JPWO2020067000A1 - 排ガス浄化触媒、排ガスの浄化方法、及び排ガス浄化触媒の製造方法 - Google Patents
排ガス浄化触媒、排ガスの浄化方法、及び排ガス浄化触媒の製造方法 Download PDFInfo
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- JPWO2020067000A1 JPWO2020067000A1 JP2020549206A JP2020549206A JPWO2020067000A1 JP WO2020067000 A1 JPWO2020067000 A1 JP WO2020067000A1 JP 2020549206 A JP2020549206 A JP 2020549206A JP 2020549206 A JP2020549206 A JP 2020549206A JP WO2020067000 A1 JPWO2020067000 A1 JP WO2020067000A1
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- catalyst layer
- exhaust gas
- composite oxide
- gas purification
- catalyst
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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 2
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Abstract
Description
かかる知見に鑑み、上記課題を解決するべく、本願では以下の態様を採用している。
また、上記態様に係る排ガスの浄化方法は、効率的に排ガスを浄化することができる。
また、上記態様に係る排ガス浄化触媒の製造方法は、優れた排ガス浄化性能を有する排ガス浄化触媒を提供することができる。
SR反応: CnHm+nH2O→nCO+((m/2)+n)H2
C3H6+3H2O→3CO+6H2 プロピレンの場合
WGS反応: CO+H2O→CO2+H2
H2によるNOx還元反応: H2+NOx→N2+H2O
S/W=[{(m/2)+n}×CHC×VHC]/[CCO×VCO]
式中、各パラメータは以下の通りである。
CCO:WGS反応での触媒入口におけるCOのモル濃度
VCO:WGS反応での触媒出口におけるCO浄化率
CHC:SR反応での触媒入口におけるCnHmのモル濃度
VHC:SR反応での触媒出口におけるCnHm浄化率
図1は、本実施形態に係る排ガス浄化触媒Cの断面模式図を示す。図1に示す排ガス浄化触媒Cは、ガソリンを燃料として使用する内燃機関からの排ガスを浄化するために用いられてよい。特に、本実施形態に係る排ガス浄化触媒Cは、MPI(Multi Port Injection)エンジンからの排ガスを浄化するのに適している。図1に示されるように、本実施形態に係る排ガス浄化触媒Cは、耐火性三次元構造体10と、第一触媒層20と、第二触媒層30とを備える。
耐火性三次元構造体10は、一般的な排ガス浄化触媒に使用されるものと同様のものでよい。耐火性三次元構造体10の全長は、特に制限されず、好ましくは10mm以上1000mm以下、より好ましくは15mm以上300mm以下、さらに好ましくは20mm以上150mm以下である。耐火性三次元構造体10はハニカム状の構造を有してもよい。
(第一触媒層)
第一触媒層20は、耐火性三次元構造体10の表面上に設けられている。第一触媒層20と耐火性三次元構造体10との間には、別の層を有してもよい。
第二触媒層30は、第一触媒層20の耐火性三次元構造体10とは反対側に設けられている。第一触媒層20と第二触媒層30との間には、別の層を有してもよい。
一実施形態において、排ガスの浄化方法は上記排ガス浄化触媒を用い、上記排ガス浄化触媒を排ガスに接触させるステップを有する。
