JP5942893B2 - 排気ガス浄化用触媒の製造方法 - Google Patents
排気ガス浄化用触媒の製造方法 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims description 150
- 238000004519 manufacturing process Methods 0.000 title claims description 21
- 239000002131 composite material Substances 0.000 claims description 106
- 239000000463 material Substances 0.000 claims description 65
- 239000011230 binding agent Substances 0.000 claims description 26
- 239000000758 substrate Substances 0.000 claims description 19
- 230000001603 reducing effect Effects 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 10
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 9
- 150000002910 rare earth metals Chemical class 0.000 claims description 8
- 229910052726 zirconium Inorganic materials 0.000 claims description 8
- 229910052684 Cerium Inorganic materials 0.000 claims description 6
- 239000010948 rhodium Substances 0.000 description 104
- 239000007789 gas Substances 0.000 description 66
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 41
- 238000000746 purification Methods 0.000 description 32
- 229910052760 oxygen Inorganic materials 0.000 description 20
- 239000001301 oxygen Substances 0.000 description 19
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 17
- 229910052751 metal Inorganic materials 0.000 description 16
- 239000002184 metal Substances 0.000 description 16
- 239000002245 particle Substances 0.000 description 15
- 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
- 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
- 230000003647 oxidation Effects 0.000 description 10
- 238000007254 oxidation reaction Methods 0.000 description 10
- 229910002091 carbon monoxide Inorganic materials 0.000 description 9
- 239000006185 dispersion Substances 0.000 description 9
- 239000002002 slurry Substances 0.000 description 9
- 238000001704 evaporation Methods 0.000 description 8
- 230000008020 evaporation Effects 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- 230000003197 catalytic effect Effects 0.000 description 7
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 5
- 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
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 230000003472 neutralizing 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
- 229910052703 rhodium Inorganic materials 0.000 description 4
- 238000003860 storage Methods 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
- 229910017493 Nd 2 O 3 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
- 230000001590 oxidative effect Effects 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 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
- 238000000975 co-precipitation Methods 0.000 description 2
- 230000000694 effects Effects 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
- 238000010298 pulverizing process Methods 0.000 description 2
- 238000011946 reduction 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
- 230000032683 aging Effects 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
- 239000007788 liquid Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 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
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
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- B01J23/464—Rhodium
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Description
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系複合酸化物を調製する工程と、
前記Rh担持Zr系複合酸化物をCOを含む還元雰囲気下において、550℃以上800℃以下で熱処理する工程と、
前記Rh担持CeZr系複合酸化物と、前記RhドープCeZr系複合酸化物と、前記熱処理されたRh担持Zr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。
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が担持され且つ還元処理が施されたRh担持Zr系複合酸化物、並びにZrとCeとを含有する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系複合酸化物を調製する工程と、
上記還元処理が施された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。
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が担持され且つ還元処理が施されたRh担持Zr系複合酸化物、並びにZrとCeとを含有するCeZr系複合酸化物にRhが固溶し且つ前記還元処理が施されていないRhドープCeZr系複合酸化物からなるバインダ材を調製する工程と、
上記還元処理が施された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ドープCeZr系複合酸化物からなる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に含まれるRh担持Zr系複合酸化物は、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、サポート材である複合酸化物の表面の金属Rhの分散度と熱処理温度との関係を検討した。そのために行った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 (還元処理された)ロジウム(Rh)
6a (酸化状態の)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
Claims (5)
- 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系複合酸化物を調製する工程と、
前記Rh担持Zr系複合酸化物をCOを含む還元雰囲気下において、550℃以上800℃以下で熱処理する工程と、
前記Rh担持CeZr系複合酸化物と、前記RhドープCeZr系複合酸化物と、前記熱処理されたRh担持Zr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。 - 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、
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が担持され且つ還元処理が施されたRh担持Zr系複合酸化物、並びにZrとCeとを含有する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系複合酸化物を調製する工程と、
上記還元処理が施された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。 - 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、
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が担持され且つ還元処理が施されたRh担持Zr系複合酸化物、並びにZrとCeとを含有するCeZr系複合酸化物にRhが固溶し且つ前記還元処理が施されていないRhドープCeZr系複合酸化物からなるバインダ材を調製する工程と、
上記還元処理が施された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ドープCeZr系複合酸化物からなる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2又は3に記載の排気ガス浄化用触媒の製造方法。
- 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を備え、
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ことを特徴とする請求項2〜4のいずれか1項に記載の排気ガス浄化用触媒の製造方法。
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DE102014001859.8A DE102014001859A1 (de) | 2013-02-21 | 2014-02-11 | Abgasreinigungskatalysator und Verfahren zum Herstellen desselben |
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JP3262044B2 (ja) * | 1996-10-07 | 2002-03-04 | 株式会社豊田中央研究所 | 複合酸化物担体および複合酸化物含有触媒 |
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