JP2018176109A - 排ガス浄化用触媒 - Google Patents
排ガス浄化用触媒 Download PDFInfo
- Publication number
- JP2018176109A JP2018176109A JP2017082716A JP2017082716A JP2018176109A JP 2018176109 A JP2018176109 A JP 2018176109A JP 2017082716 A JP2017082716 A JP 2017082716A JP 2017082716 A JP2017082716 A JP 2017082716A JP 2018176109 A JP2018176109 A JP 2018176109A
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- Prior art keywords
- layer
- upper layer
- catalyst
- substrate
- exhaust gas
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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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- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
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- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
[1]基材と、該基材の表面に形成された触媒コート層とを備える排ガス浄化用触媒であって、
触媒コート層が、基材表面に近い方を下層とし相対的に遠い方を上層とする上下層を含み、
触媒コート層の上層が、Rh及びPdと担体とを含有し、
触媒コート層の下層が、Pd及びPtから選択される少なくとも1種の貴金属と担体とを含有し、
上層に含有されるPdの65質量%以上が、基材表面に相対的に遠い上層の表面から上層の厚さ50%までの層に存在し、
上層において、Rhに対するPdの質量比(Pd/Rh)が0.5以上7.0以下である、上記排ガス浄化用触媒。
[2]上層に含有されるPdの85質量%以上が、基材表面に相対的に遠い上層の表面から上層の厚さ50%までの層に存在する、[1]に記載の排ガス浄化用触媒。
本明細書では、適宜図面を参照して本発明の特徴を説明する。図面では、明確化のために各部の寸法及び形状を誇張しており、実際の寸法及び形状を正確に描写してはいない。それ故、本発明の技術的範囲は、これら図面に表された各部の寸法及び形状に限定されるものではない。
[I−1.原料]
(1)担体として使用した原料は以下の通りである:
材料1(Al2O3)
La2O3複合化Al2O3を使用した。La2O3:1wt%〜10wt%。
材料2(ACZ)
Al2O3−CeO2−ZrO2複合酸化物を使用した。CeO2:15〜30wt%。Nd2O3、La2O3、Y2O3が微量添加され、高耐熱化が施されたもの。
材料3(CZ)
CeO2−ZrO2の複合酸化物を使用した。OSC特性の観点からPr2O3が1〜10wt%添加されたもの。
(2)基材として使用した原料は以下の通りである:
875cc(600セル六角、壁厚2mil(ミリインチ)のコージェライトハニカム基材を使用した。
<比較例1>
下層:Pd(0.23)+ACZ(45)+Al2O3(40)+硫酸Ba(5)+CZ(10)
上層:Rh(0.11)+ACZ(100)+Al2O3(30)
硝酸Pd、ACZ(材料2)、Al2O3(材料1)、硫酸Ba、材料3、Al2O3系バインダーを投入し懸濁した[スラリー1]を調製した。
さらに、調製した[スラリー1]を基材へ流し込み、ブロアーで不要分を吹き払うことで、基材壁面にコーティングした。その際にコーティング材料は、基材容量に対して、Pdが0.23g/L、ACZ(材料2)が45g/L、Al2O3(材料1)が40g/L、硫酸Baが5g/L、CZ(材料3)が10g/Lであった。最後に、120℃に保たれた乾燥機で2時間水分を飛ばした後、電気炉で500℃2時間の焼成を加えて下層を形成した。
