JP2017029981A - 触媒製造方法 - Google Patents
触媒製造方法 Download PDFInfo
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- JP2017029981A JP2017029981A JP2016162239A JP2016162239A JP2017029981A JP 2017029981 A JP2017029981 A JP 2017029981A JP 2016162239 A JP2016162239 A JP 2016162239A JP 2016162239 A JP2016162239 A JP 2016162239A JP 2017029981 A JP2017029981 A JP 2017029981A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 84
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 90
- 239000000843 powder Substances 0.000 claims abstract description 68
- 239000000463 material Substances 0.000 claims abstract description 36
- 239000000654 additive Substances 0.000 claims abstract description 10
- 230000000996 additive effect Effects 0.000 claims abstract description 10
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- 229910052751 metal Inorganic materials 0.000 claims description 42
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- 150000002736 metal compounds Chemical class 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 17
- 239000007789 gas Substances 0.000 claims description 15
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 13
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 13
- 239000012254 powdered material Substances 0.000 claims description 11
- 229910021536 Zeolite Inorganic materials 0.000 claims description 10
- 239000010457 zeolite Substances 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 230000003647 oxidation Effects 0.000 claims description 9
- 238000007254 oxidation reaction Methods 0.000 claims description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
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- 150000003623 transition metal compounds Chemical class 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
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- 229910052741 iridium Inorganic materials 0.000 claims description 6
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- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 claims description 4
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
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- 229910003455 mixed metal oxide Inorganic materials 0.000 claims description 4
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- 229910052759 nickel Inorganic materials 0.000 claims description 4
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 4
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 4
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
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- 238000001179 sorption measurement Methods 0.000 claims description 4
- 229910052718 tin Inorganic materials 0.000 claims description 4
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- 229910052721 tungsten Inorganic materials 0.000 claims description 4
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- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 2
