JP5942894B2 - 排気ガス浄化用触媒の製造方法 - Google Patents
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- 239000003054 catalyst Substances 0.000 title claims description 129
- 238000004519 manufacturing process Methods 0.000 title claims description 15
- 239000000463 material Substances 0.000 claims description 97
- 239000002131 composite material Substances 0.000 claims description 79
- 239000011230 binding agent Substances 0.000 claims description 60
- 230000009467 reduction Effects 0.000 claims description 42
- 238000000746 purification Methods 0.000 claims description 32
- 238000010438 heat treatment Methods 0.000 claims description 17
- 230000001603 reducing effect Effects 0.000 claims description 13
- 239000000758 substrate Substances 0.000 claims description 13
- 239000002002 slurry Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 229910052726 zirconium Inorganic materials 0.000 claims description 8
- 229910052684 Cerium Inorganic materials 0.000 claims description 7
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 6
- 150000002910 rare earth metals Chemical class 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 2
- 239000010948 rhodium Substances 0.000 description 106
- 239000007789 gas Substances 0.000 description 64
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 33
- 239000002245 particle Substances 0.000 description 24
- 229910052760 oxygen Inorganic materials 0.000 description 21
- 239000001301 oxygen Substances 0.000 description 19
- 229910052751 metal Inorganic materials 0.000 description 18
- 239000002184 metal Substances 0.000 description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 17
- 239000000243 solution Substances 0.000 description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 12
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 11
- 239000000843 powder Substances 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
- 229910002091 carbon monoxide Inorganic materials 0.000 description 9
- 238000001704 evaporation Methods 0.000 description 8
- 230000008020 evaporation Effects 0.000 description 8
- 230000003197 catalytic effect Effects 0.000 description 7
- 229910052703 rhodium Inorganic materials 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 230000032683 aging Effects 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 239000000470 constituent Substances 0.000 description 5
- VXNYVYJABGOSBX-UHFFFAOYSA-N rhodium(3+);trinitrate Chemical compound [Rh+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VXNYVYJABGOSBX-UHFFFAOYSA-N 0.000 description 5
- 238000003860 storage Methods 0.000 description 5
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 4
- 229910017493 Nd 2 O 3 Inorganic materials 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 230000003472 neutralizing effect Effects 0.000 description 4
- 230000001590 oxidative effect Effects 0.000 description 4
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 description 4
- 238000011946 reduction process Methods 0.000 description 4
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 4
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 229910002651 NO3 Inorganic materials 0.000 description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- UJVRJBAUJYZFIX-UHFFFAOYSA-N nitric acid;oxozirconium Chemical compound [Zr]=O.O[N+]([O-])=O.O[N+]([O-])=O UJVRJBAUJYZFIX-UHFFFAOYSA-N 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- QQZMWMKOWKGPQY-UHFFFAOYSA-N cerium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QQZMWMKOWKGPQY-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- VQVDTKCSDUNYBO-UHFFFAOYSA-N neodymium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Nd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VQVDTKCSDUNYBO-UHFFFAOYSA-N 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- -1 oxygen ion Chemical class 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910002076 stabilized zirconia Inorganic materials 0.000 description 1