以下、排ガス浄化触媒Cの製造方法を具体的に説明する。
第一スラリーは、セリウムとジルコニウムとを含む複合酸化物と、硝酸ロジウムとを含む。複合酸化物としては、第一触媒層20の複合酸化物として上述した組成のものを用いることができる。第一スラリーは、ロジウムを高分散に担持するための無機酸化物を更に含むことができる。無機酸化物は、酸化アルミニウム(アルミナ)等、第一触媒層20のロジウム担体として上述した無機酸化物を用いることができる。必要に応じて、第一スラリーは、pHを調整するための成分や界面活性剤等を含んでもよい。
第二スラリーは、セリウムとジルコニウムとを含む複合酸化物と、硝酸パラジウムとを含む。複合酸化物としては、第二触媒層30の複合酸化物として上述した組成のものを用いることができる。第二スラリーは、パラジウムを高分散に担持するための無機酸化物を更に含むことができる。無機酸化物は、酸化アルミニウム(アルミナ)等、第二触媒層30のパラジウム担体として上述した無機酸化物を用いることができる。第二スラリーは、第二族金属元素を含有する化合物を含むことが好ましい。例えば、第二スラリーが水酸化ストロンチウムを含むことが好ましい。必要に応じて、第二スラリーは、pHを調整するための成分や界面活性剤等を含んでもよい。
<排ガス浄化触媒の製造>
二酸化セリウム(CeO2)、二酸化ジルコニウム(ZrO2)、酸化ランタン(La2O3)、酸化イットリウム(Y2O3)を30:60:2:8の質量比で含む複合酸化物を用意した。当該複合酸化物のBET比表面積は、79.5m2/gであり、複合酸化物の結晶構造は、立方晶蛍石型構造であった。次に、硝酸ロジウム水溶液、酸化アルミニウム(アルミナ、Al2O3)、及び複合酸化物を、ロジウム:酸化アルミニウム:複合酸化物=0.50:75.84:20.0の質量比となるように秤量した。ここで、使用した酸化アルミニウムの平均粒径は73μmであり、そのBET比表面積は154m2/gであった。また、複合酸化物の平均粒径は11μmであった。秤量した酸化アルミニウム及び複合酸化物を水に分散させ、分散溶液に硝酸ロジウム水溶液を添加した。得られた溶液をスリーワンモーターで攪拌した後、ボールミルにて湿式粉砕することで第一スラリーを作製した。
第二スラリーに含まれる化合物の質量比を、パラジウム:酸化アルミニウム:複合酸化物:酸化ストロンチウム=5.5:52.8:41.7:8.5に変更した以外は、実施例1と同様に排ガス浄化触媒を作製した。この触媒の第一触媒層に含まれるセリウムとジルコニウムとを含む複合酸化物の質量に対する第二触媒層に含まれるセリウムとジルコニウムとを含む複合酸化物の質量の比は2.1であった。
第二スラリーに含まれる化合物の質量比を、パラジウム:酸化アルミニウム:複合酸化物:酸化ストロンチウム=5.5:52.8:33.3:8.5に変更した以外は、実施例1と同様に排ガス浄化触媒を作製した。この触媒の第一触媒層に含まれるセリウムとジルコニウムとを含む複合酸化物の質量に対する第二触媒層に含まれるセリウムとジルコニウムとを含む複合酸化物の質量の比は1.7であった。
第二スラリーに含まれる化合物の質量比を、パラジウム:酸化アルミニウム:複合酸化物:酸化ストロンチウム=5.5:52.8:20.0:8.5に変更した以外は、実施例1と同様に排ガス浄化触媒を作製した。この触媒の第一触媒層に含まれるセリウムとジルコニウムとを含む複合酸化物の量に対する第二触媒層に含まれるセリウムとジルコニウムとを含む複合酸化物の量の比は1.0であった。
第二スラリーに含まれる化合物の質量比を、パラジウム:酸化アルミニウム:複合酸化物:酸化ストロンチウム=5.5:52.8:78.6:8.5に変更した以外は、実施例1と同様に排ガス浄化触媒を作製した。この触媒の第一触媒層に含まれるセリウムとジルコニウムとを含む複合酸化物の量に対する第二触媒層に含まれるセリウムとジルコニウムとを含む複合酸化物の量の比は3.9であった。
