JP7077304B2 - メタン酸化触媒、それを調製するプロセス、およびそれを使用する方法 - Google Patents
メタン酸化触媒、それを調製するプロセス、およびそれを使用する方法 Download PDFInfo
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- JP7077304B2 JP7077304B2 JP2019511863A JP2019511863A JP7077304B2 JP 7077304 B2 JP7077304 B2 JP 7077304B2 JP 2019511863 A JP2019511863 A JP 2019511863A JP 2019511863 A JP2019511863 A JP 2019511863A JP 7077304 B2 JP7077304 B2 JP 7077304B2
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- zirconia
- impregnated
- methane
- noble metal
- methane oxidation
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- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims description 73
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- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical group 0.000 description 1
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 1
- 229940038773 trisodium citrate Drugs 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- XJUNLJFOHNHSAR-UHFFFAOYSA-J zirconium(4+);dicarbonate Chemical compound [Zr+4].[O-]C([O-])=O.[O-]C([O-])=O XJUNLJFOHNHSAR-UHFFFAOYSA-J 0.000 description 1
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Description
a.)非変性ジルコニア前駆体を675~1050℃の範囲の温度で焼成して正方晶ジルコニアを調製するステップであって、正方晶ジルコニア対単斜晶ジルコニア(存在する場合)の重量比は31:1を超える、ステップと、
b.)ステップa.)から得られたジルコニアに貴金属前駆体含有含浸溶液を含浸させるステップと、
c.)湿潤な貴金属含浸ジルコニアを120℃以下の温度で乾燥させるステップと、
d.)乾燥させた貴金属含浸ジルコニアを400~650℃の範囲の温度で焼成するステップと、を含み、正方晶ジルコニア対単斜晶ジルコニアの重量比は1:1~31:1の範囲である、メタン酸化触媒を調製するためのプロセスを提供する。
a.)非変性ジルコニア前駆体を675~1050℃の範囲の温度で焼成して正方晶ジルコニアを調製するステップであって、正方晶ジルコニア対単斜晶ジルコニア(存在する場合)の重量比は31:1を超える、ステップと、
b.)ステップb.)から得られたジルコニアに貴金属前駆体含有含浸溶液を含浸させるステップと、
c.)湿潤な貴金属含浸ジルコニアを120℃以下の温度で乾燥させるステップと、
d.)乾燥させた貴金属含浸ジルコニアを400~650℃の範囲の温度で焼成するステップと、を含み、正方晶ジルコニア対単斜晶ジルコニアの重量比は1:1~31:1の範囲である、メタン酸化触媒を調製するためのプロセスを提供する。
