JP6934041B2 - ナノサイズのゼオライト担持触媒およびその製造方法 - Google Patents
ナノサイズのゼオライト担持触媒およびその製造方法 Download PDFInfo
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- JP6934041B2 JP6934041B2 JP2019503635A JP2019503635A JP6934041B2 JP 6934041 B2 JP6934041 B2 JP 6934041B2 JP 2019503635 A JP2019503635 A JP 2019503635A JP 2019503635 A JP2019503635 A JP 2019503635A JP 6934041 B2 JP6934041 B2 JP 6934041B2
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- zeolite
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- catalyst
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- 239000003054 catalyst Substances 0.000 title claims description 109
- 239000002105 nanoparticle Substances 0.000 title claims description 85
- 238000004519 manufacturing process Methods 0.000 title description 6
- 239000010457 zeolite Substances 0.000 claims description 79
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 73
- 239000000203 mixture Substances 0.000 claims description 69
- 229910021536 Zeolite Inorganic materials 0.000 claims description 66
- 238000000034 method Methods 0.000 claims description 62
- 239000002243 precursor Substances 0.000 claims description 59
- 239000012876 carrier material Substances 0.000 claims description 45
- 229910044991 metal oxide Inorganic materials 0.000 claims description 45
- 150000004706 metal oxides Chemical class 0.000 claims description 45
- 239000011148 porous material Substances 0.000 claims description 42
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 37
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 34
- 239000013078 crystal Substances 0.000 claims description 30
- 229910052751 metal Inorganic materials 0.000 claims description 24
- 239000002184 metal Substances 0.000 claims description 24
- 238000004517 catalytic hydrocracking Methods 0.000 claims description 17
- 239000000126 substance Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 230000008569 process Effects 0.000 claims description 16
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 16
- 229910001868 water Inorganic materials 0.000 claims description 16
- 239000000377 silicon dioxide Substances 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 14
- 230000003197 catalytic effect Effects 0.000 claims description 13
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 claims description 13
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical group [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 claims description 13
- 239000012685 metal catalyst precursor Substances 0.000 claims description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 9
- 150000002739 metals Chemical class 0.000 claims description 7
- 238000010335 hydrothermal treatment Methods 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 229910052750 molybdenum Inorganic materials 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 229910052721 tungsten Inorganic materials 0.000 claims description 5
- 230000002194 synthesizing effect Effects 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 2
- 238000005470 impregnation Methods 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 13
- 239000000243 solution Substances 0.000 description 11
- 238000011282 treatment Methods 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 8
