JP7301541B2 - 触媒複合体及びnoxの選択接触還元におけるその使用方法 - Google Patents
触媒複合体及びnoxの選択接触還元におけるその使用方法 Download PDFInfo
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- JP7301541B2 JP7301541B2 JP2018565289A JP2018565289A JP7301541B2 JP 7301541 B2 JP7301541 B2 JP 7301541B2 JP 2018565289 A JP2018565289 A JP 2018565289A JP 2018565289 A JP2018565289 A JP 2018565289A JP 7301541 B2 JP7301541 B2 JP 7301541B2
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- 229910052751 metal Inorganic materials 0.000 claims description 151
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- 150000002500 ions Chemical class 0.000 claims description 10
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- UNYSKUBLZGJSLV-UHFFFAOYSA-L calcium;1,3,5,2,4,6$l^{2}-trioxadisilaluminane 2,4-dioxide;dihydroxide;hexahydrate Chemical compound O.O.O.O.O.O.[OH-].[OH-].[Ca+2].O=[Si]1O[Al]O[Si](=O)O1.O=[Si]1O[Al]O[Si](=O)O1 UNYSKUBLZGJSLV-UHFFFAOYSA-L 0.000 description 18
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Images
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
- F01N2330/00—Structure of catalyst support or particle filter
- F01N2330/18—Composite material
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
- F01N2370/00—Selection of materials for exhaust purification
- F01N2370/02—Selection of materials for exhaust purification used in catalytic reactors
- F01N2370/04—Zeolitic material
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
- F01N2510/00—Surface coverings
- F01N2510/06—Surface coverings for exhaust purification, e.g. catalytic reaction
- F01N2510/063—Surface coverings for exhaust purification, e.g. catalytic reaction zeolites
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/10—Capture or disposal of greenhouse gases of nitrous oxide (N2O)
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T10/00—Road transport of goods or passengers
- Y02T10/10—Internal combustion engine [ICE] based vehicles
- Y02T10/12—Improving ICE efficiencies
Description
(i)元素の周期表の第2~5族、第7~9族、および第11~14族から、好ましくは第2~4族、第13族及び第14族から選択される金属または半金属のイオンを含む金属有機構造体材料及び少なくとも1つの少なくとも単座有機化合物、
非骨格元素としての金属を含有するゼオライト材料、
任意に溶媒系、および
任意にペースト剤
を含む混合物を調製する工程、
(ii)工程(i)で得られた混合物をか焼する工程であって、
好ましくは前記金属有機構造体材料が少なくとも1つの少なくとも二座の有機化合物を含む工程、
を含む触媒の製造方法に関する。