(i)全懸濁液の重量に基づき10~65重量%の範囲のジルコニアを含有するジルコニアの水性懸濁液を調製するステップと、
(ii)ジルコニア粒子の水性懸濁液に酸を添加して、懸濁液のpHを3~6、好ましくは3.5~4.5の範囲のpHに調節するステップと、
(iii)ジルコニア粒子の水性懸濁液を、光の散乱によって判定すると最大20μmの体積平均粒径のジルコニア粒子を含むまで湿式粉砕し、任意選択的に、粉砕された懸濁液のpHを酸により再調節して、それを3~6、好ましくは3.5~4.5の範囲に維持するステップと、
(iv)ステップ(iii)で得られた懸濁液の層をセラミックモノリス担体または金属モノリス担体の表面上にウォッシュコートするステップと、
(v)ウォッシュコートされたセラミックモノリス担体または金属モノリス担体を120℃以下の温度で少なくとも1時間にわたって乾燥させるステップと、を含む。
以下の試験手順を使用した。
触媒性能評価試験
ステンレス鋼製の48個の固定床反応器(各反応器は1mLの全容積を有する)を有する完全自動化された並列高ハイスループット触媒試験リグ内で触媒のメタン酸化活性測定を行った。余剰酸素(燃料リーン)で作動される天然ガス燃料エンジンのものに似たシミュレートされた排気ガス組成および運転条件を使用して触媒を試験した。試験に使用した条件を表1に示す。
Bruker D8 Advance X線回折システム(Diffrac.EVAソフトウェア、ブラッグ-ブレンターノ型ジオメトリ、高分解能LYNXEYE XE検出器、5°~140°の2θ範囲のCuKα線(λ=1.5406Å)、1°ステップ、走査速度0.02°/秒、角度計半径28cm、Niフィルター、印加電力40kV/40mA)上でジルコニア系触媒材料の粉末XRD結晶相分析を行った。
本発明を裏付けるメタン酸化触媒のいくつかの試料を調製した。
平均粒径5.5μm、600℃の空気中で判定された33.2重量%の点火損失(LOI)、および非晶質結晶相構造を有する10gの水酸化ジルコニウム粉末を、空気流中で5℃/分の加熱速度を使用して850℃の温度に焼成し、この温度で12時間保持した。
tm-ZrO2触媒の調製のために、0.643mLの4.5mol/L硝酸水溶液と、0.607mLの脱イオン(さらにDIと称する)水とを含有する含浸溶液を、5gの量の試料1に含浸させた。次いで、その含浸された湿潤な粉末を、密封容器に5時間貯蔵し、80℃で16時間乾燥させ、その後、空気流中で5℃/分の加熱速度を使用して600℃に焼成し、この温度で12時間保持した。
Pd/tm-ZrO2触媒の調製のために、ジルコニアの細孔容積に合致するように、含浸前に、0.423mLのDI水で希釈された0.477mLのHNO3含有Pd(NO3)2水溶液(Pd濃度3.651mol/L)を、4.5gの量の試料1Aに含浸させた。次いで、その含浸された湿潤な試料を密閉容器内で室温で3時間にわたってエージングし、乾燥炉内で80℃で16時間乾燥させた。その後、そのようにして調製された触媒試料を、炉内に配置し、空気流中で5℃/分の加熱速度を使用して600℃に焼成し、この温度で12時間保持した。最終Pd/ZrO2触媒のPd含有量は、触媒試料全体に基づき4重量%であると判定された。
正方晶ジルコニア粉末(Saint-Gobain、ID#SZ61152、直径3mm、ロット#2005820395)を破砕し、ふるい分けして、315~500μmの範囲の粒径を有する画分を得た。次いで、得られた粉末を空気流中で5℃/分の加熱速度を使用して650℃に焼成し、この温度で12時間保持した。
含浸前に、0.636mLのDI水で希釈された1.164mLのHNO3含有Pd(NO3)2水溶液(Pd濃度1mol/L)を含浸させた試料4の3gのジルコニアを使用してメタン酸化触媒を調製した。その含浸試料を、密閉容器内で室温で3時間エージングし、80℃で乾燥炉内で16時間乾燥させた。その後、その触媒試料を炉内に配置し、空気流中で5℃/分の加熱速度を使用して600℃に焼成し、この温度で12時間保持した。最終触媒試料のPd含有量は、触媒試料全体に基づき4重量%であると判定された。