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- MMCOUVMKNAHQOY-UHFFFAOYSA-N carbonoperoxoic acid Chemical class OOC(O)=O MMCOUVMKNAHQOY-UHFFFAOYSA-N 0.000 claims description 2
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- 239000001272 nitrous oxide Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
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- XFWJKVMFIVXPKK-UHFFFAOYSA-N calcium;oxido(oxo)alumane Chemical compound [Ca+2].[O-][Al]=O.[O-][Al]=O XFWJKVMFIVXPKK-UHFFFAOYSA-N 0.000 description 1
- NKCVNYJQLIWBHK-UHFFFAOYSA-N carbonodiperoxoic acid Chemical compound OOC(=O)OO NKCVNYJQLIWBHK-UHFFFAOYSA-N 0.000 description 1
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- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 1
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- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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Abstract
Description
(i)粉末化触媒又は触媒担体材料の層を形成し、
(ii)予め定められたパターンに従って上記層中の粉末を結合又は融合させ、
(iii)(i)及び(ii)を繰り返して何層も重ねて成形ユニットを形成し、
(iv)場合によっては上記成形ユニットに触媒材料を適用する
工程を含む方法を提供する。
好ましくは、成形ユニットは、断面が円形、楕円形又は多角形、例えば三角形、正方形、長方形又は六角形であってもよい一又は複数の貫通孔を有する。貫通孔は成形ユニットの長軸に対して、平行に走る二以上の貫通孔、又は様々な角度で成形ユニットを貫通して走る非平行の孔を含みうる。一般的なペレット化及び押出技術を使用すると現在はできない、湾曲した貫通孔もまたALM法を使用して作製することができる。
触媒が金属粉末である場合、好ましくは金属粉末は、場合によっては一又は複数の遷移金属と混合されて、例えばPt、Pd、Ir、Ru、Reの一又は複数を含む貴金属触媒粉末を含む。
あるいは、触媒粉末はゼオライトを含みうる。
あるいは、触媒担体粉末はゼオライトを含みうる。
成形ユニットに塗布される触媒材料は金属、金属化合物又はゼオライトを含みうる。
バーンアウト添加剤を触媒粉末又はバインダーに含めて、得られる成形ユニットの孔隙率を制御してもよい。
ALM法を使用して調製される触媒は、反応物質混合物が触媒反応を行わしめる条件下で触媒成形ユニットと接触させる。あるいは、成形ユニットが収着プロセスにおいて使用され、液体又は気体でありうるプロセス流体から物質を触媒的に除去されうる。
図1に図示したワイヤフレームアンモニア酸化触媒を、市販のペレット化アンモニア酸化触媒と比較した。
図1に係る成形ユニットにおける有効面積はおよそ545mm2である。形状体積はおよそ135mm3である。充填体積はおよそ90mm3と推定される。
これを元にすると、同じ操作条件下で同じ変換効率が一般的なペレットの数の15−16%で得られうることが予想される。
図2の12面体フレーム構造を、Phenix Systems PXシリーズのレーザー焼結機を使用して調製した。およそ10ミクロンの平均粒径の未変性アルミナ粉末を用い、レーザー溶融前にそれぞれの新粉末層を圧密化し、およそ100ミクロンのステップを使用して、ビルドが達成された。300Wのファイバーレーザーを使用し、標準的なソフトウェアによって駆動されるトラックに沿ってアルミナを溶融させた。ビルド完了時は部品は壊れやすく、粉末床から注意して取り除いた。強度の増強は約1800℃までの温度でのビルド後焼結によって達成されうる。
図3のアルミナ−シリカ12面体形状の「3Dプリンティング」を、Z−Corp 3Dプリンターと標準的な市販の結合媒を使用して達成した。中央値がおよそ30ミクロンの粒径の粉末を、常套的な加工条件を使用して100ミクロンステップでプリントした。製造した未焼結(green)構造体を、およそ8時間にわたってゆっくりした温度の立ち上がりとしておよそ1000℃まで燃やし続け、結合剤を燃やして除去し、完全な状態を損ねないで部品を緻密化(収縮)させた。完了時に、十分に強く触媒コーティングに耐える多量の3D形状体が製造された。
Claims (39)
- 添加剤層法を使用する触媒の製造方法であって、
(i)粉末化触媒又は触媒担体材料の層を形成し、
(ii)予め定められたパターンに従って上記層中の粉末を結合又は融合させ、
(iii)(i)及び(ii)を繰り返して何層も重ねて成形ユニットを形成し、
(iv)場合によっては上記成形ユニットに触媒材料を適用する
ことを含む方法。 - 粉末化材料が触媒粉末である請求項1に記載の方法。
- 触媒粉末が金属粉末又は粉末化金属化合物を含む請求項2に記載の方法。
- 触媒粉末が、Na、K、Mg、Ca、Ba、Al、Si、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、Y、Zr、Nb、Mo、Ru、Rh、Pd、Ag、Sn、Sb、La、Hf、W、Re、Ir、Pt、Au、Pb、又はCeからなる群から選択される金属を含む一又は複数の金属又は金属化合物を含む請求項2又は請求項3に記載の方法。
- 触媒粉末が、Pt、Pd、Ir、Ru又はReの一又は複数を含む、貴金属触媒粉末を含む請求項2から4の何れか一項に記載の方法。
- 触媒粉末が、金属酸化物、金属水素化物、金属炭酸塩、金属ヒドロキシ炭酸塩又はその混合物から選択される遷移金属化合物を含む請求項2から4の何れか一項に記載の方法。
- 遷移金属酸化物が単一の又は混合された金属酸化物か又は二以上の遷移金属酸化物を含む組成物を含む請求項6に記載の方法。
- 触媒粉末が一又は複数の不活性材料を更に含む請求項2から7の何れか一項に記載の方法。
- 不活性材料が、アルミナ、シリカ、窒化珪素、炭化珪素、炭素及びそれらの混合物からなる群から選択される請求項8に記載の方法。
- 触媒粉末がゼオライトを含む請求項2に記載の方法。