(i.a)(ii)でか焼する前に、(i)で得られた混合物を均質化し成形する工程
を含むことが好ましい。
(i.b)(i)または(i.a)で得られた混合物を乾燥させる工程
を含むことが好ましい。
(i)元素の周期表の第2~5族、第7~9族、および第11~14族から、好ましくは第2~4族、第13族、および第14族から選択される金属または半金属のイオンを含む金属有機構造体材料、および少なくとも1つの少なくとも単座有機化合物、
非骨格元素としての金属を含有するゼオライト材料、
任意に溶媒系、および
任意にペースト剤
を含む混合物を調製する工程;
(i.A)(i)で得られた混合物を均質化する工程であって、ここにおいて、混合物は溶媒系を含み;
(i.B)支持基材を提供する工程;
(i.C)(i.A)で得られた均質化混合物で(i.B)で提供された支持基材を被覆する工程;
(i.D)任意に、(i.C)で得られた被覆支持基材を乾燥させる工程;
(i.E)(i.C)または(i.D)で得られた被覆支持基材をか焼する工程であって、好ましくは前記金属有機構造体材料が少なくとも1つの少なくとも二座有機化合物を含む
を含む触媒の製造方法に関する。
(1)NOXを含むガス流を供給する工程;
(2)(1)で供給されたガス流を、本願で定義されるような本発明の触媒の特定且つ好ましい実施形態のいずれかによる触媒と接触させる工程
を含む、NOXの選択接触還元方法に関する。
(i)元素周期表の第2~5族、第7~9族、および第11~14族から、好ましくは第2~4族、第13族、及び第14族から選択される金属または半金属のイオンを含む金属有機構造体材料、並びに少なくとも1種の少なくとも単座有機化合物、
非骨格元素としての金属を含有するゼオライト材料、
溶媒系、及び
任意にペースト剤
を含む混合物を調製する工程;
(i.A)(i)で得られた混合物を均質化する工程であって、ここで混合物は溶媒系を含んでおり;
(i.B)支持基材を提供する工程;
(i.C)(i.A)で得られた均質化混合物で(i.B)で提供された支持基材を被覆する工程;
(i.D)任意に、(i.C)で得られた被覆支持基材を乾燥させる工程;
(i.E)(i.C)または(i.D)で得られた被覆支持基材をか焼する工程
を含み、
好ましくは、金属有機構造体材料が少なくとも1種の少なくとも二座の有機化合物を含む、触媒の製造方法。
ここで、より好ましくは溶媒系は水、好ましくは蒸留水を含み、より好ましくは溶媒系は水、好ましくは蒸留水からなる、実施形態1~3の何れかに記載の製造方法。
(i)元素周期表の第2~5族、第7~9族、および第11~14族から、好ましくは第2~4族、第13族、および第14族から選択される金属または半金属のイオンを含む金属有機構造体材料、ならびに少なくとも1種の少なくとも単座有機化合物、
非骨格元素として金属を含有するゼオライト材料、
任意に溶媒系、及び
任意にペースト剤
を含む混合物を調製する工程、
(ii)(i)で得られた混合物をか焼する工程であって、好ましくは金属有機構造体材料が少なくとも1種の少なくとも二座の有機化合物を含む工程
を含む触媒の製造方法。
(i.a)(ii)でか焼する前に、(i)で得られた混合物を均質化し成形する工程
を含む、実施形態13に記載の製造方法。
(i.b)(i)または(i.a)で得られた混合物を乾燥する工程
を含む、実施形態14~15のいずれかに記載の製造方法。
ここで、少なくとも単座の有機化合物は、好ましくはそれぞれ任意に少なくとも部分的に脱プロトン化されたイミダゾール、ジカルボン酸、トリカルボン酸、テトラカルボン酸、およびそれらの2種以上の混合物からなる群から選択され、
ここで、少なくとも単座の有機化合物は、より好ましくは、それぞれ任意に少なくとも部分的に脱プロトン化されたイミダゾール、アセチレンジカルボン酸、カンファージカルボン酸(camphordicarboxylic acid)、フマル酸、コハク酸、ベンゼンジカルボン酸、ナフタレンジカルボン酸、ビフェニルジカルボン酸、ピラジンジカルボン酸、ビピリジンジカルボン酸、ベンゼントリカルボン酸、ベンゼンテトラカルボン酸、アダマンタンテトラカルボン酸、ジヒドロキシテレフタル酸、およびそれらの2種以上の混合物からなる群から選択され、
ここで前記有機化合物は、より好ましくは、任意に少なくとも部分的に脱プロトン化されたフマル酸である、実施形態1~23の何れかに記載の製造方法。
内燃機関が、好ましくは希薄燃焼機関、より好ましくはディーゼルエンジンである、排ガス処理システム。
(1)NOXを含むガス流を供給する工程;
(2)(1)で提供されたガス流を実施形態39~55のいずれかに記載の触媒と接触させる工程
を含むNOXの選択接触還元方法。
図に示されているX線回折(XRD)パターンは、それぞれCu Kアルファ-1線を使用して測定された。それぞれの回折図において、横軸に回折角2θ(°)が示されており、強度は縦軸にプロットされている。
米国特許第2012/0082864A1号の実施例6に記載されているように、フマル酸アルミニウムMOF粉末を調製した。次いで、得られた粉末を540℃へと7時間(1℃/分)、空気中(200Nl/時)で加熱し、その温度で5時間粉末を保持することによりか焼した。