硝酸Rh、ACZ(材料2)、Al2O3(材料1)、Al2O3系バインダーを投入し懸濁した[スラリー2]を調製した。
調製した[スラリー2]を、下層を形成した基材へ流し込み、ブロアーで不要分を吹き払うことで、上層コーティングした。その際にコーティング材料は、基材容量に対して、Rhが0.11g/L、ACZ(材料2)が100g/L、Al2O3(材料1)が30g/Lであった。最後に、120℃に保たれた乾燥機で2時間水分を飛ばした後、電気炉で500℃2時間の焼成を加えて触媒を得た。
下層:Pd(0.23)+ACZ(45)+Al2O3(40)+硫酸Ba(5)+CZ(10)
上層:Rh(0.11)+ACZ(100)+Pd(0.7)+Al2O3(30)
比較例1の[スラリー2]調製工程の代わりに、Pdを含む[スラリー3]の調製工程を行った以外は、比較例1と同様にして触媒を得た。
[スラリー3]は、硝酸Pd、ACZ(材料2)、硝酸Rh、Al2O3(材料1)、Al2O3系バインダーを投入し懸濁して調製した。
調製した[スラリー3]を、下層を形成した基材へ流し込み、ブロアーで不要分を吹き払うことで、上層コーティングした。その際にコーティング材料は、基材容量に対して、Rhが0.11g/L、Pdが0.7g/L、ACZ(材料2)が100g/L、Al2O3(材料1)が30g/Lであった。最後に、120℃に保たれた乾燥機で2時間水分を飛ばした後、電気炉で500℃2時間の焼成を加えて触媒を得た。
その際、上層のPdは表面層(基材表面に相対的に遠い上層の表面から上層の厚さ50%までの層)に50%存在している。
下層:Pd(0.23)+ACZ(45)+Al2O3(40)+硫酸Ba(5)+CZ(10)
上層:Rh(0.11)+ACZ(100)+Al2O3(30)+Pd(1.2)
比較例1の上層コーティングの後Pdを担持した以外は、比較例1と同様にして触媒を得た。
比較例1において乾燥・焼成した上層コーティングにPd溶液を吸水させ、ブロアーで不要分を吹き払うことで、Pdを1.2g/L担持した。その上で120℃に保たれた乾燥機で2時間水分を飛ばした後、電気炉で500℃2時間の焼成を加えて触媒を得た。結果としてRhとPdが含まれる上層を調製した。その際、Pd溶液のpHを1以上かつ2以下とすることにより、表面層に約90%のPdが存在するように条件を調整した。
下層:Pd(0.23)+ACZ(45)+Al2O3(40)+硫酸Ba(5)+CZ(10)
上層:Rh(0.11)+ACZ(100)+Pd(0.055)+Al2O3(30)
上層コーティングの際のコーティング材料が、基材容量に対して、Rhが0.11g/L、Pdが0.055g/L、ACZ(材料2)が100g/L、Al2O3(材料1)が30g/Lであった以外は、比較例2と同様にして触媒を得た。
その際、上層のPdは表面層(基材表面に相対的に遠い上層の表面から上層の厚さ50%までの層)に50%存在している。
下層:Pd(0.23)+ACZ(45)+Al2O3(40)+硫酸Ba(5)+CZ(10)
上層:Rh(0.11)+ACZ(100)+Pd(0.20)+Al2O3(30)
上層コーティングの際のコーティング材料が、基材容量に対して、Rhが0.11g/L、Pdが0.20g/L、ACZ(材料2)が100g/L、Al2O3(材料1)が30g/Lであった以外は、比較例2と同様にして触媒を得た。
その際、上層のPdは表面層(基材表面に相対的に遠い上層の表面から上層の厚さ50%までの層)に50%存在している。
下層:Pd(0.23)+ACZ(45)+Al2O3(40)+硫酸Ba(5)+CZ(10)
上層:Rh(0.11)+ACZ(100)+Al2O3(30)+Pd(0.7)
比較例1の上層コーティングの後Pdを担持した以外は、比較例1と同様にして触媒を得た。
比較例1において乾燥・焼成した上層コーティングにPd溶液を吸水させ、ブロアーで不要分を吹き払うことで、Pdを0.7g/L担持した。その上で120℃に保たれた乾燥機で2時間水分を飛ばした後、電気炉で500℃2時間の焼成を加えて触媒を得た。結果として、RhとPdが含まれる上層を調製した。その際、Pd溶液のpHを1以下とすることにより、表面層に約65%のPdが存在するように条件を調整した。
