JP2009233662A - 炭化水素を分解する多孔質触媒体及びその製造方法、炭化水素から水素を含む混合改質ガスを製造する方法、並びに燃料電池システム - Google Patents
炭化水素を分解する多孔質触媒体及びその製造方法、炭化水素から水素を含む混合改質ガスを製造する方法、並びに燃料電池システム Download PDFInfo
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- JP2009233662A JP2009233662A JP2009052519A JP2009052519A JP2009233662A JP 2009233662 A JP2009233662 A JP 2009233662A JP 2009052519 A JP2009052519 A JP 2009052519A JP 2009052519 A JP2009052519 A JP 2009052519A JP 2009233662 A JP2009233662 A JP 2009233662A
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- Prior art keywords
- nickel
- catalyst body
- porous catalyst
- magnesium
- aluminum
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- 229930195733 hydrocarbon Natural products 0.000 title claims abstract description 150
- 150000002430 hydrocarbons Chemical class 0.000 title claims abstract description 148
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- 239000001257 hydrogen Substances 0.000 title claims description 28
- 229910052739 hydrogen Inorganic materials 0.000 title claims description 28
- 238000004519 manufacturing process Methods 0.000 title claims description 24
- 239000000446 fuel Substances 0.000 title claims description 22
- 230000003197 catalytic effect Effects 0.000 title abstract description 36
- 125000004435 hydrogen atom Chemical class [H]* 0.000 title 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 162
- 239000003054 catalyst Substances 0.000 claims abstract description 149
- 239000011777 magnesium Substances 0.000 claims abstract description 65
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 63
- 239000011148 porous material Substances 0.000 claims abstract description 54
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 53
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 53
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 53
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 52
- 229910001701 hydrotalcite Inorganic materials 0.000 claims abstract description 49
- 229960001545 hydrotalcite Drugs 0.000 claims abstract description 49
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 claims abstract description 13
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- 239000010419 fine particle Substances 0.000 claims description 23
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 21
- 229910052799 carbon Inorganic materials 0.000 claims description 21
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 21
- 229910052707 ruthenium Inorganic materials 0.000 claims description 14
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 12
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- 239000010941 cobalt Substances 0.000 claims description 11