- 粉末化材料が触媒担体粉末であり、上記成形ユニットに触媒材料を適用することを含む、請求項1に記載の方法。
- 触媒担体粉末が一又は複数の不活性材料を含む請求項11に記載の方法。
- 不活性材料が、アルミナ、シリカ、窒化珪素、炭化珪素、炭素及びそれらの混合物からなる群から選択される請求項12に記載の方法。
- 触媒担体粉末が、一又は複数の金属酸化物、金属水素化物、金属炭酸塩、金属ヒドロキシ炭酸塩又はそれらの混合物から選択される、ランタニド金属化合物及びアクチニド金属化合物を含む一又は複数の遷移金属化合物を含む請求項11から13の何れか一項に記載の方法。
- 遷移金属化合物が単一又は混合された金属酸化物か又は二以上の遷移金属酸化物を含む組成物を含む請求項14に記載の方法。
- 触媒担体粉末がアルミナ、金属アルミネート、シリカ、アルミノ-シリケート、チタニア、ジルコニア、亜鉛酸化物、又はそれらの混合物を含む請求項12から15の何れか一項に記載の方法。
- 触媒担体粉末が金属粉末を含む請求項11に記載の方法。
- 金属粉末が貴金属粉末又は非貴金属粉末を含む請求項17に記載の方法。
- 非貴金属粉末がフェライト合金又は鋼を含む請求項18に記載の方法。
- 触媒担体粉末がゼオライトを含む請求項11に記載の方法。
- 成形ユニットに適用される触媒材料が金属、金属化合物又はゼオライトを含む請求項11から20の何れか一項に記載の方法。
- 金属が成形ユニットに金属蒸着によって適用される請求項21に記載の方法。
- 金属、金属化合物又はゼオライトが、金属、金属化合物又はゼオライトの溶液又は分散体から成形ユニットに適用される請求項21に記載の方法。
- 金属又は金属化合物が、Na、K、Mg、Ca、Ba、Al、Si、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、Y、Zr、Nb、Mo、Ru、Rh、Pd、Ag、Sn、Sb、La、Hf、W、Re、Ir、Pt、Au、Pb、又はCeからなる群から選択される一又は複数の金属を含む請求項22又は請求項23に記載の方法。
- 粉末化材料が1から200マイクロメートルの平均粒径D50を有する請求項1から24の何れか一項に記載の方法。
- 添加剤層法が3Dプリンティング、ステレオリソグラフィー又はレーザ焼結法を含む請求項1から25の何れか一項に記載の方法。
- 各層の粉末がレーザーによって融合される請求項1から26の何れか一項に記載の方法。
- 各層の粉末がバインダーと共に結合される請求項1から27の何れか一項に記載の方法。
- バインダーが無機バインダー又は有機バインダーである請求項28に記載の方法。
- 得られる成形ユニットの細孔度を制御するために触媒粉末又はバインダー中にバーンアウト添加剤が含まれる請求項28又は請求項29に記載の方法。
- 成形ユニットが加熱工程に供される請求項1から30の何れか一項に記載の方法。
- 一又は複数の還元性金属化合物を含む成形ユニットが還元工程に供される請求項1から31の何れか一項に記載の方法。
- 還元工程が、成形ユニットを150〜800℃の温度範囲の水素含有ガス流に曝露することによって実施される請求項33に記載の方法。
- 成形ユニット中の還元された金属が、酸素含有ガス流への成形ユニットの制御された曝露によって不動態化されて、上記還元金属上に不動態化層が形成される請求項33に記載の方法。
- 成形ユニットが、内部に複数の内部強化ロッドを有しうる空隙空間を含むワイヤフレーム構造又は骨格フレームワークである請求項1から34の何れか一項に記載の方法。
- 請求項1から35の何れか一項に記載の方法によって得られた触媒。
- 請求項36に記載の又は請求項1から35の何れか一項に記載の方法に従って調製された触媒を使用する方法であって、反応物混合物を触媒成形ユニットに触媒反応又は収着を行わしめる条件下で接触させることを含む方法。
- 水素化脱硫を含む水素化処理、水素化、プレリフォーミング、接触スチームリフォーミング、オートサーマルリフォーミング及び二次リフォーミングを含むスチームリフォーミング及び鉄の直接還元に使用されるリフォーミングプロセス、接触部分酸化、等温シフト、サワーシフト、低温シフト、中間温度シフト、中温シフト及び高温シフト反応を含む水性ガスシフト、メタン化合成、フィッシャー・トロプシュ反応による炭化水素合成、メタノール合成、アンモニア合成、アンモニア酸化及び亜酸化窒素分解反応、又は内燃機関又は発電所排気ガスの選択的酸化又は還元反応から選択される触媒反応を含む請求項37に記載の方法。
- 汚染ガス又は液体流体流からの水銀及びヒ素等の重金属又は硫黄化合物、又は内燃機関又は発電所の排気ガスからのパティキュレートマターの回収から選択される収着を含む請求項37に記載の方法。
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WO2012032325A1 (en) | 2012-03-15 |
US9278338B2 (en) | 2016-03-08 |
JP6389490B2 (ja) | 2018-09-12 |
US20160136634A1 (en) | 2016-05-19 |
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GB201014950D0 (en) | 2010-10-20 |
EP2752244A1 (en) | 2014-07-09 |
AU2011300512B2 (en) | 2017-02-02 |
EP2613879B2 (en) | 2024-02-14 |
CN105107551A (zh) | 2015-12-02 |
US20130230721A1 (en) | 2013-09-05 |
RU2013115444A (ru) | 2014-10-20 |
CN103118782B (zh) | 2015-11-25 |
RU2598381C2 (ru) | 2016-09-27 |
CN103118782A (zh) | 2013-05-22 |
EP2613879B1 (en) | 2021-01-27 |
CN105195235A (zh) | 2015-12-30 |
RU2016134735A (ru) | 2018-12-11 |
AU2011300512A1 (en) | 2013-05-02 |
BR112013004969A2 (pt) | 2016-08-16 |
US9839907B2 (en) | 2017-12-12 |
EP2752244B1 (en) | 2021-01-27 |
RU2016134735A3 (ja) | 2019-12-04 |
EP2613879A1 (en) | 2013-07-17 |
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