JP2019503842A - 窒素酸化物の選択的触媒還元のためのモノリス触媒の調製方法 - Google Patents
窒素酸化物の選択的触媒還元のためのモノリス触媒の調製方法 Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000003054 catalyst Substances 0.000 title claims abstract description 21
- 238000010531 catalytic reduction reaction Methods 0.000 title claims description 4
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 title description 19
- 239000000758 substrate Substances 0.000 claims abstract description 51
- 238000001035 drying Methods 0.000 claims abstract description 37
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000005470 impregnation Methods 0.000 claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 10
- 239000002002 slurry Substances 0.000 claims abstract description 8
- 239000011248 coating agent Substances 0.000 claims abstract description 6
- 238000000576 coating method Methods 0.000 claims abstract description 6
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000010304 firing Methods 0.000 claims abstract description 4
- 229910001935 vanadium oxide Inorganic materials 0.000 claims abstract description 4
- 230000003213 activating effect Effects 0.000 claims abstract description 3
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 12
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 claims description 12
- 229910010293 ceramic material Inorganic materials 0.000 claims description 4
- 230000005484 gravity Effects 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000001125 extrusion Methods 0.000 claims description 3
- 239000003365 glass fiber Substances 0.000 claims description 3
- 238000004804 winding Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 2
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 2
- 239000006255 coating slurry Substances 0.000 abstract 1
- 229910052720 vanadium Inorganic materials 0.000 description 11
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 11
- 239000007789 gas Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 4
- 229910052721 tungsten Inorganic materials 0.000 description 4
- 239000010937 tungsten Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910052878 cordierite Inorganic materials 0.000 description 1
- 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
- 239000000835 fiber Substances 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 150000003682 vanadium compounds Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
4NO+4NH3+O2→4N2+6H2O
NO+NO2+2NH3→2N2+3H2O
(a)複数の並行ガス流路を有するモノリス形状基材を準備するステップと、
(b)基材を、チタニアを含むウォッシュコートスラリーでコーティングするステップと、