- WQOXQRCZOLPYPM-UHFFFAOYSA-N dimethyl disulfide Chemical compound CSSC WQOXQRCZOLPYPM-UHFFFAOYSA-N 0.000 description 8
- 238000005984 hydrogenation reaction Methods 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- 239000003921 oil Substances 0.000 description 7
- 238000000926 separation method Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 6
- 230000008025 crystallization Effects 0.000 description 6
- 238000005336 cracking Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 229930195733 hydrocarbon Natural products 0.000 description 5
- 150000002430 hydrocarbons Chemical class 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 238000001354 calcination Methods 0.000 description 4
- 239000000295 fuel oil Substances 0.000 description 4
- 229910021485 fumed silica Inorganic materials 0.000 description 4
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- 229910002016 Aerosil® 200 Inorganic materials 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- -1 WO 3 Chemical class 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910000323 aluminium silicate Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 239000013626 chemical specie Substances 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000012263 liquid product Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 229910003208 (NH4)6Mo7O24·4H2O Inorganic materials 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 235000003385 Diospyros ebenum Nutrition 0.000 description 1
- 241000792913 Ebenaceae Species 0.000 description 1
- 229910018590 Ni(NO3)2-6H2O Inorganic materials 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 235000012438 extruded product Nutrition 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 150000002605 large molecules Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052680 mordenite Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005486 sulfidation Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Description
ナノサイズのゼオライトを形成するために、ヒュームドシリカ(AEROSIL(登録商標)200、エボニックインダストリーズより入手可能)、アルミニウム粉末、およびテトラエチル水酸化アンモニウム(TEAOH)(35wt%水溶液、アルドリッチより入手可能)を、それぞれ、シリカ供給源、アルミニウム供給源、およびテンプレート剤として使用した。前駆体ゲルは、30TEAOH:50SiO2:Al2O3:750H2Oの酸化物モル組成比を有していた。金属アルミニウムを、TEAOH含有水溶液の一部に溶解して透明な溶液を作り、次に、ヒュームドシリカおよびTEAOH含有水溶液の他の部分により作製したスラリーに加えた。形成したアルミノケイ酸塩流体ゲルを、ビーカー内で周囲温度にて4時間撹拌し、次に、125ミリリットル(mL)のポリテトラフルオロエチレン(PTFE)で線を引いたステンレス・スティールのオートクレーブに移した。結晶化を、413ケルビン(K)にて、オーブン内での静止状態下、またはオイルバス中60rpmでの回転状態下のいずれかで生じさせた。様々な結晶化期間の後、オートクレーブをクエンチして結晶化プロセスを停止させた。
従来のナノサイズのゼオライト触媒を、以下のプロセスにより調製した。ヒュームドシリカ(AEROSIL(登録商標)200、エボニックインダストリーズより入手可能)、アルミニウム粉末、およびTEAOH(35wt%水溶液、アルドリッチより入手可能)を、それぞれ、シリカ供給源、アルミニウム供給源、およびテンプレート剤として使用した。前駆体ゲルは、酸化物モル組成30TEAOH:50SiO2:Al2O3:750H2Oを有していた。金属アルミニウムを、TEAOH含有水溶液の一部に溶解して透明な溶液を作り、次に、ヒュームドシリカおよびTEAOH含有水溶液の他の部分により作製したスラリーに加えた。形成したアルミノケイ酸塩流体ゲルを、ビーカー内で周囲温度にて4時間撹拌し、次に、125mLのPTFEで線を引いたステンレス・スティールのオートクレーブに移した。結晶化を、413Kにて、オーブン内での静止状態下、またはオイルバス中での回転状態(60rpm)下のいずれかで生じさせた。様々な結晶化期間の後、オートクレーブをクエンチして結晶化プロセスを停止させた。最終生成物を、液体から16,000rpmの遠心分離を使用して分離し、pH<9.0まで脱イオン水で数回洗浄し、383Kにてオーブン内で乾燥させた。
により決定した。実施例1および実施例2の触媒についての触媒活性試験の結果を、表3において示す。
以下、本発明の好ましい実施形態を項分け記載する。
実施形態1
コロイド状混合物を金属酸化物担体物質と合わせて担体前駆物質を形成する工程であって、ここで、前記コロイド状混合物は、ナノサイズのゼオライト結晶を含み、前記ナノサイズのゼオライト結晶は、平均サイズ100nm未満を有する、形成する工程、
前記担体前駆物質を処理して担体物質を形成する工程、および、