下層:Pd(0.23)+ACZ(45)+Al2O3(40)+硫酸Ba(5)+CZ(10)
上層:Rh(0.11)+ACZ(100)+Al2O3(30)+Pd(0.7)
比較例1の上層コーティングの後Pdを担持した以外は、比較例1と同様にして触媒を得た。
比較例1において乾燥・焼成した上層コーティングにPd溶液を吸水させ、ブロアーで不要分を吹き払うことで、Pdを0.7g/L担持した。その上で120℃に保たれた乾燥機で2時間水分を飛ばした後、電気炉で500℃2時間の焼成を加えて触媒を得た。結果として、RhとPdが含まれる上層を調製した。その際、Pd溶液のpHを1以上かつ2以下とすることにより、表面層に約90%のPdが存在するように条件を調整した。
下層:Pd(0.23)+ACZ(45)+Al2O3(40)+硫酸Ba(5)+CZ(10)
上層:Rh(0.11)+ACZ(100)+Al2O3(30)+Pd(0.33)
比較例1の上層コーティングの後Pdを担持した以外は、比較例1と同様にして触媒を得た。
比較例1において乾燥・焼成した上層コーティングにPd溶液を吸水させ、ブロアーで不要分を吹き払うことで、Pdを0.33g/L担持した。その上で120℃に保たれた乾燥機で2時間水分を飛ばした後、電気炉で500℃2時間の焼成を加えて触媒を得た。結果としてRhとPdが含まれる上層を調製した。その際、Pd溶液のpHを1以上かつ2以下とすることにより、表面層に約90%のPdが存在するように条件を調整した。
下層:Pd(0.23)+ACZ(45)+Al2O3(40)+硫酸Ba(5)+CZ(10)
上層:Rh(0.11)+ACZ(100)+Al2O3(30)+Pd(0.055)
比較例1の上層コーティングの後Pdを担持した以外は、比較例1と同様にして触媒を得た。
比較例1において乾燥・焼成した上層コーティングにPd溶液を吸水させ、ブロアーで不要分を吹き払うことで、Pdを0.055g/L担持した。その上で120℃に保たれた乾燥機で2時間水分を飛ばした後、電気炉で500℃2時間の焼成を加えて触媒を得た。結果としてRhとPdが含まれる上層を調製した。その際、Pd溶液のpHを1以上かつ2以下とすることにより、表面層に約90%のPdが存在するように条件を調整した。
下層:Pd(0.23)+ACZ(45)+Al2O3(40)+硫酸Ba(5)+CZ(10)
上層:Rh(0.11)+ACZ(100)+Al2O3(30)+Pd(0.20)
比較例1の上層コーティングの後Pdを担持した以外は、比較例1と同様にして触媒を得た。
比較例1において乾燥・焼成した上層コーティングにPd溶液を吸水させ、ブロアーで不要分を吹き払うことで、Pdを0.20g/L担持した。その上で120℃に保たれた乾燥機で2時間水分を飛ばした後、電気炉で500℃2時間の焼成を加えて触媒を得た。結果としてRhとPdが含まれる上層を調製した。その際、Pd溶液のpHを1以上かつ2以下とすることにより、表面層に約90%のPdが存在するように条件を調整した。
[II−1.物性評価]
物性評価は、各触媒(耐久試験後)を所定のサイズに切り出し、樹脂埋め後、研磨、Au蒸着し、FE−EPMA(JXA−8530F JEOL製)を用いて行った。
具体的には、表面層に存在するPd量の割合は、FE−EPMAで触媒コート層を観察し、触媒コート層断面の厚さ方向に対してPdのライン分析を行い、上層にあるPd量と、表面から厚さ50%までの範囲にあるPd元素を積算することにより得た上層の上半分にあるPd量とから算出した。
上層におけるRhに対するPdの質量比(Pd/Rh)は、上層コーティング層に吸水させたPd量と上層コーティング層に担持したRhの比率により算出した。
各触媒について、実際のエンジンを用いて耐久試験を実施した。具体的には、各触媒をV型8気筒エンジンの排気系にそれぞれ装着し、触媒床温1000℃で50時間にわたり、ストイキ及びリーンの各雰囲気の排ガスを一定時間ずつ繰り返して流すことにより行った。
各触媒の活性を、L4エンジンを用いて評価した。
T50評価:空燃比(A/F)14.4(リッチ)の排ガスを供給し、高Ga条件(Ga=35g/s)での昇温特性(〜500℃)を評価した(SV=110000hr−1)。入りガス温度が500℃となった際の浄化率により触媒活性を評価した。
上記[II−1.物性評価]及び[II−3.性能評価]により得られた各触媒の評価結果を表1に示す。
11・・基材