515.8g(H2O中20.17質量%;0.49モル)の水酸化アダマンチルトリメチルアンモニウムを196.5g(10.92モル)の蒸留水に溶解し、これに224.3gの水酸化テトラメチルアンモニウム水溶液(H2O中25質量%;0.62モル)を加えた。そこにアルミニウムトリイソプロピレート93.5g(0.46モル)を周囲温度で攪拌しながら添加した。次に、19.0gの菱沸石種結晶(SiO2に基づいて5質量%)を混合物に添加し、続いてこれを5分間撹拌した。最後に950.8gのコロイダルシリカ(H2O中Ludox AS 40:40質量%;6.34モル)をそれに添加し、次いで混合物を20分間撹拌した。得られた混合物のpHは13.6であった。次に混合物を撹拌している2.5Lオートクレーブ(430rpm)に入れ、8時間かけて175℃の温度まで徐々に加熱し、その温度で24時間保持した。得られた固形物を濾過し、蒸留水10リットルで250μS/cm3未満の導電率まで洗浄した。次に粉末を120℃で一晩乾燥させ、続いて2℃/分の割合で600℃まで徐々に加熱することによってか焼し、その温度で6時間保持して、384gの白色粉末を得た。
参考例2からの30gの銅チャバザイトを1.5gのポリエチレンオキシド(Alkox E-160、明星化学工業株式会社製)および31gの蒸留水と混合し、得られた混合物を混練し、引き続き約10バールの圧力で押出し、直径1.5mmの紐を押し出した。次いで押出物を1時間かけて120℃に徐々に加熱し、次いでその温度で5時間保持し、続いて7時間で540℃に徐々に加熱し(1℃/分)、空気下で(200Nl/h)その温度で5時間か焼した。
参考例2からの25.5gの銅チャバザイトを1.5gのポリエチレンオキシド(Alkox E-160、明星化学工業株式会社製)、4.5gの参考例1からのフマル酸アルミニウムMOF粉末、および30gの蒸留水と混合し、得られた混合物を混練し、続いて約10バールの圧力で押出して直径1.5mmの紐を押し出した。押出物を次いで1時間かけて120℃に徐々に加熱し、次いでその温度で5時間保持し、続いて7時間で540℃に徐々に加熱し(1℃/分)、そしてその温度で空気下(200Nl/h)で5時間か焼した。
参考例2からの21gの銅チャバザイトを1.5gのポリエチレンオキシド(Alkox E-160、明星化学工業株式会社製)、9gの参考例1からのフマル酸アルミニウムMOF粉末、および32gの蒸留水と混合し、得られた混合物を混練し、次いで約10バールの圧力で押し出して直径1.5mmの紐を押し出した。次いで押出し物を1時間かけて120℃に徐々に加熱し、次いでその温度で5時間保持し、続いて7時間で540℃へと徐々に加熱し(1℃/分)、そして空気下(200Nl/h)で5時間の範囲の時間の温度で焼成した。
参考例2からの13gの銅チャバザイトを1.3gのポリエチレンオキシド(Alkox E-160、明星化学工業株式会社製)、13gの参考例1からのフマル酸アルミニウムMOF粉末、および27gの蒸留水と混合し、得られた混合物を混練し、続いて約10バールの圧力で押出して直径1.5mmの紐を押出した。押出物を次いで1時間かけて120℃に徐々に加熱し、次いでその温度で5時間保持し、続いて7時間で540℃に徐々に加熱し(1℃/分)、そしてその温度で空気下(200Nl/h)で5時間か焼した。
WO2015/185625A1の実施例3に従って得られた30gの銅チャバザイトを、1.5gのポリエチレンオキシド(Alkox E-160、明星化学工業株式会社製)および29gの蒸留水と混合し、得られた混合物を混練し、続いて約10バールの圧力で押出して直径1.5mmの紐を押出した。次いで、押出物を1時間かけて120℃に徐々に加熱し、次いでその温度で5時間保持し、続いて7時間で540℃に徐々に加熱し(1℃/分)、そしてその温度で空気下(200Nl/h)で5時間か焼した。
フマル酸ジルコニウムMOFは、WO2015/127033Aの段落[00208](MOF-801-P)に記載の手順に従って得た。
WO2015/185625A1の実施例3に従って得られた21gの銅チャバザイトを1.5gのポリエチレンオキシド(Alkox E-160、明星化学工業株式会社製)、参考例3に従って得られた9gのフマル酸ジルコニウムMOF、及び22gの蒸留水と混合し、得られた混合物を混練し、続いて約10バールの圧力で押出して直径1.5mmの紐を押出した。次いで押出物を1時間かけて120℃に徐々に加熱し、次いでその温度で5時間保持し、続いて7時間で540℃に徐々に加熱し(1℃/分)、次いで空気下(200Nl/h)でその温度で5時間か焼した。
粉体テスト
触媒試験の前に、触媒試料を、高さ500mmおよび内径18mmの厚さ1mmの鋼管(Buhlmann Groupからのグレード1.4841)からなるエージング反応器中でエージングした。管状金属マントに基づく炉を使用して反応器を目標反応温度に加熱し、これを試料の位置で内部熱電対によって監視した。飽和器を介して調製された量の水を加熱することによってガス流を水で飽和させた。水飽和ガス流を、底部から上部へと反応器を通過させた。実施例1~4及び比較例1及び2に記載されたように形成された押出物を、管状炉において、10%H2O、10%O2、残部N2を有する12,500h -1の空間速度のガス流中で6時間、850℃で水熱的にエージングさせた。