- 238000000629 steam reforming Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005406 washing Methods 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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
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- 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
- B01D53/9445—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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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/024—Multiple impregnation or coating
- B01J37/0244—Coatings comprising several layers
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Description
バインダ材となるCeZr系複合酸化物にRhが固溶し且つ還元処理してなるRhドープバインダ材、Zrと、Ce以外の希土類金属とからなるZr系複合酸化物にRhが担持され且つ前記還元処理が施されていないRh担持Zr系複合酸化物、並びにZrとCeとを含むCeZr系複合酸化物にRhが担持され且つ前記還元処理が施されていないRh担持CeZr系複合酸化物をそれぞれ調製する工程と、
前記還元処理してなるRhドープバインダ材と、前記還元処理が施されていないRh担持Zr系複合酸化物と、前記還元処理が施されていないRh担持CeZr系複合酸化物とを混合し、スラリー化してRh含有触媒材を調製する工程と、
前記Rh含有触媒材を前記基材上に設ける工程とを備えていることを特徴とする。
まず、本発明の一実施形態に係る排気ガス浄化用触媒の触媒層構成を図1を参照しながら説明する。図1は本実施形態に係る排気ガス浄化用触媒の触媒層構成を示す断面図である。
次に、上記の各触媒材の調製方法について説明する。
本実施形態において、上述の通りRh含有触媒層4のバインダ材であるRhドープバインダ材10は、予め還元処理を受けており、還元処理は、CO雰囲気下で熱処理することにより行われる。ここで、触媒効果を向上できる還元処理に最適な熱処理温度を明らかにするために、還元処理の有無によるCeZr系複合酸化物におけるRhの状態についてX線光電子分光法(XPS)を用いて検討した。その試験について以下に説明する。
2 基材(ハニカム担体)
3 Pd含有触媒層
4 Rh含有触媒層
5 Zr系複合酸化物
6 ロジウム(Rh)
7 CeZr系複合酸化物
8 ロジウム(Rh)
9 アルミナ粒子
10 Rhドープバインダ材
11 CeZr系複合酸化物
12 アルミナ粒子
13 パラジウム(Pd)
14 ジルコニアバインダ材
15 CeZr系複合酸化物粒子
16 (還元処理された)ロジウム(Rh)
16a (酸化状態の)ロジウム(Rh)
Claims (4)
- 基材上にRhを含むRh含有触媒層が設けられている排気ガス浄化用触媒の製造方法であって、
前記基材の表面上にPdを含むPd含有触媒層を設ける工程と、
Zrと、Ce以外の希土類金属とからなるZr系複合酸化物にRhが担持されたRh担持Zr系複合酸化物、ZrとCeとを含むCeZr系複合酸化物にRhが担持されたRh担持CeZr系複合酸化物、及びバインダ材となるCeZr系複合酸化物にRhを固溶してなるRhドープCeZr系複合酸化物をそれぞれ調製する工程と、
前記RhドープCeZr系複合酸化物をCOを含む還元雰囲気下において、500℃以上800℃以下で熱処理してRhドープバインダ材を調製する工程と、
前記Rh担持Zr系複合酸化物と、前記Rh担持CeZr系複合酸化物と、前記Rhドープバインダ材とを混合し、スラリー化してRh含有触媒材を調製する工程と、
前記Rh含有触媒材を前記Pd含有触媒層の表面上に設ける工程とを備えていることを特徴とする排気ガス浄化用触媒の製造方法。 - 前記Rh含有触媒材を調製する工程では、前記Rh担持Zr系複合酸化物及び前記Rh担持CeZr系複合酸化物は前記熱処理をすることなく、前記Rhドープバインダ材と混合することを特徴とする請求項1に記載の排気ガス浄化用触媒の製造方法。
- 基材上にRhを含むRh含有触媒層が設けられている排気ガス浄化用触媒の製造方法であって、
バインダ材となるCeZr系複合酸化物にRhが固溶し且つ還元処理してなるRhドープバインダ材、Zrと、Ce以外の希土類金属とからなるZr系複合酸化物にRhが担持され且つ前記還元処理が施されていないRh担持Zr系複合酸化物、並びにZrとCeとを含むCeZr系複合酸化物にRhが担持され且つ前記還元処理が施されていないRh担持CeZr系複合酸化物をそれぞれ調製する工程と、
前記還元処理してなるRhドープバインダ材と、前記還元処理が施されていないRh担持Zr系複合酸化物と、前記還元処理が施されていないRh担持CeZr系複合酸化物とを混合し、スラリー化してRh含有触媒材を調製する工程と、
前記Rh含有触媒材を前記基材上に設ける工程とを備えていることを特徴とする排気ガス浄化用触媒の製造方法。 - 前記還元処理は、COを含む還元雰囲気における550℃以上800℃以下の熱処理であることを特徴とする請求項3に記載の排気ガス浄化用触媒の製造方法。
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JP2013031868A JP5942894B2 (ja) | 2013-02-21 | 2013-02-21 | 排気ガス浄化用触媒の製造方法 |
DE102014001205.0A DE102014001205B4 (de) | 2013-02-21 | 2014-01-30 | Abgasreinigungskatalysator |
CN201410047250.0A CN104001508B (zh) | 2013-02-21 | 2014-02-11 | 尾气净化用催化剂及其制备方法 |
US14/183,352 US9144788B2 (en) | 2013-02-21 | 2014-02-18 | Exhaust gas purification catalyst and method for producing the same |
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US9144788B2 (en) | 2015-09-29 |
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DE102014001205B4 (de) | 2019-07-11 |
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DE102014001205A1 (de) | 2014-08-21 |
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