JP6317668B2 - 炭化水素の自己熱水蒸気改質(atr)のための触媒構造 - Google Patents
炭化水素の自己熱水蒸気改質(atr)のための触媒構造 Download PDFInfo
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- JP6317668B2 JP6317668B2 JP2014505203A JP2014505203A JP6317668B2 JP 6317668 B2 JP6317668 B2 JP 6317668B2 JP 2014505203 A JP2014505203 A JP 2014505203A JP 2014505203 A JP2014505203 A JP 2014505203A JP 6317668 B2 JP6317668 B2 JP 6317668B2
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- hydrogen
- atr
- catalyst
- temperature
- metal
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/32—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air
- C01B3/34—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents
- C01B3/48—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents followed by reaction of water vapour with carbon monoxide
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
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Description
a.10またはそれ以上のpHを有する塩基性溶液であって、水酸化物、好ましくは、アルカリ金属水酸化物と、炭酸ナトリウムと、水とを含む、塩基性溶液を調製すること。
b.酸性溶液が、塩の混合物を水と組み合わせることによって調製され、塩が、カチオンおよびアニオンから成り、カチオンが、マグネシウム、ニッケル、およびアルミニウムから成り、酸性溶液が、約1.5Mの総カチオン濃度を有する、7未満のpHを有する酸性溶液を調製すること。
c.ゾル・ゲルを形成するように動作可能な期間にわたって、酸性溶液および塩基性溶液をともに混合すること。
d.形成固体を形成するように、所定の期間にわたってゾル・ゲルを熟成させること。
e.略中性pHに達するまで、水で形成固体を洗浄および濾過すること。
f.乾燥固体を形成するように、所定の期間にわたって形成固体を乾燥させることと。
g.焼成物質を形成するように、所定の期間にわたって所定の温度で乾燥固体を焼成すること。
h.ナノサイズ混合金属酸化物が、約40〜約300nmの範囲内の直径を有する、ATR触媒構造であって、全体を通して分散されたナノサイズ混合酸化物粒子を有する、ATR触媒構造を形成するように、約450℃から約700℃の範囲内の温度で焼成物質を水素および窒素ガスの混合物と接触させることによって、焼成物質に金属還元ステップを受けさせること。
[触媒構造の実験的設計:]
混合金属酸化物の形態での0.2から5の間のAl/Mgモル比
焼成温度:500℃〜600℃
還元温度:500℃
水素の濃度:5〜20モル%
ニッケル取り込み方法:マグネシウムおよびアルミニウムを同時に用いた共沈、またはAl−Mg担体上の含浸
ニッケル含有量: 10重量%
カチオン比[Al/(Al+Mg+Ni)]: 0.20
焼成温度: 550℃
還元温度: 500℃
ニッケル取り込み方法: マグネシウムおよびアルミニウムを用いた共沈
炭化水素供給: n−オクタン
反応温度: 500℃、550℃、および600℃
全圧力: 3バール
単位時間あたりの重量空間速度 (WHSV): 5000時間−1
酸素/炭素 (モル比): 0.5
蒸気/炭素 (モル比): 3
(1)LDH物質の焼成/還元によって得られた触媒は、水素生成用の液体炭化水素の自己熱改質のための好適な触媒物質であることが判明した。これらの触媒物質は、基質の内側で安定しており、有利に高い表面積を有する、高度に分散した金属結晶または粒子を呈する。