本発明の触媒で被覆されたフィルタ基材に対して行われたコア試験のために、比較例2に従って得られたCu交換ゼオライトの試料を、均質な混合物が得られるまで連続的な撹拌下で蒸留水と混合し、続いて粉砕した。次に、参考例1からのフマル酸アルミニウムMOFのスラリーを4~6μmのD90の範囲に予備粉砕し、続いて予備粉砕したゼオライトスラリーと混合して、3質量%のアルミナ装填量に相当する、10質量%のフマル酸アルミニウムを含有する最終スラリーを得た。次いで、スラリーを、2回の浸漬の間に乾燥工程を含む浸漬によって高多孔度SiCフィルタ(1.5”×5.54”)上に被覆し、次いで450℃で被覆した基材のか焼を行った。比較のために、フマル酸アルミニウムMOFを使用せずにこの手順を繰り返した。Cu-CHA含有コアについてのウォッシュコート装填量は2g/in3として得られ、Cu-CHA/Al2O3含有コアについては1.9g/in3として得られた。
Claims (11)
- NOXの選択接触還元および/または排ガスの処理のために使用される触媒の製造方法であって、
(i)Alおよび/またはZrである金属のイオン、ならびに単座の有機化合物、二座の有機化合物、三座の有機化合物、四座の有機化合物またはそれらの2種以上の混合物を含む金属有機構造体材料、
非骨格元素としての金属を含むゼオライト材料、
溶媒系、及び
任意にペースト剤
を含む混合物を調製する工程;
(i.A)工程(i)で得られた混合物を均質化する工程、ここにおいて混合物は溶媒系を含んでおり;
(i.B)支持基材を提供する工程;
(i.C)工程(i.B)で提供された支持基材を、工程(i.A)で得られた均質化された混合物で被覆する工程;
(i.D)任意に、工程(i.C)で得られた被覆された支持基材を乾燥する工程;
(i.E)工程(i.C)又は(i.D)で得られた被覆された支持基材をか焼する工程を含み、且つ
(i.E)工程におけるか焼が300℃から750℃の範囲の温度で3時間から7時間の範囲の期間で実施され;
得られた触媒が非晶質メソポーラス金属酸化物を含む、触媒の製造方法。 - 前記支持基材が、顆粒、ペレット、メッシュ、リング、球、円柱、中空円柱、モノリス並びにこれらの2種以上の混合物及び組み合わせからなる群から選択される請求項1に記載の触媒の製造方法。
- NOXの選択接触還元および/または排ガスの処理のために使用される触媒の製造方法であって、
(i)Alおよび/またはZrである金属のイオン、ならびに単座の有機化合物、二座の有機化合物、三座の有機化合物、四座の有機化合物またはそれらの2種以上の混合物を含む金属有機構造体材料、
非骨格元素としての金属を含むゼオライト材料、
任意に溶媒系、及び
任意にペースト剤を含む混合物を調製する工程、
(ii)工程(i)で得られた混合物をか焼する工程であって、か焼が250℃から560℃の範囲の温度で3時間から7時間の範囲の期間で実施される工程
を含み、且つ
得られた触媒が非晶質メソポーラス金属酸化物を含む、触媒の製造方法。 - 前記ゼオライト材料に含まれる非骨格元素としての前記金属が、元素の周期表の第3~12族の元素およびこれらの2種以上の組み合わせからなる群から選択される請求項1~3の何れか一項に記載の触媒の製造方法。
- 非晶質メソポーラス金属酸化物とゼオライト材料とを含有する複合材料を含み、NOXの選択接触還元および/または排ガスの処理のために使用される触媒であって、
前記金属はAlおよび/またはZrであり、
前記ゼオライト材料が非骨格元素として金属を含有し、
前記複合材料が上部に施された支持基材をさらに含み、
前記ゼオライト材料がCHA型の骨格構造を有する、触媒。 - 前記非晶質メソポーラス金属酸化物が、2nm~50nmの範囲で測定された多孔度に基づいて3~10nmの範囲の平均孔径を示し、
前記平均孔径がISO15901-2:2006に従って決定される、請求項5に記載の触媒。 - 前記支持基材が、顆粒、ペレット、メッシュ、リング、球、円柱、中空円柱、モノリス並びにこれらの2種以上の混合物及び組み合わせからなる群から選択される請求項5~6の何れか一項に記載の触媒。
- 前記支持基材が、セラミック及び/又は金属物質を含む、請求項5~7の何れか一項に記載の触媒。
- 前記ゼオライト材料に含まれる非骨格元素としての前記金属が、元素の周期表の第3~12族の元素及びこれらの2種以上の組み合わせからなる群から選択される請求項5~8の何れか一項に記載の触媒。
- NOXの選択接触還元のための方法であって、
(1)NOXを含むガス流を供給する工程;
(2)工程(1)で供給されたガス流を請求項5~9の何れか一項に記載の触媒に接触させる工程を含む方法。 - 排ガスの処理における請求項5~9の何れか一項に記載の触媒の使用方法。
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