記複数の候補担体のうちから、前記ピーク面積の比率が前記閾値以上であり、且つ前記モル比率が前記閾値以上であると判断された担体を選択すること
を含む
ことを特徴とする方法。
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CN201280057832.6A CN103998134B (zh) | 2011-11-25 | 2012-11-01 | 用于负载金属的载体、负载金属型催化剂、甲烷化反应设备和与其相关的方法 |
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CN103998134B (zh) | 2018-02-13 |
KR20140102192A (ko) | 2014-08-21 |
EP2783751A4 (en) | 2015-08-19 |
EP2783751A1 (en) | 2014-10-01 |
CA2855920C (en) | 2022-03-15 |
KR102040342B1 (ko) | 2019-11-04 |
US10005701B2 (en) | 2018-06-26 |
JP5889613B2 (ja) | 2016-03-22 |
CA2855920A1 (en) | 2013-05-30 |
WO2013077165A1 (ja) | 2013-05-30 |
US20140296357A1 (en) | 2014-10-02 |
CN103998134A (zh) | 2014-08-20 |
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