(2)本発明の種々の実施形態に従って得られる触媒物質は、液体炭化水素、蒸気、および空気を、水素および二酸化炭素に変換するために、触媒膜で使用することができる。触媒活性試験は、いかなる一酸化炭素生成も伴わずに生成された大きいレベルの水素とともに、ほぼ完全な液体炭化水素変換を生じ、したがって、ATRおよびWGS複合反応の優れた均衡を示した。加えて、WGS反応が、メタン化反応より有利であり、低減した量のメタンガスを生成させた。また、コークス形成も低減させられ、これが全体的な触媒活性を向上させ、したがって、より長い実行時間につながる。
(3)共沈によって触媒物質に取り込まれたニッケルは、含浸方法よりも高度かつ微細に分散したニッケル粒子をもたらす。
(4)合成パラメータは、金属・担体相互作用に重要な影響を及ぼす。より強力な金属・担体相互作用が有益であるとき、触媒構造が向上させられる。加えて、触媒性能は、ニッケル粒径、ならびに選択された担体物質およびその性能に強力に結び付けられる。
[CMRアセンブリの実験的設計:]
TEOS: 0.9部分
Pt-Rh: 0.5〜2.5部分
水: 4部分
HNO3: 0.01部分
エタノール: 10部分
その後、結果として生じる溶液が、室温で約12時間にわたって加水分解された。適切な量の硝酸の0.1M溶液を添加した後、溶液が、コロイドゾル溶液に変換するように室温で約5時間にわたって放置され、次いで、膜管の内壁を被覆するために使用された。
CMRアセンブリの実験結果:
Claims (12)
- 自己熱改質(ATR)触媒構造を構築するための方法であって、
塩基性pHを有する塩基性溶液であって、アルカリ金属水酸化物と、アルカリ金属炭酸塩と、水とを含む、塩基性溶液を得ることと、
酸性pHを有する酸性溶液であって、塩が、カチオンおよびアニオンから成り、前記カチオンが、マグネシウム、ニッケル、およびアルミニウムから成り、前記カチオンが、白金、ロジウム、金、イリジウム、オスミウム、パラジウム、レニウム、および、ルテニウムである高価値金属を含まず、前記塩と、水とを含む、前記酸性溶液を得ることと、
前記塩基性溶液を用いた前記カチオンの共沈を通して、層状結晶構造を備えた層状複水酸化物(LDH)前駆体を有するゾル・ゲルを作成するように、前記塩基性溶液を前記酸性溶液と混合することと、
前記LDH前駆体が少なくとも部分的に分解されて、ナノサイズに混合された混合金属酸化物の焼成物質を形成するように、所定量の時間にわたって、500℃以上および焼結温度以下の熱分解温度で前記ゾル・ゲルを加熱することと、
全体を通して均質的に分散された金属粒子を有する、ATR触媒構造を形成するように、450℃から700℃の範囲内の温度で、5〜20モル%の範囲の水素、および窒素を有するガス混合物を使用して、前記LDH前駆体内の前記層状結晶構造を崩壊させるために前記焼成物質に金属還元ステップを行うことと、
を含み、
前記ATR触媒構造は、多孔質管状担体に取り込まれた後、ATR反応の使用を通して、液体炭化水素を有する供給流から水素生成物流を生成するように動作可能である方法。 - 前記金属粒子は、100〜300m2/gの間の表面積を有する、請求項1に記載の方法。
- 前記塩基性溶液は、10から12の間のpHを有する、請求項1または2記載の方法。
- 前記塩基性溶液はさらに、前記塩基性溶液が12のpHを有するように、NaOHおよびNa2CO3の混合物を含む、請求項1〜3のいずれかに記載の方法。
- 前記酸性溶液は、1.5Mの総カチオン濃度を有する、請求項1〜4のいずれかに記載の方法。
- 前記カチオンは、20〜35モル%の間のアルミニウム濃度を有する、請求項1〜5のいずれかに記載の方法。
- 前記熱分解温度は、500℃から600℃の範囲内である、請求項1〜6のいずれかに記載の方法。
- 自己熱改質(ATR)触媒を構築する方法であって、
(a)10またはそれ以上のpHを有する塩基性溶液を調製することと、
(b)酸性溶液が、塩の混合物を水と組み合わせることによって調製され、前記塩が、カチオンおよびアニオンから成り、前記カチオンが、マグネシウム、ニッケル、およびアルミニウムから成り、前記カチオンが、白金、ロジウム、金、イリジウム、オスミウム、パラジウム、レニウム、および、ルテニウムである高価値金属を含まず、前記酸性溶液が、1.5Mの総カチオン濃度を有する、7未満のpHを有する前記酸性溶液を調製することと、
(c)ゾル・ゲルを形成するように、前記酸性溶液および前記塩基性溶液をともに混合することと、
(d)形成固体を形成するように、前記ゾル・ゲルを熟成させることと、
(e)略中性pHに達するまで、水で前記形成固体を洗浄および濾過することと、
(f)乾燥固体を形成するように、所定の期間にわたって前記形成固体を乾燥させることと、
(g)焼成物質である混合金属酸化物を形成するように、500℃から600℃の間の温度で前記乾燥固体を焼成することと、
