JP2022028661A - 粒子状安定化発泡体で基材をコーティングする方法 - Google Patents
粒子状安定化発泡体で基材をコーティングする方法 Download PDFInfo
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- B32B5/16—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by features of a layer formed of particles, e.g. chips, powder or granules
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- F01N3/033—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters in combination with other devices
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- F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
- F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
- F01N3/105—General auxiliary catalysts, e.g. upstream or downstream of the main catalyst
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- F01N3/18—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by methods of operation; Control
- F01N3/20—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by methods of operation; Control specially adapted for catalytic conversion ; Methods of operation or control of catalytic converters
- F01N3/2066—Selective catalytic reduction [SCR]
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- F01N3/24—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by constructional aspects of converting apparatus
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- F01N3/24—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by constructional aspects of converting apparatus
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- F01N3/24—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by constructional aspects of converting apparatus
- F01N3/28—Construction of catalytic reactors
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- F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
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- F01N3/24—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by constructional aspects of converting apparatus
- F01N3/28—Construction of catalytic reactors
- F01N3/2803—Construction of catalytic reactors characterised by structure, by material or by manufacturing of catalyst support
- F01N3/2825—Ceramics
- F01N3/2828—Ceramic multi-channel monoliths, e.g. honeycombs
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- B01D2255/20—Metals or compounds thereof
- B01D2255/207—Transition metals
- B01D2255/20761—Copper
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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- F01N2370/02—Selection of materials for exhaust purification used in catalytic reactors
- F01N2370/04—Zeolitic material
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- 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
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Abstract
Description
(a)基材の第1の端部におけるチャネルの開放端を通じて、複数のチャネルを含む基材に発泡体を導入すること、及び
