JP5618543B2 - 排ガス中の窒素酸化物の選択的接触還元法 - Google Patents
排ガス中の窒素酸化物の選択的接触還元法 Download PDFInfo
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- B01D53/34—Chemical or biological purification of waste gases
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- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
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- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- 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
- F01N3/18—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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2251/106—Peroxides
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- B01D2251/206—Ammonium compounds
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- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/10—Noble metals or compounds thereof
- B01D2255/102—Platinum group metals
- B01D2255/1023—Palladium
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
- B01D53/9459—Removing one or more of nitrogen oxides, carbon monoxide, or hydrocarbons by multiple successive catalytic functions; systems with more than one different function, e.g. zone coated catalysts
- B01D53/9477—Removing one or more of nitrogen oxides, carbon monoxide, or hydrocarbons by multiple successive catalytic functions; systems with more than one different function, e.g. zone coated catalysts with catalysts positioned on separate bricks, e.g. exhaust systems
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- F01N2240/00—Combination or association of two or more different exhaust treating devices, or of at least one such device with an auxiliary device, not covered by indexing codes F01N2230/00 or F01N2250/00, one of the devices being
- F01N2240/25—Combination or association of two or more different exhaust treating devices, or of at least one such device with an auxiliary device, not covered by indexing codes F01N2230/00 or F01N2250/00, one of the devices being an ammonia generator
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Description
従来技術によれば、アンモニア(NH3)は還元剤として乗り物の酸素含有排ガス中の窒素酸化物の選択的接触還元の際に用いられ、該還元剤は、特殊なSCR触媒の上流で、またはマフラーに組み込まれる並行して流通可能なSCR触媒モジュールのクラスターの上流で、燃焼システムおよび内燃機関の排ガスライン、殊に自動車の内燃機関の排ガスラインに導入され、かつSCR触媒中で、排ガス中に含有される窒素酸化物の還元をもたらす。SCRは、酸素の存在下での窒素酸化物(NOx)の選択的接触還元を意味する。
(H2N2)CO→HNCO+NH3 [1]
に従って、主としてイソシアン酸(HNCO)とアンモニア(NH3)とに分解する。
HNCO+H2O→NH2+CO2 [2]
に従って、アンモニア(NH3)と二酸化炭素(CO2)とに加水分解する。
R=H、NH2、C1〜C12−アルキル、
=アセテート、カーボネート、シアネート、ホルメート、ヒドロキシド、メトキシドおよびオキサレートを意味する]
の化合物である。
R=H、NH2、C1〜C12−アルキル、
=アセテート、カーボネート、シアネート、ホルメート、ヒドロキシド、メトキシドおよびオキサレートを意味する]
の化合物が有効であることが実証された。
図1に描写されたものに相応する自己圧力式のアンモニア発生装置中でのアンモニア前駆体物質としての40質量%のギ酸グアニジニウム水溶液(GF)(Fp.<−20℃)の使用
乗用車エンジン1が200Nm3/hの排ガス流を生み出し、該排ガス流を、中間管2を介して白金酸化触媒3およびパティキュレートフィルター4を通して排ガス中間管6の中に導く。FTIRガス分析装置5を用いて測定した中間管6の中の排ガス組成は:窒素酸化物、NO 150ppm;二酸化窒素、NO2 150ppm;二酸化炭素、CO2 7%;水蒸気 8%、一酸化炭素、CO 10ppmである。
GF溶液8の計量供給は、FTIRガス分析装置17を用いて270ppmのアンモニア濃度を測定することができるように、圧力調整ポンプ9を用いて制御する。この際、同時にGF溶液8のホルメート部分の分解によってCO濃度90から100ppmへの上昇が生じる。GF溶液8の蒸発および分解によるCO2含有量および水蒸気含有量の上昇は期待通り僅かであり、かつ殆ど測定可能ではない。GFの接触加水分解は完全なものである。それというのも、ガス分析装置17を用いてイソシアン酸、HNCOは検出することができず、尿素およびその分解生成物の付着物を確認することができなかったからである。