(c)ウォッシュコートスラリーを乾燥及び焼成するステップと、
(d)乾燥及び焼成したウォッシュコートに、バナジウム酸化物の前駆体を含む水性含浸溶液を含浸させるステップと、
(e)このようにコーティングし含浸させたウォッシュコートを、5mm/分以下の乾燥速度で乾燥するステップと、
(f)コーティングし含浸させ乾燥したウォッシュコートを、焼成することによって活性化するステップと
を含む方法を提供する。
含浸させたウォッシュコートの乾燥速度は、乾燥空気の流速及び温度を制御することによって制御される;
含浸させたウォッシュコートの乾燥は、マイクロ波又は長波加熱によって実施される;
含浸させたウォッシュコートの乾燥は、ウォッシュコートした基材を重力に対して水平位置に置くことによって実施される;
含浸溶液は、タングステン酸化物前駆体化合物を更に含む;
モノリス形状基材は、互いに積層している複数の波形シートから構成される;
それぞれの波形シートには、積層される前に平面シートが備えられている;
波形形状基材は、波形シートを巻くことによって形成されている:
波形シートには、巻かれる前に平面シートが備えられている;
波形シート(複数可)は、ガラスファイバーを含む;
モノリス形状基材は、セラミック材料の押出しによって得られる;
コーティングし活性化した基材は、五酸化バナジウムを含む;
コーティングし活性化した基材は、三酸化タングステンを更に含む;
モノリスSCR触媒は、壁流フィルタの形態である;
乾燥空気の速度は0であり、乾燥は、室温で実施される。
実施例1
ハニカム構造基材を、チタニアスラリーでウォッシュコーティングして、ウォッシュコート層厚0.3〜0.5mmとした。ウォッシュコーティングした基材を乾燥し、550℃で焼成した。乾燥及び焼成した基材に、続いて、1.95wt%のメタバナジウム酸アンモニウム及び9.66wt%のメタタングステン酸アンモニウムを含有する水性含浸溶液を含浸させた。次に、含浸させた基材を、50℃及び空気流速2m/秒の温風で乾燥したところ、乾燥速度0.8〜1.2mm/分の結果となった。乾燥した後、含浸させた基材を450℃で2時間焼成した。焼成した基材の壁厚にわたるバナジウム及びタングステンの分布プロファイルを図3に示す。図3から分かるように、緩徐乾燥した基材は、ウォッシュコートの厚さにわたってタングステンの分布に濃度勾配をほぼ有さず、バナジウムの濃度勾配は、以下の比較例において調製した、急速乾燥した基材の勾配と比較して、はるかに低減されている(図2参照)。
ウォッシュコーティングし含浸させたハニカム構造基材を、実施例1の通りに調製した。含浸させた基材を、250℃及び空気流速2m/秒の温風で乾燥したところ、乾燥速度6〜8mm/分の結果となり、450℃で2時間焼成した。
実施例1及び比較例において調製されたハニカム触媒のSCR活性を、温度200〜550℃、NO/NH3モル比1.2で試験した。試験の結果を図1に示す。図1から分かるように、0.8〜1.2mm/分の速度で乾燥したハニカム触媒は、6〜8mm/分のより速い乾燥速度で乾燥した触媒と比較して、350℃を超える温度で、改善されたSCR活性を有している。
Claims (15)
- 複数のガス流路を有するモノリス選択的触媒還元用触媒を調製する方法であって、
(a)複数の並行ガス流路を有するモノリス形状の基材を準備するステップと、
(b)前記基材を、チタニアを含むウォッシュコートスラリーでコーティングするステップと、
(c)ウォッシュコーティングした基材を乾燥及び焼成するステップと、
(d)ウォッシュコーティングし乾燥及び焼成した基材に、バナジウム酸化物の前駆体を含む水性含浸溶液を含浸させるステップと、
(e)ウォッシュコーティングし含浸させた基材を、5mm/分以下の乾燥速度で乾燥するステップと、
(f)ウォッシュコーティングし含浸させ乾燥した基材を、焼成することによって活性化するステップとを含む方法。 - 前記乾燥速度が、乾燥空気流速を0〜3m/秒に制御すること及び乾燥空気温度を70℃未満に制御することによって制御される、請求項1に記載の方法。
- 前記ウォッシュコーティングし含浸させた基材の乾燥が、マイクロ波又は長波加熱によって実施される、請求項1に記載の方法。
- 前記ウォッシュコーティングし含浸させた基材の乾燥が、前記基材を重力に対して水平位置に置くことによって実施される、請求項1から3のいずれか一項に記載の方法。
- 前記水性含浸溶液が、タングステン酸化物の前駆体化合物を更に含む、請求項1から4のいずれか一項に記載の方法。
- 前記モノリス形状の基材が、互いに積層している複数の波形シートから構成される、請求項1から5のいずれか一項に記載の方法。
- 前記複数の波形シートの各々には、積層される前に平面シートが備えられる、請求項6に記載の方法。
- 波形形状の基材が、単一の波形シートを巻くことによって形成されている、請求項1から5のいずれか一項に記載の方法。
- 前記単一の波形シートには、巻かれる前に平面シートが備えられる、請求項8に記載の方法。
- 前記波形シートがガラスファイバーを含む、請求項6から9のいずれか一項に記載の方法。
- 前記モノリス形状の基材が、セラミック材料の押出しによって得られる、請求項1から5のいずれか一項に記載の方法。
- ステップ(f)で活性化した基材が、五酸化バナジウムを含む、請求項1から11のいずれか一項に記載の方法。
- 前記活性化した基材が、三酸化タングステンを更に含む、請求項12に記載の方法。
- 前記モノリス選択的触媒還元用触媒が壁流フィルタの形態である、請求項1から13のいずれか一項に記載の方法。
- 乾燥空気流速が0m/秒であり、乾燥が室温で実施される、請求項2から14のいずれか一項に記載の方法。
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