(b)任意選択的に、(i)基材の第2の端部におけるチャネルの開放端に真空を、及び/又は(ii)基材の第1の端部におけるチャネルの開放端に圧力を適用すること
を含み、ここで、発泡体は微粒子状材料を含み、且つ発泡体は安定化粒子である。
(a)耐火性酸化物の粒子、好ましくは≦約50m2/gの平均比表面積を有する耐火性酸化物の粒子、及び/又は
(b)Pt合金金属の粒子、好ましくは≧約10nmの平均粒子サイズ及び/又は≦約10%の分散を有するPt合金金属の粒子
を含むか、又は本質的にそれらからなる。
(a)触媒材料上に配置又は担持されうる;及び/又は
(b)基材上に直接配置されうる[すなわち捕獲材料は基材の表面と接触する];及び/又は
(c)触媒材料と接触しうる[すなわち捕獲材料は触媒材料に隣接又は当接する]。
本明細書及び添付の特許請求の範囲で使用される場合、単数形「a」、「an」及び「the」は、文脈が相反することを明記しないかぎり、複数の言及を含む。したがって、例えば、「微粒子状材料」への言及は、二以上の微粒子状材料の混合物等を含む。
確立されたコーティング法は、国際公開第99/47260号、同第2011/080525号及び同第2014/19568号の開示及び教示によるものである。
適切な量の粉末と水を混合することによってガンマ-アルミナ懸濁液を調製pHをHNO3を用いて5.5に調整し、懸濁液を均質になるまで撹拌した。懸濁液を粉砕し、d50を<6ミクロンにした。
ベーマイト粉末(Sasolにより供給されるアルミナ)を脱塩水に添加した。この懸濁液を3時間撹拌した。CHA構造を有し、SARが25であるCu交換小細孔ゼオライト(3.0重量%Cu)をゆっくりと添加した(ゼオライト:ベーマイト比9:1)。この懸濁液の総固体含有量は31重量%であった。
実施例2のものと同様の組成の懸濁液を希釈し、その後均質になるまで撹拌して、懸濁液を調製した。
実施例2及び3のような三つの懸濁液をそれぞれ調製した。これらの各吉草酸(表2に記載の量)を添加し、水酸化テトラ-n-プロピル-アンモニウム(TPAOH)でpHを4.75の目標に調整した。泡立て器を備えたKenwood Chef ClassicTMフードミキサーを使用して懸濁液に空気を導入し、最大速度で10分間撹拌して発泡体を生成した。
国際公開第2011/080525号に記載の方法を使用して、1平方インチ当たり300セルを有するSiCフィルター基材の出口チャネルに196.6gの懸濁液4aを適用した。強制空気流を使用して発泡体コーティングを乾燥させ、500℃で焼成した。コーティングされた基材を縦方向に切断して、コーティング深さを調べ、SEMを使用してコーティングを調べた。
国際公開第2011/080525号に記載の方法を使用して、1平方インチ当たり300セルを有するSiCフィルター基材の出口チャネルに二部の懸濁液4aを適用した。第1の適用は223.3gの発泡体、第2の適用は143.0gの発泡体であった。各適用後に強制空気流を使用して発泡体コーティングを乾燥させ、500℃で焼成した。SEMを使用してコーティングを調べた。
国際公開第2011/080525号に記載の方法を使用して、1平方インチ当たり300セルを有するSiCフィルター基材の出口チャネルに三部の懸濁液4cを適用した。第1の適用は191.1gの発泡体、第2の適用は170.8gの発泡体、第3の適用は193.6gの発泡体であった。各適用後に強制空気流を使用して発泡体コーティングを乾燥させ、500℃で焼成した。SEMを使用してコーティングを調べた。
実施例5a-フィルターASCストライプ
発泡体コーティング層の適用前に、フィルターのための従来のSCRウォッシュコート層でフィルターをコーティングした。
ガンマ-アルミナ粉末(SCFa-140、Sasolより供給)を水に添加することにより懸濁液を調製し、4.5ミクロンのd50に粉砕した。Ptの可溶性塩及び0.5%のヒドロキシエチルセルロースを添加した。懸濁液を均質化するよう撹拌した。
シリカ-アルミナ粉末を水中でスラリー化し、d90<20ミクロンに粉砕する。酢酸バリウムをスラリーに加え、その後、適量の可溶性の白金とパラジウムの塩を加えた。スラリーが質量で77%のシリカ-アルミナ及び23%のゼオライトを含有するように、ベータゼオライトを加えた。スラリーを撹拌して均質化した。国際公開第99/47260号に記載のような確立されたコーティング技術を用いて、得られたウォッシュコートをフロースルーモノリスの入口チャネルに塗布した。その後、これを乾燥させ、500℃で焼成した。
1.2重量%のPdを含む比表面積(SSA)m2/gのアルファアルミナ上の予め形成されたPdを水中でスラリー化し、d90<20ミクロンに粉砕した。活性化ベーマイトスラリーを結合剤として(全固体含有量の10%として)添加し、懸濁液が25%の総固体含有量を有するまで水を加えた。0.6重量%のセルロール系増粘剤を懸濁液に添加した。続いて、水性アンモニア及び吉草酸(0.2%)を添加して、この懸濁液のpHを4.7に調整した。気体誘導羽根車を用いて15分間空気を懸濁液中に導入し、安定な泡を生成させた。
試験は、コーティングされたCu/CHAゼオライトSCR触媒のエイジングしたコアを実施例6又は7のいずれかのコアの下流の導管に配置した図9に図示する第1の合成触媒活性試験(SCAT)実験反応器で実施した。合成ガス混合物を6リットル/分の速度で導管に通した。炉を用いて、触媒出口温度900℃で2時間にわたり、定常状態の温度でDOC試料を加熱(又は「エイジング」)した。SCR触媒はDOC試料の下流に配置し、炉出口とSCR入口との間の管の長さを調節することによって、エージングプロセス中に300℃の触媒温度に保持したが、水冷式熱交換器ジャケットを必要に応じて使用することができた。温度は、適切に配置された熱電対(T1及びT2)を用いて決定した。エイジング中に使用したガス混合物は、40%の空気、50%のN2、10%のH2Oであった。
合成ガスベンチ反応器を使用して、NOx変換活性に関してSCRコアを試験した。試験は、合成気体混合物(最大利用可能NOx変換が65%であるように、O2=10%;H2O=5%;CO2=7.5%;NH3=325ppm;NO=500ppm;NO2=0ppm;N2=残り、すなわち0.65のアルファ値を使用(NH3:NOxの比))を使用して、500℃で行った。また、得られたNOx変換を図11に示す。