第一スラリーに複合酸化物を加えなかったこと、及び、第二スラリーに含まれる化合物の質量比を、パラジウム:酸化アルミニウム:複合酸化物:酸化ストロンチウム=5.5:52.8:61.7:8.5に変更したこと以外は、実施例1と同様に排ガス浄化触媒を作製した。この触媒の第一触媒層には、セリウムとジルコニウムとを含む複合酸化物は含まれていない。
第一スラリーに含まれる化合物の質量比を、ロジウム:酸化アルミニウム:複合酸化物=0.50:75.84:50.0の質量比となるように変更し、第二スラリーに含まれる化合物の質量比を、パラジウム:酸化アルミニウム:複合酸化物:酸化ストロンチウム=5.5:52.8:20.0:8.5に変更した以外は、実施例1と同様に排ガス浄化触媒を作製した。この触媒の第一触媒層に含まれるセリウムとジルコニウムとを含む複合酸化物の量に対する第二触媒層に含まれるセリウムとジルコニウムとを含む複合酸化物の量の比は0.4であった。
第一スラリーに含まれる化合物の質量比を、ロジウム:酸化アルミニウム:複合酸化物=0.50:75.84:74.0の質量比となるように変更し、第二スラリーに含まれる化合物の質量比を、パラジウム:酸化アルミニウム:複合酸化物:酸化ストロンチウム=5.5:52.8:0:8.5に変更した以外は、実施例1と同様に排ガス浄化触媒を作製した。この触媒の第一触媒層に含まれるセリウムとジルコニウムとを含む複合酸化物の量に対する第二触媒層に含まれるセリウムとジルコニウムとを含む複合酸化物の量の比は0であった。
第一スラリーが、硝酸パラジウム水溶液、酸化アルミニウム、複合酸化物、及び酸化ストロンチウムを、パラジウム:酸化アルミニウム:複合酸化物:酸化ストロンチウム=5.5:52.8:20.0:8.5の質量比で含み、第二スラリーが、硝酸ロジウム水溶液、酸化アルミニウム、及び複合酸化物を、ロジウム:酸化アルミニウム:複合酸化物=0.50:75.84:41.7の質量比で含むように変更した以外は、実施例1と同様に排ガス浄化触媒を作製した。
第一スラリーが、硝酸パラジウム水溶液、酸化アルミニウム、複合酸化物、及び酸化ストロンチウムを、パラジウム:酸化アルミニウム:複合酸化物:酸化ストロンチウム=5.5:52.8:20.0:8.5の質量比で含み、第二スラリーが、硝酸ロジウム水溶液、酸化アルミニウム、及び複合酸化物を、ロジウム:酸化アルミニウム:複合酸化物=0.50:75.84:78.6の質量比で含むように変更した以外は、実施例1と同様に排ガス浄化触媒を作製した。
上記で製造した排ガス浄化触媒の耐熱処理を行った。各排ガス浄化触媒を、V型8気筒、4.6リットルエンジンの排気口から25cm下流側に設置した。当該耐熱処理は、触媒の初期劣化を想定したものである。触媒床部(触媒入口側端面から1インチの中心)の温度が1000℃となるように設定し、50時間排ガスを流し、耐熱処理を行った。
耐熱処理後の排ガス浄化触媒について、模擬ガスを用いて一酸化炭素浄化性能の評価(水性ガスシフト(WGS)反応試験)を行った。ガス条件が表2に示されている。耐熱処理を行った触媒のガス流入側端面から1cm手前の温度を500℃に保持し、表2に示したWGS1(酸素あり)の混合ガスを触媒に5分間流した。WGS1の混合ガスの温度は500℃とした。次に、表2に示したWGS2(酸素なし)の混合ガスを5分間触媒に流した。WGS2の混合ガスの温度は500℃とした。WGS2導入後5分後に、排ガス浄化触媒を通過した気体を非分散型赤外分光法で分析し、水性ガスシフト反応による一酸化炭素の浄化率を求めた。また、同時に、質量分析法により水素の生成を確認した。
耐熱処理後の排ガス浄化触媒について、模擬ガスを用いて炭化水素浄化性能の評価(水蒸気改質(SR)反応試験)を行った。ガス条件が表2に示されている。耐熱処理を行った触媒のガス流入側端面から1cm手前の温度を500℃に保持し、表2に示したSR1(酸素あり)の混合ガスを5分間触媒に流した。SR1の混合ガスの温度は500℃とした。次に、表2に示したSR2(酸素なし)の混合ガスを5分間流した。SR2の混合ガスの温度は500℃とした。SR2導入後5分後に、排ガス浄化触媒を通過した気体を水素イオン化検出器で分析し、水蒸気改質反応による炭化水素の浄化率を求めた。また、同時に、質量分析法により水素の生成を確認した。