12・・触媒コート層
13・・下層
14・・上層
15・・基材表面に相対的に遠い上層の表面から上層の厚さ50%までの層(表面層)
16・・基材表面に相対的に近い上層の表面から上層の厚さ50%までの層
Claims (2)
- 基材と、該基材の表面に形成された触媒コート層とを備える排ガス浄化用触媒であって、
触媒コート層が、基材表面に近い方を下層とし相対的に遠い方を上層とする上下層を含み、
触媒コート層の上層が、Rh及びPdと担体とを含有し、
触媒コート層の下層が、Pd及びPtから選択される少なくとも1種の貴金属と担体とを含有し、
上層に含有されるPdの65質量%以上が、基材表面に相対的に遠い上層の表面から上層の厚さ50%までの層に存在し、
上層において、Rhに対するPdの質量比(Pd/Rh)が0.5以上7.0以下である、上記排ガス浄化用触媒。 - 上層に含有されるPdの85質量%以上が、基材表面に相対的に遠い上層の表面から上層の厚さ50%までの層に存在する、請求項1に記載の排ガス浄化用触媒。
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US10413885B2 (en) | 2017-10-06 | 2019-09-17 | Toyota Jidosha Kabushiki Kaisha | Exhaust gas purification catalyst |
JP2020182915A (ja) * | 2019-05-09 | 2020-11-12 | トヨタ自動車株式会社 | 排ガス浄化用触媒 |
EP3885030A1 (en) | 2020-03-25 | 2021-09-29 | Toyota Jidosha Kabushiki Kaisha | Exhaust gas purification catalyst |
JP6997838B1 (ja) | 2020-08-07 | 2022-01-18 | 株式会社キャタラー | 排ガス浄化用触媒 |
US11400436B2 (en) | 2019-12-26 | 2022-08-02 | Toyota Jidosha Kabushiki Kaisha | Exhaust gas purification catalyst |
US11577226B2 (en) | 2019-12-26 | 2023-02-14 | Toyota Jidosha Kabushiki Kaisha | Exhaust gas purification catalyst |
US11719144B2 (en) | 2019-12-26 | 2023-08-08 | Toyota Jidosha Kabushiki Kaisha | Exhaust gas purification catalyst |
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KR102211944B1 (ko) * | 2019-04-04 | 2021-02-03 | 희성촉매 주식회사 | 귀금속 박층을 최상층으로 포함하는 다층구조의 배기가스 정화용 촉매 및 이의 제조방법 |
JP7372052B2 (ja) * | 2019-05-15 | 2023-10-31 | 株式会社キャタラー | 排ガス浄化触媒装置 |
EP3889404A1 (en) * | 2020-03-30 | 2021-10-06 | Johnson Matthey Public Limited Company | Multi-region twc catalysts for gasoline engine exhaust gas treatments with improved h2s attenuation |
JP2022050754A (ja) * | 2020-09-18 | 2022-03-31 | 株式会社キャタラー | 排ガス浄化用触媒 |
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US10307736B2 (en) | 2019-06-04 |
DE102018108460A1 (de) | 2018-10-25 |
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