JP2021104472A - 排ガス浄化用触媒 - Google Patents
排ガス浄化用触媒 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 155
- 238000000746 purification Methods 0.000 title claims abstract description 56
- 239000010419 fine particle Substances 0.000 claims abstract description 101
- 239000002245 particle Substances 0.000 claims abstract description 85
- 239000002131 composite material Substances 0.000 claims abstract description 60
- 230000005540 biological transmission Effects 0.000 claims abstract description 12
- 229910004625 Ce—Zr Inorganic materials 0.000 claims abstract 4
- 239000000463 material Substances 0.000 claims description 109
- 239000003426 co-catalyst Substances 0.000 claims description 15
- 230000000694 effects Effects 0.000 abstract description 21
- 239000000758 substrate Substances 0.000 abstract description 8
- 239000010948 rhodium Substances 0.000 description 132
- 239000010410 layer Substances 0.000 description 105
- 239000007789 gas Substances 0.000 description 65
- 239000002585 base Substances 0.000 description 29
- 229910000510 noble metal Inorganic materials 0.000 description 23
- 230000000052 comparative effect Effects 0.000 description 19
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 19
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 15
- 229910052751 metal Inorganic materials 0.000 description 14
- 239000002184 metal Substances 0.000 description 13
- 238000000034 method Methods 0.000 description 13
- 239000002243 precursor Substances 0.000 description 12
- 239000006185 dispersion Substances 0.000 description 11
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 9
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 7
- 239000003929 acidic solution Substances 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 5
- 229910052684 Cerium Inorganic materials 0.000 description 5
- 229910052693 Europium Inorganic materials 0.000 description 5
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 5
- 229910052765 Lutetium Inorganic materials 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 229910052727 yttrium Inorganic materials 0.000 description 5
- 229910052726 zirconium Inorganic materials 0.000 description 5
- 239000003637 basic solution Substances 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 4
- -1 inorganic acid salt Chemical class 0.000 description 4
- 229910052746 lanthanum Inorganic materials 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 229910044991 metal oxide Inorganic materials 0.000 description 4
- 150000004706 metal oxides Chemical class 0.000 description 4
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 description 4
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 description 4
- 238000011144 upstream manufacturing Methods 0.000 description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 3
- 229910052779 Neodymium Inorganic materials 0.000 description 3
- 229910052772 Samarium Inorganic materials 0.000 description 3
- 238000004220 aggregation Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 229910002091 carbon monoxide Inorganic materials 0.000 description 3
- 230000006866 deterioration Effects 0.000 description 3
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 239000000446 fuel Substances 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 3
- 229910052763 palladium Inorganic materials 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 239000010970 precious metal Substances 0.000 description 3
- 229910052703 rhodium Inorganic materials 0.000 description 3
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 3
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 3
- 229910052688 Gadolinium Inorganic materials 0.000 description 2
- 241000003832 Lantana Species 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 229910052777 Praseodymium Inorganic materials 0.000 description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 2
- 229910052769 Ytterbium Inorganic materials 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 2
- 239000011362 coarse particle Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000002296 dynamic light scattering Methods 0.000 description 2
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 2
- 229910052741 iridium Inorganic materials 0.000 description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 150000007530 organic bases Chemical class 0.000 description 2
- 229910052762 osmium Inorganic materials 0.000 description 2
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229910052707 ruthenium Inorganic materials 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 2