実施例1と同じように作業するが、しかしながら二酸化チタン触媒14の代わりに、酸化パラジウム−二酸化チタン−触媒を使用し、その際、該二酸化チタンは、Pd(NO3)2水溶液を用いて、乾燥およびか焼後に(500℃で5時間)、PdO 1質量%(=約0.9質量%のPd)を含有し、かつ一酸化炭素の部分酸化をもたらす触媒が生じるように含浸した。FTIRガス分析装置17では、CO濃度の上昇を測定することはできなかった。
実施例1と同じように作業するが、しかしながら40質量%のギ酸グアニジニウム溶液の代わりに、15質量%のジ−グアニジニウムカーボネート溶液を使用する。反応器11を同様に250℃で加熱し、触媒13および14は実施例1のものと同一である。
実施例1と同じように作業するが、しかしながら触媒13および14はAl2O3から成り、かつ反応器11は350℃の温度で作動させる。
Claims (17)
- 排ガス中でのアンモニアを用いた窒素酸化物の選択的接触還元法において、
以下の一般式(I)
Rは、H、NH2、またはC1〜C12−アルキルを意味し、かつ、
は、アセテート、カーボネート、シアネート、ホルメート、ヒドロキシド、メトキシドまたはオキサレートを意味する]で示され、かつ、80〜850g/kgのアンモニア生成能を有する化合物の溶液を、触媒活性でありかつ酸化活性ではないコーティングの存在下で接触分解し、ここで、該コーティングが、二酸化チタン、酸化アルミニウム、二酸化ケイ素およびその混合物の群から選択された酸化物から構成されているか、または/かつ、該コーティングが、完全にまたは部分的に金属交換されている水熱安定性のゼオライトから構成されており、かつ、
得られるアンモニア含有ガスを排ガスにSCR触媒の上流で供給する
ことを特徴とする方法。 - 2つ以上の異なる前記式(I)の化合物からの混合物を使用することを特徴とする、請求項1または2記載の方法。
- 請求項1で定義される前記式(I)の化合物が、250〜600g/kgのアンモニア生成能を有することを特徴とする、請求項1から3までのいずれか1項記載の方法。
- 前記式(I)の化合物と尿素の溶液においては、前記式(I)の化合物の含有率が5〜60質量%であり、かつ、尿素の含有率が5〜35質量%であることを特徴とする、請求項2記載の方法。
- 前記式(I)の化合物とアンモニアもしくは前記式(II)の化合物の溶液においては、前記式(I)の化合物の含有率が5〜60質量%であり、かつ、アンモニアもしくは前記式(II)の化合物の含有率が5〜40質量%であることを特徴とする、請求項2記載の方法。
- 前記式(I)の化合物ならびに場合によりさらに別の成分を、水および/またはC1〜C4−アルコールから成る溶剤中で使用することを特徴とする、請求項1から6までのいずれか1項記載の方法。
- 前記の水性および/またはアルコール性の溶液においては、請求項1で定義される前記一般式(I)の化合物の含有率が5〜85質量%または30〜80質量%であることを特徴とする、請求項7記載の方法。
- 前記式(I)の化合物の溶液または前記式(I)の化合物の混合物の溶液であって、場合によりさらに尿素が水中に混じった溶液が、溶液1リットル当たりアンモニア0.2〜0.5kgのアンモニア生成能または0.25kg〜0.35kg/lのアンモニア生成能を有することを特徴とする、請求項1から8までのいずれか1項記載の方法。
- 前記式(I)の化合物ならびに場合によりさらに別の成分を、排ガス内部での排ガスのメインフロー、パーシャルフローもしくはバイパスフローにおいてか、または排ガス外部で自己圧力式のかつ外部加熱される装置において接触分解によってアンモニアに変換することを特徴とする、請求項1から9までのいずれか1項記載の方法。
- アンモニア、二酸化炭素および場合により一酸化炭素への前記式(I)の化合物ならびに場合によりさらに別の成分の接触分解のために、酸化活性ではないコーティングを有する触媒以外にさらに酸化活性コーティングを有する触媒をも使用することを特徴とする、請求項1から10までのいずれか1項記載の方法。
- 金および/またはパラジウムにより含浸されている、二酸化チタン、酸化アルミニウムならびに二酸化ケイ素の群から選択された酸化物、水熱安定性の金属ゼオライトおよびその混合物からの酸化活性コーティングを有する触媒を使用することを特徴とする、請求項11記載の方法。
- 活性成分としてのパラジウムおよび/または金から成る酸化活性コーティングであって貴金属含有率が0.001〜2質量%の酸化活性コーティングを有する触媒を使用することを特徴とする、請求項11記載の方法。
- 2つの部分から成る触媒を使用し、その際、第一の部分は酸化活性ではないコーティングを含有し、かつ第二の部分は酸化活性コーティングを含有することを特徴とする、請求項1から13までのいずれか1項記載の方法。
- 前記触媒の5〜90体積%が酸化活性ではないコーティングから成り、かつ10〜95体積%が酸化活性コーティングから成ることを特徴とする、請求項14記載の方法。
- 接触分解を2つの連続して配置された触媒の存在下で実施し、その際、第一の触媒は酸化活性ではないコーティングから成り、かつ第二の触媒は酸化活性コーティングから成ることを特徴とする、請求項1から15までのいずれか1項記載の方法。
- 前記式(I)の化合物の溶液の接触分解を150〜350℃で実施することを特徴とする、請求項1から16までのいずれか1項記載の方法。
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PCT/EP2007/011285 WO2008077588A1 (de) | 2006-12-23 | 2007-12-20 | Verfahren zur selektiven katalytischen reduktion von stikoxiden in abgasen von fahrzeugen |
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JP2009541892A Expired - Fee Related JP5618542B2 (ja) | 2006-12-23 | 2007-12-20 | 排ガス中の窒素酸化物の選択的接触還元のためのアンモニア前駆物質としてのギ酸グアニジニウム含有水溶液の使用 |
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US (2) | US8652426B2 (ja) |
EP (2) | EP2111287B1 (ja) |
JP (2) | JP5618543B2 (ja) |
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