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 11
- 229910052763 palladium Inorganic materials 0.000 claims description 11
- 229910052697 platinum Inorganic materials 0.000 claims description 11
- 229910052703 rhodium Inorganic materials 0.000 claims description 11
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- 239000010949 copper Substances 0.000 claims description 10
- 229910052741 iridium Inorganic materials 0.000 claims description 10
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 10
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 9
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- 239000011651 chromium Substances 0.000 claims description 9
- 229910052802 copper Inorganic materials 0.000 claims description 9
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 9
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- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 9
- 229910052702 rhenium Inorganic materials 0.000 claims description 9
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 claims description 9
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- 239000002131 composite material Substances 0.000 claims description 5
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 2
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- 239000011572 manganese Substances 0.000 claims description 2
- 229910001111 Fine metal Inorganic materials 0.000 claims 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims 1
- 238000004939 coking Methods 0.000 abstract description 22
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 15
- 239000011593 sulfur Substances 0.000 abstract description 15
- 229910052717 sulfur Inorganic materials 0.000 abstract description 15
- 238000000465 moulding Methods 0.000 abstract description 11
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- 229940091250 magnesium supplement Drugs 0.000 description 45
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- 239000002994 raw material Substances 0.000 description 16
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 15
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 15
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- 239000003513 alkali Substances 0.000 description 12
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 10
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- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 9
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- 238000010438 heat treatment Methods 0.000 description 8
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 8