Claims (33)
- 発泡体で基材をコーティングする方法であって、
(a)基材の第1の端部におけるチャネルの開放端を通じて、複数のチャネルを含む基材に発泡体を導入すること、及び
(b)任意選択的に、(i)基材の第2の端部におけるチャネルの開放端に真空を、及び/又は(ii)基材の第1の端部におけるチャネルの開放端に圧力を適用すること
を含み、
発泡体が微粒子状材料を含み、且つ発泡体が安定化粒子である、方法。 - 工程(a)が、基材を実質的に垂直に保持する工程(i)、及び第1の端部におけるチャネルの開放端を通じて、基材に発泡体を押し込む又は注入する工程(ii)を含む、請求項1に記載の方法。
- 基材に発泡体を押し込む又は注入する工程(ii)が、ピストンを使用する発泡体の押し込み又は注入(ii)でありうる、請求項2に記載の方法。
- 工程(a)が、基材の第1の端部の頂部に抑制手段を配置する工程(i)、抑制手段に発泡体を投与する工程(ii)、並びに[1]基材の第2の端部におけるチャネルの開放端に真空を、及び/又は[2]基材の第1の端部のチャネルにおける開放端に圧力を適用する工程(iii)を含む、請求項1に記載の方法。
- 工程(a)が、発泡体を所定の量で導入することをさらに含む、請求項1から4のいずれか一項に記載の方法。
- 粒子状安定化発泡体を含有する基材を、基材上に配置又は担持される固体発泡体層を得るために、乾燥及び/又は焼成する工程(c)をさらに含む、請求項1から5のいずれか一項に記載の方法。
- 固体発泡体層が連続気泡構造を含む、請求項6に記載の方法。
- 固体発泡体層がセル容積を有し、セル容積の20%超が相互接続している、請求項6又は7に記載の方法。
- 発泡体が、水性媒体中で微粒子状材料の懸濁液を調製する工程(i)と;気体を懸濁液に導入することによって懸濁液を発泡させて、粒子安定化発泡体を生成する工程(ii)とを含む方法によって得られる、又は得ることができる、請求項1から8のいずれか一項に記載の方法。
- 工程(i)が、両親媒性物質を含有する水性媒体中で微粒子状材料の懸濁液を調製する工程である、請求項9に記載の方法。
- 微粒子状材料が1nmから50μmのメジアン粒子サイズを有する、請求項1から10のいずれか一項に記載の方法。
- 発泡体が1μmから1mmの直径を有する気泡を含有する、請求項1から11のいずれか一項に記載の方法。
- 内燃機関により生成される排気ガスによる汚染物質を処理又は除去するための排出制御装置であって、基材上に配置される固体発泡体層を含み、基材上に配置される固体発泡体層が、
(i)請求項6から12のいずれか一項に記載の方法から得られる、又は得ることができる;且つ/又は
(ii)連続気泡構造を有する、
排出制御装置。 - 固体発泡体層がセル容積を有し、セル容積の20%超が相互接続している、請求項13に記載の排出制御装置。
- 固体発泡体層が1~100μmのメジアン細孔直径を有する、請求項13又は14に記載の排出制御装置。
- 固体発泡体層が、5μm~500μmの範囲のサイズ分布を有する気泡様構造を含む、請求項13から15のいずれか一項に記載の排出制御装置。
- 固体発泡体層が部分的に崩壊した構造を含む、請求項13から16のいずれか一項に記載の排出制御装置。
- 固体発泡体層の厚さが500μm以下である、請求項13から17のいずれか一項に記載の排出制御装置。
- 固体発泡体層がチャネル壁上に実質的に局在している、請求項13から18のいずれか一項に記載の排出制御装置。
- 基材が多孔質モノリスである、請求項13から15のいずれか一項に記載の排出制御装置。
- 固体発泡体層が微粒子状材料を含む、請求項13から20のいずれか一項に記載の排出制御装置。
- 微粒子状材料がセラミック材料、触媒材料又は収着剤材料である、請求項21に記載の排出制御装置。
- 微粒子状材料が、担体材料上に担持される触媒活性金属を含む触媒材料である、請求項22に記載の排出制御装置。
- 触媒活性金属が、鉄、銅、ニッケル、金、白金、パラジウム、ロジウム及びルテニウムより選択される少なくとも一の遷移金属である、請求項23に記載の排出制御装置。
- 担持材料が耐火性酸化物、金属アルミネート又はゼオライトである、請求項23又は24に記載の排出制御装置。
- 担体材料が、アルミナ、シリカ、チタニア、マグネシア、ジルコニア、セリア、ランタナ及びそれら二つ以上の混合又は複合酸化物、例えばシリカ-アルミナ、チタニア-アルミナ、ジルコニア-アルミナ、セリア-アルミナ、チタニア-シリカ、ジルコニア-シリカ、ジルコニア-チタニア、セリア-ジルコニア、セリア-ジルコニア-アルミナ又はアルミナ-酸化マグネシウムからなる群より選択される耐火性酸化物である、請求項23から25のいずれか一項に記載の排出制御装置。
- 微粒子状材料が、金属酸化物系SCR触媒配合物、モレキュラーシーブ系SCR触媒配合物又はそれらの混合物である、請求項21から25のいずれか一項に記載の排出制御装置。
- 微粒子状材料がモレキュラーシーブ系SCR触媒配合物であり、好ましくはモレキュラーシーブ系SCR触媒配合物が遷移金属交換モレキュラーシーブを含む、請求項27に記載の排出制御装置。
- 遷移金属交換モレキュラーシーブの遷移金属が銅であり、モレキュラーシーブが、骨格タイプコードCHAにより表される骨格構造を有するゼオライトである、請求項28に記載の排出制御装置。
- 微粒子状材料が、耐火性酸化物の粒子及び/又はPt合金金属の粒子を含む揮発性Ptのための捕獲材料である、請求項21から25のいずれか一項に記載の排出制御装置。
- 触媒材料をさらに含む排出制御装置であって、触媒材料が白金(Pt)を含み、且つ固体発泡体層が、排気ガスが白金(Pt)を含む触媒材料と接触した後に、排気ガスと接触するよう配置されている、請求項30に記載の排出制御装置。
- 排気システム内の背圧の蓄積を回避するための、内燃機関の排気システムにおける、請求項13から31のいずれか一項に記載の排出制御装置の使用。
- 内燃機関により生成される排気ガスの処理のために排気システム中の揮発性白金(Pt)を捕獲するための、請求項30又は31に記載の固体発泡体層の使用。
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