耐熱処理後の触媒に、ガソリン車両の排ガス(特に、加速域の排ガス)を模擬した混合ガスを流通し、模擬排ガス浄化性能の評価(過渡性能評価)を行った。ガス条件を下記表3に示す。耐熱処理を行った触媒のガス流入側端面から1cm手前の温度を500℃に保持し、表3のLeanを8秒間、Richを1秒間、交互に触媒に流通させた。Lean及びRichのガス温度は、いずれも500℃とした。LeanとRichをそれぞれ10回繰り返し、1回目から10回目までの各回におけるRich時における一酸化炭素の浄化率の平均値、炭化水素の浄化率の平均値、及びNOxの浄化率の平均値をそれぞれ算出した。
表4の結果から、実施例の触媒は、S/W比が比較例の触媒よりも高かった。この結果から、実施例の触媒は比較例の触媒よりもSR反応が促進されていることが分かる。
10 耐火性三次元構造体
20 第一触媒層
30 第二触媒層
Claims (9)
- 耐火性三次元構造体と、
前記耐火性三次元構造体の表面上に設けられた第一触媒層と、
前記第一触媒層の前記耐火性三次元構造体とは反対側に設けられた第二触媒層とを備え、
前記第一触媒層は、セリウムとジルコニウムとを含む複合酸化物と、ロジウム元素とを含み、
前記第二触媒層は、セリウムとジルコニウムとを含む複合酸化物と、パラジウム元素とを含み、
前記第二触媒層に含まれるセリウムの量が、二酸化セリウム換算で、前記耐火性三次元構造体1リットル当たり10g以上25g以下である、排ガス浄化触媒。 - 前記第一触媒層の複合酸化物がイットリウムを含み、前記第一触媒層に含まれるイットリウムの量が、酸化イットリウム(Y2O3)換算で、前記耐火性三次元構造体1リットル当たり0.1g/L以上15g/L以下である、請求項1に記載の排ガス浄化触媒。
- 前記第一触媒層に含まれるセリウムとジルコニウムとを含む複合酸化物の質量に対する前記第二触媒層に含まれるセリウムとジルコニウムとを含む複合酸化物の質量の比が1.1以上3.8以下である、請求項1又は2に記載の排ガス浄化触媒。
- 前記第二触媒層が第二族金属元素を含む、請求項1から3のいずれか一項に記載の排ガス浄化触媒。
- 前記第二触媒層が酸化アルミニウムを含み、
前記第二触媒層に含まれる酸化アルミニウムの量が前記耐火性三次元構造体1リットル当たり80g以下である、請求項1から4のいずれか一項に記載の排ガス浄化触媒。 - 水蒸気改質(SR)反応によって生じる水素の量が、水性ガスシフト(WGS)反応によって生じる水素の量よりも多い、請求項1から5のいずれか一項に記載の排ガス浄化触媒。
- S/W比が1.8以上である、請求項1から6のいずれか一項に記載の排ガス浄化触媒。
- 請求項1から7のいずれか一項に記載の排ガス浄化触媒を用いる、排ガスの浄化方法。
- 請求項1から7のいずれか一項に記載の排ガス浄化触媒の製造方法であって、
耐火性三次元構造体の表面上に第一スラリーを塗布し、塗布された前記第一スラリーを乾燥及び焼成して第一触媒層を形成する第一ステップと、
前記第一触媒層の表面上に第二スラリーを塗布し、塗布された前記第二スラリーを乾燥及び焼成して第二触媒層を形成する第二ステップとを有し、
前記第一スラリーはセリウムとジルコニウムとを含む複合酸化物と、硝酸ロジウムとを含み、
前記第二スラリーはセリウムとジルコニウムとを含む複合酸化物と、硝酸パラジウムとを含み、
前記第二触媒層に含まれるセリウムが、二酸化セリウム換算で、前記耐火性三次元構造体1リットル当たり10g以上25g以下であるように前記第二ステップを行う、排ガス浄化触媒の製造方法。
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