単斜晶ジルコニア粉末(Saint-Gobain、ID#SZ31164、直径3.175mm、ロット#SN2004910029)を破砕し、ふるい分けして、315~500μmの範囲の粒径を有する画分を得た。得られた粉末を空気流中で5℃/分の加熱速度を使用して650℃に焼成し、この温度で12時間保持した。
3gの量の比較試料5に、含浸前に、1.238mLのDI水で希釈された1.162mLのHNO3含有Pd(NO3)2水溶液(Pd濃度1mol/L)を含浸させた。次いで、その含浸試料を、密閉容器内で室温で3時間エージングし、80℃で乾燥炉内で16時間乾燥させた。その後、その触媒試料を炉内に配置し、空気流中で5℃/分の加熱速度を使用して600℃に焼成し、この温度で12時間保持した。最終触媒試料のPd含有量は、触媒試料全体に基づき4重量%であると判定された。
315~500μmの範囲の粒径を有する画分を得るために、アルミナ押出物試料(Saint-Gobain、ID#SA6175、直径1.59mm、ロット#9608006)を破砕し、ふるい分けした。次いで、得られた粉末を空気中で650℃で12時間焼成した。
50gの量の試料6のガンマ-アルミナに、含浸前に、31.22mLのDI水で希釈された18.78mLの水性HNO3含有Pd(NO3)2の溶液(濃度1mol/L)を含浸させた。次いで、その含浸された湿潤な触媒試料を、密閉容器内で室温で3時間エージングし、80℃で乾燥炉内で16時間乾燥させた。その後、その乾燥させた触媒試料を、5℃/分で600℃に加熱し、この温度で12時間保持することによって、空気流中で焼成した。得られた触媒試料のPd含有量は、触媒試料全体に基づき4重量%であると判定された。
315~500μmの範囲の粒径を有する画分を得るために、アルミナ押出物試料(Saint-Gobain、ID#SA6175、直径1.59mm、ロット#9608006)を破砕し、ふるい分けした。次いで、得られた粉末を空気中で650℃で12時間焼成した。貴金属を含浸させるために、アルミナ画分の3gに、含浸前に、0.62mLのDI水で希釈された0.97mLの水性HNO3含有Pd(NO3)2(濃度1mol/L)と0.22mLの水性HNO3含有Pt(NO3)2(濃度0.5mol/L)とを含有する溶液を含浸させた。その得られた湿潤な触媒試料を、密閉容器内で室温で3時間エージングし、80℃で乾燥炉内で16時間乾燥させた。その後、そ触媒を空気流中で5℃/分の加熱速度を使用して600℃に焼成し、この温度で12時間保持した。最終触媒の貴金属含有量(PdおよびPt)は、触媒試料全体に基づき4重量%、すなわち3.6重量%のPdと0.4重量%のPtであると判明した。
正方晶ジルコニア粉末(Saint-Gobain、ID#SZ61152、直径3mm、ロット#2005820395)を破砕し、ふるい分けして、315~500μmの粒径を有する画分を得た。次いで、得られた粉末を空気流中で5℃/分の加熱速度を使用して650℃に焼成し、この温度で12時間保持して、t-ZrO2に属するXRD反射のみを示すジルコニア(ジルコニア粉末A)を得た。単斜晶ジルコニア粉末(Saint-Gobain、ID#SZ31164、直径3.175mm、ロット#SN2004910029)を破砕し、ふるい分けして、315~500μmの粒径を有する画分を得た。得られた粉末を空気流中で5℃/分の加熱速度を使用して650℃に焼成し、この温度で12時間保持して、純m-ZrO2に属する粉末XRD反射を呈するジルコニア(ジルコニア粉末B)を得た。両ジルコニア粉末を混合して、正方晶対単斜晶の重量比19:1に相当する95重量%(t-ZrO2、ジルコニア粉末A)と5重量%(m-ZrO2、ジルコニア粉末B)の比率を含有する物理的混合物を調製した。
1.5gの量の比較試料8の物理的に混合されたt-/m-ZrO2粉末に、0.582mLのHNO3含有Pd(NO3)2水溶液(Pd濃度1mol/L)を含浸させた。含浸前に、上記Pd(NO3)2溶液を0.093mLのDI水で希釈した。次いで、その湿潤な触媒試料を、密閉容器内で室温で3時間エージングし、80℃で乾燥炉内で16時間乾燥させた。その後、乾燥させた触媒試料を炉内に配置し、空気流中で5℃/分の加熱速度を使用して600℃に焼成し、この温度で12時間保持した。最終触媒のPd含有量は、触媒試料発明全体に基づき4重量%であると判定された。