- 239000002243 precursor Substances 0.000 description 8
- 238000010298 pulverizing process Methods 0.000 description 8
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 8
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- 230000032683 aging Effects 0.000 description 7
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 7
- 238000001914 filtration Methods 0.000 description 7
- 238000010304 firing Methods 0.000 description 7
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 7
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- ZSDSQXJSNMTJDA-UHFFFAOYSA-N trifluralin Chemical compound CCCN(CCC)C1=C([N+]([O-])=O)C=C(C(F)(F)F)C=C1[N+]([O-])=O ZSDSQXJSNMTJDA-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
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- H01M8/0606—Combination of fuel cells with means for production of reactants or for treatment of residues with means for production of gaseous reactants
- H01M8/0612—Combination of fuel cells with means for production of reactants or for treatment of residues with means for production of gaseous reactants from carbon-containing material
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Abstract
【解決手段】 少なくともマグネシウム、アルミニウム及びニッケルからなり、マグネシウムを10〜50wt%、アルミニウムを5〜35wt%、ニッケルを0.1〜30wt%含有し、細孔容積が0.01〜0.5cm3/g、平均細孔径が300Å以下、平均圧壊強度が3kgf(29.4N)以上である炭化水素を分解する多孔質触媒体は、少なくともマグネシウム、アルミニウム及びニッケルを含有したハイドロタルサイトを成形し、700℃〜1500℃の範囲で焼成して得ることができる。
【選択図】 なし
Description
CnH2n+2 + nH2O → nCO + (2n+1)H2
CO + H2O → CO2 + H2
一般に、この反応は600℃〜800℃で行われ、S/C(水蒸気/炭素比:Steam/Carbon比)が2.0〜3.5付近で行われる。この反応は吸熱反応であり、温度が高い程、反応を促進することができる。
上記活性金属種は炭化水素を分解する多孔質触媒体を作製する際に同時に含ませることも可能であり、炭化水素を分解する多孔質触媒体を作製後に担持させても良く、特に限定されるものではない。担持方法に関しても特に限定されず、スプレードライ法や含浸法など一般に行われている手法で良い。
還元時の雰囲気は、水素を含んだガスなど還元雰囲気であれば特に限定されない。
還元処理の時間は特に限定されないが0.5〜24時間が望ましい。24時間を越えると工業的にメリットが見出せない。好ましくは1〜10時間である。
本発明に係る炭化水素を分解する多孔質触媒体が大きな比表面積、細孔容積、高い圧壊強度を有し、且つ、優れた触媒活性、耐硫黄被毒性、耐コーキング性を有する理由については、本発明者は次のように推定している。
MgSO4・7H2O 1927.7gとAl2(SO4)3・8H2O 1001.2g、NiSO4・6H2O 541.2gとを純水で溶解させ12000mlとした。別にNaOH 8044ml(14mol/L濃度)とNa2CO3 305.5gを溶解させたものを合わせた23000mlのアルカリ混合溶液を用意した。このアルカリ混合溶液に前記マグネシウム塩とアルミニウム塩、ニッケル塩との混合溶液を加え、95℃で8時間熟成を行ってハイドロタルサイト化合物を得た。これを濾別分離後、乾燥、粉砕しハイドロタルサイト化合物粉末を得た。得られたハイドロタルサイト化合物粉末のBET比表面積は43.2m2/gであった。また粉砕処理後の二次凝集粒子の平均粒子径は13.7μmであった。
得られたハイドロタルサイト化合物粉末 1058.7gにベーマイト 127.1gとPVA 121.2g、さらに水 105.8gとプロピレングリコール 741.1gを混合し、スクリューニーダーで5時間混練した。混練後の粘土状混練物を圧縮成形法により直径5.1mmφの球状に成形後、105℃で乾燥し、1100℃で3時間熱処理を行った。さらにその後、780℃にて水素/アルゴン体積比が10/90のガス気流中において3時間還元処理を行い、炭化水素を分解する多孔質触媒体を得た。
炭化水素を分解する多孔質触媒体の性能評価は、触媒を直径20mmのステンレス製反応管に10〜50g充填して触媒管を作った。
この触媒管(反応器)に対して、原料ガス及び水蒸気を、反応圧力0.1MPa、反応温度300℃〜800℃、空間速度を10000h−1として流通させた。この時の水蒸気/炭素比は1.0、水蒸気/炭素比は3.0である。なお、炭化水素を含有する原料ガスとして原料ガスには都市ガス(13A)を用いて反応を行った。