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000010757 Reduction Activity Effects 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 229910052878 cordierite Inorganic materials 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009792 diffusion process Methods 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
- 239000012153 distilled water Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- VSZWPYCFIRKVQL-UHFFFAOYSA-N selanylidenegallium;selenium Chemical compound [Se].[Se]=[Ga].[Se]=[Ga] VSZWPYCFIRKVQL-UHFFFAOYSA-N 0.000 description 1
- 238000010008 shearing Methods 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
- 241000894007 species Species 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000011206 ternary composite Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
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- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/066—Zirconium or hafnium; Oxides or hydroxides thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- B01D53/9409—Nitrogen oxides
- B01D53/9413—Processes characterised by a specific catalyst
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- 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
- B01D53/9445—Simultaneously removing carbon monoxide, hydrocarbons or nitrogen oxides making use of three-way catalysts [TWC] or four-way-catalysts [FWC]
- B01D53/945—Simultaneously removing carbon monoxide, hydrocarbons or nitrogen oxides making use of three-way catalysts [TWC] or four-way-catalysts [FWC] characterised by a specific catalyst
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- B01J21/02—Boron or aluminium; Oxides or hydroxides thereof
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- B01J23/46—Ruthenium, rhodium, osmium or iridium
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Abstract
Description
(1)基材と、該基材上に形成された触媒コート層を有する排ガス浄化用触媒であって、
前記触媒コート層が、Rh微粒子と、Ce−Zr系複合酸化物及びCe酸化物を含まないZr系複合酸化物からなる助触媒とを含み、
前記Rh微粒子が、透過型電子顕微鏡観察により測定された平均粒径が1.0nm以上2.0nm以下であり、且つ粒径の標準偏差σが0.8nm以下であり、
前記Rh微粒子が、前記Ce−Zr系複合酸化物及び前記Ce酸化物を含まないZr系複合酸化物のそれぞれに担持されている、排ガス浄化用触媒。
(1)反応場のクリアランスが所定の範囲に設定された反応器中で、Rh化合物の酸性溶液と、塩基性溶液とを反応させる方法(方法1)、及び
(2)Rh化合物の酸性溶液と、塩基性溶液とを混合して反応させた後、高速ミキサー中で撹拌処理する方法(方法2)。
使用原料
材料1:ZrO2:6重量%−La2O3、10重量%−Y2O3複合化ZrO2
材料2:ZC:21重量%−CeO2、72重量%−ZrO2、1.7重量%−La2O3、5.3重量%−Y2O3複合酸化物
材料3:硝酸Rh溶液
材料4:Rh/ZrO2:Rhが材料1に担持された材料
材料5:Rh/ZC:Rhが材料2に担持された材料
材料6:粒径制御Rh分散液
材料7:粒径制御Rh/ZrO2:材料6のRhが材料1に担持された材料
材料8:粒径制御Rh/ZC:材料6のRhが材料2に担持された材料
基材:875cc(400セル四角 壁厚4mil)のコージェライトハニカム基材
材料3と材料1とを接触させた後、焼成することにより、担持量0.2重量%のRhが材料1に担持された材料4を得た。透過型電子顕微鏡によって測定したRh微粒子の平均粒径は0.7nmであった。
材料3と材料2とを接触させた後、焼成することにより、担持量0.2重量%のRhが材料2に担持された材料5を得た。透過型電子顕微鏡によって測定したRh微粒子の平均粒径は0.7nmであった。
イオン交換水50mL中に硝酸Rh(III)0.2gを加えて溶解し、Rh化合物の酸性溶液(pH1.0)を調製した。
材料6と材料1とを接触させた後、焼成することにより、担持量0.2重量%のRhが材料1に担持された材料7を得た。透過型電子顕微鏡によって測定したRh微粒子の平均粒径は1.4nmであり、粒径の標準偏差σは0.48nmであった。
材料6と材料2とを接触させた後、焼成することにより、担持量0.2重量%のRhが材料2に担持された材料8を得た。透過型電子顕微鏡によって測定したRh微粒子の平均粒径は1.4nmであり、粒径の標準偏差σは0.48nmであった。
蒸留水に、Rh量0.45g/Lの材料6と、次に材料1を順番に攪拌しながら投入した後、10分間攪拌した。次に、材料1及びAl2O3系バインダーを投入し、約10分間攪拌した。その後、材料2を投入し、約10分間攪拌し、これらの材料が懸濁したスラリーを調製した。次に、調製したスラリーを基材へ流し込み、ブロアーで不要分を吹き払い、基材壁面に材料をコーティングした。コート量は、基材容量に対して、材料1が50g/L、材料2が30g/Lとなるようにした。最後に、120℃の乾燥機で2時間乾燥した後、電気炉で500℃にて2時間焼成し、基材上に触媒コート層を調製した。触媒コート層において、粒径制御Rhは材料1のZrO2及び材料2のZCのそれぞれに担持されていた。透過型電子顕微鏡によって測定したRh微粒子の平均粒径は1.4nmであり、粒径の標準偏差σは0.48nmであった。
材料2及び材料6を材料5に置き換えた以外は、実施例1と同様にして比較例1の触媒を調製した。
材料2及び材料6を材料8に置き換えた以外は、実施例1と同様にして比較例2の触媒を調製した。
材料1及び材料6を材料4に置き換えた以外は、実施例1と同様にして比較例3の触媒を調製した。
材料1及び材料6を材料7に置き換えた以外は、実施例1と同様にして比較例4の触媒を調製した。
材料6を材料3に置き換えた以外は、実施例1と同様にして比較例5の触媒を調製した。透過型電子顕微鏡によって測定したRh微粒子の平均粒径は0.7nmであった。
調製した実施例1及び比較例1〜5の各排ガス浄化用触媒について、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、耐久試験は、各排ガス浄化用触媒を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900℃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(3:1の比率)ずつ繰り返して流すことにより行った。
耐久試験を行った各排ガス浄化用触媒をL型4気筒エンジンの排気系にそれぞれ装着し、空燃比(A/F)=14.4の排ガスを供給し、Ga=35g/sの条件において、触媒床温200〜600℃(20℃/分)で昇温した。NOx浄化率50%の際の温度(NOx50%浄化温度)を測定し、低温活性を評価した。この値が低い程、低温活性に優れる。
20:排ガス浄化用触媒、21:基材、22:上層、23:下層、24:触媒コート層
30:排ガス浄化用触媒、31:基材、32:上層、33:下層、34:触媒コート層
40:排ガス浄化用触媒、41:基材、42:上層、43:下層、44:触媒コート層
Claims (1)
- 基材と、該基材上に形成された触媒コート層を有する排ガス浄化用触媒であって、
前記触媒コート層が、Rh微粒子と、Ce−Zr系複合酸化物及びCe酸化物を含まないZr系複合酸化物からなる助触媒とを含み、
前記Rh微粒子が、透過型電子顕微鏡観察により測定された平均粒径が1.0nm以上2.0nm以下であり、且つ粒径の標準偏差σが0.8nm以下であり、
前記Rh微粒子が、前記Ce−Zr系複合酸化物及び前記Ce酸化物を含まないZr系複合酸化物のそれぞれに担持されている、排ガス浄化用触媒。
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