正方晶の硫黄変性ジルコニア粉末(Saint-Gobain、ID#SZ61192、直径3mm、ロット#2013820069)を破砕し、ふるい分けして、315~500μmの範囲の粒径を有する画分を得た。得られた粉末を空気流中で5℃/分の加熱速度を使用して650℃に焼成し、この温度で12時間保持した。
3gの量の比較試料9に、含浸前に、0.036mLのDI水で希釈された1.163mLのHNO3含有Pd(NO3)2水溶液(Pd濃度1mol/L)を含浸させた。次いで、その含浸されたt-ZrO2-S試料を、密閉容器内で室温で3時間エージングし、80℃で乾燥炉内で16時間乾燥させた。その後、その触媒試料を炉内に配置し、空気流中で5°C/分の加熱速度を使用して600℃に焼成し、この温度で12時間保持した。最終PD/t-ZrO2-S触媒試料のPd含有量は、触媒試料全体に基づき4重量%であると判定された。
正方晶のタングステン変性ジルコニア粉末(Saint-Gobain、ID#SZ61143、直径3mm、ロット#2014820006)を破砕し、ふるい分けして、315~500μmの範囲の粒径を有する画分を得た。得られた粉末を空気流中で5℃/分の加熱速度を使用して650℃に焼成し、この温度で12時間保持した。
3gの量の比較試料10に、含浸前に、0.560mLのDI水で希釈された0.580mLのHNO3含有Pd(NO3)2水溶液(Pd濃度1mol/L)を含浸させた。次いで、その含浸試料を、密閉容器内で室温で3時間エージングし、80℃で乾燥炉内で16時間乾燥させた。その後、その試料に二度目として、含浸前に、0.560mLのDI水で希釈された0.580mLのHNO3含有Pd(NO3)2水溶液(Pd濃度1mol/L)を含浸させた。次いで、その含浸試料を、密閉容器内で室温で3時間エージングし、80℃で乾燥炉内で16時間乾燥させた。最後に、その触媒試料を炉内に配置し、空気流中で5℃/分の加熱速度を使用して600℃に焼成し、この温度で12時間保持した。最終Pd/t-ZrO2-W触媒試料のPd含有量は、触媒試料全体に基づき4重量%であると判定された。
Claims (16)
- メタン酸化触媒を調製するためのプロセスであって、以下のステップ、
a.)ジルコニア前駆体を675~1050℃の範囲の温度で焼成して正方晶ジルコニアを含む焼成ジルコニア前駆体を調製するステップであって、焼成後に、検出可能な単斜晶ジルコニアが存在しないか又は存在する場合には正方晶ジルコニア対単斜晶ジルコニアの重量比は31:1を超え、前記ジルコニア前駆体は硫酸化されておらず、かつタングステン変性されていない、ステップと、
a’.)ステップa.)から得られた焼成ジルコニア前駆体に硝酸を含有する含浸溶液を含浸させて硝酸含浸ジルコニアを生成し、前記硝酸含浸ジルコニアを乾燥して乾燥された硝酸含浸ジルコニアを生成し、そして前記乾燥された硝酸含浸ジルコニアを焼成して焼成された硝酸含浸ジルコニアを生成するステップと、
b.)ステップa’.)から得られた焼成された硝酸含浸ジルコニアに貴金属前駆体含有含浸溶液を含浸させて湿潤の貴金属含浸ジルコニアを生成するステップと、
c.)前記湿潤な貴金属含浸ジルコニアを120℃以下の温度で乾燥させて乾燥させた貴金属含浸ジルコニアを生成するステップと、
d.)前記乾燥させた貴金属含浸ジルコニアを400~650℃の範囲の温度で焼成するステップと、を含み、正方晶ジルコニア対単斜晶ジルコニアの重量比は1:1~31:1の範囲である、メタン酸化触媒を調製するためのプロセス。 - ステップa.)の前記焼成後に、正方晶ジルコニア対単斜晶ジルコニアの前記重量比が、35:1~1000:1の範囲である、請求項1に記載のプロセス。
- ステップa.)の前記焼成後に、検出可能な単斜晶ジルコニアが、存在しない、請求項1に記載のプロセス。