前記担体物質に1つまたは複数の金属を含浸させて前記ゼオライト担持触媒を形成する工程、
を含む、ゼオライト担持触媒を合成する方法。
実施形態2
前記コロイド状混合物が、第4級アンモニウム塩、シリカ、アルミナ、および水を少なくとも含有する混合物をオートクレーブすることにより形成される、実施形態1に記載の方法。
実施形態3
前記第4級アンモニウム塩が、テトラメチルアンモニウムヒドロキシド(TEAOH)である、実施形態2に記載の方法。
実施形態4
第4級アンモニウム塩、シリカ、アルミニウム、および水を少なくとも含有する前記混合物が、
アルミナ1モル、
前記第4級アンモニウム塩15モル〜35モル、
シリカ20モル〜80モル、および
水250モル〜1000モル、のモル比を有する、実施形態2に記載の方法。
実施形態5
ナノサイズのゼオライトを含む前記コロイド状混合物と合わされる前記金属酸化物担体物質が、
孔サイズ0.4mL/g〜0.6mL/gを有する細孔サイズ金属酸化物、および、
孔サイズ0.8mL/g〜1.2mL/gを有する大孔サイズ金属酸化物、を含む、実施形態1に記載の方法。
実施形態6
前記細孔サイズ金属酸化物が、前記大孔サイズ金属酸化物が、ナノサイズのゼオライトを含む前記コロイド状混合物と合わされる前に、ナノサイズのゼオライトを含む前記コロイド状混合物と合わされる、実施形態5に記載の方法。
実施形態7
前記担体前駆物質が硝酸をさらに含む、実施形態1に記載の方法。
実施形態8
前記金属酸化物担体物質がアルミナである、実施形態1に記載の方法。
実施形態9
前記金属酸化物担体物質が多孔質アルミナである、実施形態1に記載の方法。
実施形態10
前記担体前駆物質を処理する前記工程が、前記担体前駆物質を乾燥させて押出可能な物質を形成することを含む、実施形態1に記載の方法。
実施形態11
前記担体前駆物質を処理する前記工程が、前記担体前駆物質を成形することを含む、実施形態1に記載の方法。
実施形態12
前記担体前駆物質が押し出される、実施形態11に記載の方法。
実施形態13
前記担体前駆物質を処理する前記工程が、前記担体前駆物質を水熱で処理することを含む、実施形態1に記載の方法。
実施形態14
前記担体前駆物質を水熱で処理することが、前記担体前駆物質を圧力2bar〜4barに温度450℃〜600℃で0.5時間〜3時間曝露することを含む、実施形態13に記載の方法。
実施形態15
前記水熱処理が、自己発生した蒸気を生み出す、実施形態13に記載の方法。
実施形態16
前記担体物質に含浸させる前記工程が、前記担体物質を、1つまたは複数の金属触媒前駆体を含む溶液と接触させることを含み、ここで、前記金属触媒前駆体が、Ni、W、Mo、Coのうちの1つまたは複数を含む、実施形態1に記載の方法。
実施形態17
多孔質アルミナ20wt%〜75wt%、
金属触媒物質20wt%〜30wt%、および
ナノサイズのゼオライト5wt%〜50wt%、を含むゼオライト担持触媒であって、
ここで、
前記ナノサイズのゼオライトが、平均サイズ100nm未満を有し、
前記ゼオライト担持触媒が、表面積少なくとも180m 2 /gを有する、ゼオライト担持触媒。
実施形態18
前記ゼオライト担持触媒が、孔体積少なくとも0.45mL/gを有する、実施形態17に記載の方法。
実施形態19
前記ゼオライト担持触媒が、孔サイズ少なくとも9.5nmを有する、実施形態17に記載の方法。
実施形態20
前記金属触媒物質が、WO 3 、MoO 3 、NiO、およびCoOのうちの1つまたは複数を含む、実施形態17に記載の方法。
Claims (19)
- コロイド状混合物を金属酸化物担体物質と合わせて担体前駆物質を形成する工程であって、ここで、前記コロイド状混合物は、平均サイズ100nm未満を有するナノサイズのゼオライト結晶を含み、前記金属酸化物担体物質は、孔体積0.4mL/g〜0.6mL/gを有する細孔サイズ金属酸化物、および孔体積0.8mL/g〜1.2mL/gを有する大孔サイズ金属酸化物を含む、形成する工程、
前記担体前駆物質を処理して担体物質を形成する工程、および、
前記担体物質に1つまたは複数の金属を含浸させて前記ゼオライト担持触媒を形成する工程、
を含む、ゼオライト担持触媒を合成する方法。 - 前記コロイド状混合物が、第4級アンモニウム塩、シリカ、アルミナ、および水を少なくとも含有する混合物をオートクレーブすることにより形成される、請求項1に記載の方法。
- 前記第4級アンモニウム塩が、テトラエチルアンモニウムヒドロキシド(TEAOH)である、請求項2に記載の方法。
- 第4級アンモニウム塩、シリカ、アルミニウム、および水を少なくとも含有する前記混合物が、
アルミナ1モル、
前記第4級アンモニウム塩15モル〜35モル、
シリカ20モル〜80モル、および
水250モル〜1000モル、のモル比を有する、請求項2に記載の方法。 - 前記細孔サイズ金属酸化物が、前記大孔サイズ金属酸化物が、ナノサイズのゼオライトを含む前記コロイド状混合物と合わされる前に、ナノサイズのゼオライトを含む前記コロイド状混合物と合わされる、請求項1に記載の方法。
- 前記担体前駆物質が硝酸をさらに含む、請求項1に記載の方法。
- 前記金属酸化物担体物質がアルミナである、請求項1に記載の方法。
- 前記金属酸化物担体物質が多孔質アルミナである、請求項1に記載の方法。
- 前記担体前駆物質を処理する前記工程が、前記担体前駆物質を乾燥させて押出可能な物質を形成することを含む、請求項1に記載の方法。
- 前記担体前駆物質を処理する前記工程が、前記担体前駆物質を成形することを含む、請求項1に記載の方法。
- 前記担体前駆物質が押し出される、請求項10に記載の方法。
- 前記担体前駆物質を処理する前記工程が、前記担体前駆物質を水熱で処理することを含む、請求項1に記載の方法。
- 前記担体前駆物質を水熱で処理することが、前記担体前駆物質を圧力2bar(200kPa)〜4bar(400kPa)に温度450℃〜600℃で0.5時間〜3時間曝露することを含む、請求項12に記載の方法。
- 前記水熱処理が、自己発生した蒸気を生み出す、請求項12に記載の方法。
- 前記担体物質に含浸させる前記工程が、前記担体物質を、1つまたは複数の金属触媒前駆体を含む溶液と接触させることを含み、ここで、前記金属触媒前駆体が、Ni、W、Mo、Coのうちの1つまたは複数を含む、請求項1に記載の方法。
- 多孔質アルミナ20重量%〜75重量%、
WO 3 含有金属触媒物質20重量%〜30重量%、および
ナノサイズのゼオライト5重量%〜50重量%、を含むゼオライト担持触媒であって、
ここで、
前記多孔質アルミナは、孔体積0.4mL/g〜0.6mL/gを有する細孔サイズアルミナ、および孔体積0.8mL/g〜1.2mL/gを有する大孔サイズアルミナを含み、
前記ナノサイズのゼオライトが、平均サイズ100nm未満を有し、
前記ゼオライト担持触媒が、表面積少なくとも180m2/gを有する、ゼオライト担持水素化分解触媒。 - 前記ゼオライト担持触媒が、孔体積少なくとも0.45mL/gを有する、請求項16に記載のゼオライト担持水素化分解触媒。
- 前記ゼオライト担持触媒が、孔サイズ少なくとも9.5nmを有する、請求項16に記載のゼオライト担持水素化分解触媒。
- 前記金属触媒物質が、さらに、MoO3、NiO、およびCoOのうちの1つまたは複数を含む、請求項16に記載のゼオライト担持水素化分解触媒。
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