(h)全体を通して分散された金属粒子を有する、ATR触媒構造を形成するように、450℃から700℃の範囲内の温度で前記焼成物質を水素と接触させることによって、前記焼成物質の中の金属を還元することと、
を含み、
前記ATR触媒構造は、多孔質管状担体に取り込まれた後、ATR反応の使用を通して、液体炭化水素供給流から水素生成物流を生成するように動作可能である方法。 - 前記アニオンは、硝酸塩イオンを含む、請求項8に記載の方法。
- ステップ(a)の前記塩基性溶液は、前記塩基性溶液が12のpHを有するように、NaOHおよびNa2CO3を組み合わせることによって調製される、請求項8または9に記載の方法。
- 前記水素生成物流は、一酸化炭素を実質的に含まない、請求項8〜10のいずれかに記載の方法。
- 前記水素生成物流は、わずか0.5容量%の一酸化炭素を含む、請求項8〜10のいずれかに記載の方法。
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JP5477561B2 (ja) * | 2009-09-09 | 2014-04-23 | 戸田工業株式会社 | 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 |
JP4669931B1 (ja) | 2010-01-29 | 2011-04-13 | 国立大学法人 岡山大学 | 燃料品質判定方法および燃料品質判定装置 |
CN101875012B (zh) | 2010-04-13 | 2011-12-21 | 沈阳化工学院 | 制备联产甲基异丁基酮和二异丁基酮Ni/MgO-Al2O3催化剂的方法 |
US9168511B2 (en) | 2010-11-16 | 2015-10-27 | Stichting Energieonderzoek Centrum Nederland | Catalyst for hydrogen production |
US8597383B2 (en) * | 2011-04-11 | 2013-12-03 | Saudi Arabian Oil Company | Metal supported silica based catalytic membrane reactor assembly |
US9745191B2 (en) * | 2011-04-11 | 2017-08-29 | Saudi Arabian Oil Company | Auto thermal reforming (ATR) catalytic structures |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2023217591A1 (en) * | 2022-05-09 | 2023-11-16 | Refractory Intellectual Property Gmbh & Co. Kg | Insulating lining, use of an alumina-based part, reactor for hydrocarbon reforming and process for hydrocarbon reforming |
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AU2012243060A1 (en) | 2013-10-31 |
US10252911B2 (en) | 2019-04-09 |
US20160214859A1 (en) | 2016-07-28 |
EP2696976A1 (en) | 2014-02-19 |
US9745191B2 (en) | 2017-08-29 |
US20160214091A1 (en) | 2016-07-28 |
US10071909B2 (en) | 2018-09-11 |
US20120258857A1 (en) | 2012-10-11 |
CN104220161A (zh) | 2014-12-17 |
US10252910B2 (en) | 2019-04-09 |
US20160214090A1 (en) | 2016-07-28 |
JP2014514148A (ja) | 2014-06-19 |
WO2012142006A1 (en) | 2012-10-18 |
AU2012243060B2 (en) | 2016-12-08 |
US20160214089A1 (en) | 2016-07-28 |
US10093542B2 (en) | 2018-10-09 |
AU2017201051A1 (en) | 2017-03-09 |
AU2017201051B2 (en) | 2019-05-23 |
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