- ステップd.)における焼成後に得られた焼成した貴金属含浸ジルコニアを、層、フィルム、またはコーティングの形態で、セラミックモノリス担体または金属モノリス担体上に堆積させることをさらに含む、請求項1に記載のプロセス。
- ステップa’.)で得られた前記焼成された硝酸含浸ジルコニアを、層、フィルム、またはコーティングの形態で、セラミックモノリス担体または金属モノリス担体上に堆積させ、その後に、ステップb.)~d.)に従って堆積された前記焼成された硝酸含浸ジルコニアを含浸させ、処理することをさらに含む、請求項1に記載のプロセス。
- ステップd.)で得られた前記貴金属含浸ジルコニアまたはステップa’.)で得られた前記焼成された硝酸含浸ジルコニアが、ウォッシュコートステップによってセラミックモノリスまたは金属モノリス上に堆積される、請求項1~5のいずれか一項に記載のプロセス。
- 前記貴金属前駆体含有含浸溶液が、パラジウム化合物、白金化合物、ロジウム化合物、およびそれらの混合物からなる群から選択される貴金属前駆体を含む、請求項1~6のいずれか一項に記載のプロセス。
- 前記貴金属前駆体含有含浸溶液が、少なくとも1つ以上の貴金属錯化化合物または貴金属キレート化合物を、錯化化合物またはキレート化合物対貴金属のモル比1:1~5:1で含む、請求項1~7のいずれか一項に記載のプロセス。
- ステップa.)における前記焼成が、800~1025℃の範囲の温度で行われる、請求項1~8のいずれか一項に記載のプロセス。
- 前記ジルコニア前駆体が、正方晶ジルコニアを含む、請求項1~9のいずれか一項に記載のプロセス。
- メタン酸化触媒において、前記単斜晶ジルコニアが、前記正方晶ジルコニア中の単斜晶ジルコニアの分散体として存在する、請求項1~10のいずれか一項に記載のプロセス。
- 前記セラミックモノリス担体または金属モノリス担体が、細孔チャネル内面を画定する細孔チャネルを含み、メタン酸化触媒が、10~250μmの範囲の厚さのコーティング、ウォッシュコート、またはフィルムの形態で前記細孔チャネル内面上に堆積される、請求項4~6のいずれか一項に記載のプロセス。
- 前記乾燥された貴金属含浸ジルコニアが、貴金属(複数可)と、正方晶および単斜晶ジルコニアとの総重量に基づいて、0.5~15重量%の範囲で貴金属を含む、請求項1~12のいずれか一項に記載のプロセス。
- 請求項1~13のいずれか一項に記載のメタン酸化触媒を調製するためのプロセスによって調製されるメタン酸化触媒。
- 酸素の存在下でメタンを含むガス流を、請求項14に記載のメタン酸化触媒と接触させ、前記ガス流中の前記メタンの少なくとも一部を酸化して二酸化炭素および水にすることによって、メタンを酸化する方法。
- メタンを含む前記ガス流が、天然ガス燃料エンジンからの排気ガスである、請求項15に記載の方法。
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BR112019004036A2 (pt) | 2019-05-28 |
CA3035129C (en) | 2024-04-09 |
CN109641200B (zh) | 2022-01-11 |
AU2017318279B2 (en) | 2019-12-05 |
ES2898788T3 (es) | 2022-03-08 |
US20210322965A1 (en) | 2021-10-21 |
KR102379498B1 (ko) | 2022-03-28 |
SG11201901346YA (en) | 2019-03-28 |
AU2017318279A1 (en) | 2019-03-07 |
EP3507009B1 (en) | 2021-09-22 |
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WO2018041632A1 (en) | 2018-03-08 |
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