例)原料ガスにプロパンを用いた場合
プロパン転化率
=100×(CO+CO2+CH4+C2H6)/(CO+CO2+CH4+C2H6+C3H8)
Cn転化率(全炭化水素転化率)
=(CO+CO2)/(CO+CO2+CH4+C2H6+C3H8)
表1には、原料ガスとして都市ガス(13A)を用いGHSVが3000h−1、50000h−1、水蒸気/炭素(S/C)が3.0、反応時間が24hの反応条件における、反応温度(300℃〜700℃)と転化率との関係を示す。
表2には、原料ガスとして都市ガス(13A)を用い、GHSVが3000h−1、反応温度が700℃、水蒸気/炭素(S/C)が1.5の場合における、反応時間とプロパン転化率及び触媒活性測定前後の炭素析出量、さらに水蒸気/炭素(S/C)が1.5の場合における、反応時間と圧壊強度、BET比表面積、細孔容積の関係を示す。
MgCl2・6H2O 5619.8gとAlCl3・9H2O 741.5g、NiCl2・6H2O 142.9gを純水で溶解させ12000mlとした。別にNaOH 9924ml(14mol/L濃度)とNa2CO3 455.8gを溶解させたものを合わせた28000mlのアルカリ混合溶液を用意した。このアルカリ混合溶液に前記マグネシウム塩とアルミニウム塩、ニッケル塩の混合溶液を加え、180℃で8時間熟成を行ってハイドロタルサイト化合物を得た。これを濾別分離後、乾燥、粉砕しハイドロタルサイト化合物粉末を得た。得られたハイドロタルサイト化合物粉末のBET比表面積は12.2m2/gであった。また粉砕処理後の二次凝集粒子の平均粒子径は32.2μmであった。
Mg(NO3)2・6H2O 864.3gとAl(NO3)3・9H2O 549.8g、Ni(NO3)2・6H2O 639.2gとを純水で溶解させ10000mlとした。別にNaOH 2638ml(14mol/L濃度)とNa2CO3 217.5gを溶解させたものを合わせた24000mlのアルカリ混合溶液を用意した。このアルカリ混合溶液に前記マグネシウム塩とアルミニウム塩、ニッケル塩との混合溶液を加え、70℃で6時間熟成を行って含水複水酸化物を得た。これを濾別分離後、乾燥、粉砕しハイドロタルサイト化合物粉末を得た。得られたハイドロタルサイト化合物粉末のBET比表面積は119.2m2/gであった。また粉砕処理後の二次凝集粒子の平均粒子径は52.1μmであった。
MgSO4・7H2O 3223.3gとAl2(SO4)3・8H2O 1272.1g、NiSO4・6H2O 1100.3gとを純水で溶解させ15000mlとした。別にNaOH 4552ml(14mol/L濃度)とNa2CO3 388.3gを溶解させたものを合わせた23000mlのアルカリ混合溶液を用意した。このアルカリ混合溶液に前記マグネシウム塩とアルミニウム塩、ニッケル塩との混合溶液を加え、80℃で6時間熟成を行ってハイドロタルサイト化合物を得た。これを濾別分離後、乾燥、粉砕しハイドロタルサイト化合物粉末を得た。得られたハイドロタルサイト化合物粉末のBET比表面積は72.4m2/gであった。また粉砕処理後の二次凝集粒子の平均粒子径は2.2μmであった。
MgCl2・6H2O 1597.3gとAlCl3・9H2O 431.1g、NiCl2・6H2O 664.8g、CoCl2・6H2O 169.9を純水で溶解させ8000mlとした。別にNaOH 4755ml(14mol/L濃度)とNa2CO3 265.0gを溶解させたものを合わせた22000mlのアルカリ混合溶液を用意した。このアルカリ混合溶液に前記マグネシウム塩とアルミニウム塩、ニッケル塩、コバルト塩の混合溶液を加え、140℃で10時間熟成を行ってハイドロタルサイト化合物を得た。これを濾別分離後、乾燥、粉砕しハイドロタルサイト化合物粉末を得た。得られたハイドロタルサイト化合物粉末のBET比表面積は13.2m2/gであった。また粉砕処理後の二次凝集粒子の平均粒子径は22.2μmであった。
実施例1と同様にして直径5.2mmφの球状に成形した粘土状混練物を、120℃で乾燥し、1000℃で8時間熱処理を行った。その後、金属換算でRuを2.2wt%となるようにスプレー担持させ、乾燥後、760℃にて水素/アルゴン体積比が10/90のガス気流中において2時間還元処理を行った。
Mg(NO3)2・6H2O 1523.1gとAl(NO3)3・9H2O 618.9gとを純水で溶解させ10000mlとした。別にNaOH 2400ml(14mol/L濃度)とNa2CO3 244.9gを溶解させたものを合わせた15000mlのアルカリ混合溶液を用意した。このアルカリ混合溶液に前記マグネシウム塩とアルミニウム塩との混合溶液を加え、85℃で4時間熟成を行って含水複水酸化物を得た。これを濾別分離後、乾燥、粉砕しハイドロタルサイト化合物粉末を得た。得られたハイドロタルサイト化合物粉末のBET比表面積は86.5m2/gであった。また粉砕処理後の二次凝集粒子の平均粒子径は42.1μmであった。
その後、金属換算でNiを8.0wt%となるようにニッケル塩をスプレー担持させ、乾燥後、760℃にて水素/アルゴン体積比が50/50のガス気流中において5時間還元処理を行い、炭化水素を分解する多孔質触媒体を得た。
MgO 895.6gとγ−アルミナ 9.652gとPVA 71.52gと水521.3gを混合し、スクリューニーダーで1時間混練した。混練後の粘土状混練物を圧縮成形法により直径5.1mmφの球状に成形後、120℃で乾燥し、1250℃で8時間熱処理を行った。その後、金属換算でNiを34wt%となるようにスプレー担持させ、乾燥後、800℃にて水素/アルゴン体積比が10/90のガス気流下において3時間還元処理を行った。
得られた球状(直径3.2mmφ)の触媒体のBET比表面積は2.2m2/gであり、平均細孔径は382Åであり、細孔容積は0.009cm3/gであった。また、マグネシウムの含有量は39.77wt%であり、アルミニウムの含有量は0.563wt%であり、Ni含有量は33.33wt%であった。また、金属ニッケル微粒子の大きさは35.5nmであった。さらに平均圧壊強度は4.3kgfであった。
γ−アルミナ 845.3gにPVA 22.54gを混合したものを、転動造粒機にて純水をスプレーしながら造粒し、直径4.8mmφの球状のγ−アルミナ成形体を得た。得られた成形体を120℃で乾燥し、850℃で10時間熱処理を行った。その後、金属換算でNiを20wt%となるようにスプレー担持させ、乾燥後、780℃にて水素/アルゴン体積比が10/90のガス気流下において2時間還元処理を行った。
得られた球状(直径2.7mmφ)の触媒体のBET比表面積は185.5m2/gであり、平均細孔径は322Åであり、細孔容積は0.532cm3/gであった。また、アルミニウムの含有量は42.96wt%であり、Ni含有量は18.79wt%であった。また、金属ニッケル微粒子の大きさは25.5nmであった。さらに平均圧壊強度は1.2kgfであった。
実施例1で作製したハイドロタルサイト化合物粉末 847.2gに水 440.4gを混合し、スクリューニーダーで5時間混練した。混練後の粘土状混練物を圧縮成形法により直径5.3mmφの球状に成形後、105℃で乾燥し、1100℃で3時間熱処理を行った。さらにその後、780℃にて水素/アルゴン体積比が10/90のガス気流中において3時間還元処理を行い、炭化水素を分解する多孔質触媒体を得た。
得られた球状(直径4.5mmφ)の炭化水素を分解する多孔質触媒体のBET比表面積は65.2m2/gであり、平均細孔径は144Åであり、細孔容積は0.198cm3/gであった。またMg含有量は分析の結果、29.42wt%であり、Al含有量は17.19wt%、Ni含有量は18.71wt%であり、金属ニッケル微粒子の大きさは6.5nmであった。平均圧壊強度は1.1kgfであった。
Claims (7)
- 炭化水素を分解する多孔質触媒体であって、少なくともマグネシウム、アルミニウム及びニッケルからなり、マグネシウム及びアルミニウムが複合酸化物として存在し、ニッケルが金属ニッケルとして存在し、マグネシウム元素を10〜50wt%、アルミニウム元素を5〜35wt%、ニッケル元素を0.1〜30wt%含有し、細孔容積が0.01〜0.5cm3/gであり、平均細孔径が300Å以下であり、平均圧壊強度が3kgf以上であることを特徴とする炭化水素を分解する多孔質触媒体。
- 金属ニッケルが微粒子として存在し、該金属ニッケル微粒子の平均粒子径が1〜20nmである請求項1記載の炭化水素を分解する多孔質触媒体。
- BET比表面積が10〜100m2/gである請求項1又は2記載の炭化水素を分解する多孔質触媒体。
- 少なくともマグネシウム、アルミニウム及びニッケルを含有したハイドロタルサイトを成形し、700℃〜1500℃の範囲で焼成す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炭化水素を分解する多孔質触媒体の製造方法。
- 請求項1乃至3のいずれかに記載の炭化水素を分解する多孔質触媒体に、平均粒径が50nm以下の金、銀、白金、パラジウム、ルテニウム、コバルト、ロジウム、イリジウム、レニウム、銅、マンガン、クロム、バナジウム、チタンから選ばれる一種または二種以上の活性金属種を担持する炭化水素を分解する多孔質触媒体。
- 請求項1、2、3又は5のいずれかに記載の炭化水素を分解する多孔質触媒体を用いて、反応温度が250℃〜850℃であって、スチームとカーボンのモル比(S/C)が1.0〜6.0であって、空間速度(GHSV)が100〜100000h−1の条件下で、炭化水素と水蒸気を反応させることを特徴とする炭化水素から水素を含む混合改質ガスを製造する方法。
- 請求項1、2、3又は5のいずれかに記載の炭化水素を分解する多孔質触媒体を用いることを特徴とする燃料電池システム。
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JP2011143361A (ja) * | 2010-01-15 | 2011-07-28 | Nikki Universal Co Ltd | 炭化水素改質触媒、該触媒の製造方法および該触媒を用いる改質方法 |
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JP7455206B2 (ja) | 2020-10-27 | 2024-03-25 | コリア クンホ ペトロケミカル カンパニー リミテッド | 触媒成形体、その製造方法及びこれを用いた環状ケトンの製造方法 |
KR102376875B1 (ko) * | 2021-11-24 | 2022-03-18 | 부경대학교 산학협력단 | 니켈계 촉매상에서 바이오매스 유래 오일의 수증기 개질 및 수소화 반응에 의한 수소의 생산 방법 |
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US8486368B2 (en) | 2013-07-16 |
US20130045159A1 (en) | 2013-02-21 |
EP2251080B1 (en) | 2022-05-18 |
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EP2251080A4 (en) | 2011-08-31 |
US20110038775A1 (en) | 2011-02-17 |
US8304367B2 (en) | 2012-11-06 |
KR101523122B1 (ko) | 2015-05-26 |
US20130287679A1 (en) | 2013-10-31 |
KR20100125262A (ko) | 2010-11-30 |
US8883118B2 (en) | 2014-11-11 |
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