WO2010073956A1 - 触媒及び排ガス浄化方法 - Google Patents
触媒及び排ガス浄化方法 Download PDFInfo
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- WO2010073956A1 WO2010073956A1 PCT/JP2009/071019 JP2009071019W WO2010073956A1 WO 2010073956 A1 WO2010073956 A1 WO 2010073956A1 JP 2009071019 W JP2009071019 W JP 2009071019W WO 2010073956 A1 WO2010073956 A1 WO 2010073956A1
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- Prior art keywords
- catalyst
- exhaust gas
- catalyst layer
- platinum
- particle size
- Prior art date
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- 239000003054 catalyst Substances 0.000 title claims abstract description 157
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000004140 cleaning Methods 0.000 title abstract 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 128
- 239000002245 particle Substances 0.000 claims abstract description 79
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 64
- 239000007789 gas Substances 0.000 claims abstract description 53
- 238000009826 distribution Methods 0.000 claims abstract description 17
- 239000011224 oxide ceramic Substances 0.000 claims abstract description 8
- 229910052574 oxide ceramic Inorganic materials 0.000 claims abstract description 8
- 229910017464 nitrogen compound Inorganic materials 0.000 claims abstract description 3
- 150000002830 nitrogen compounds Chemical class 0.000 claims abstract description 3
- 238000000746 purification Methods 0.000 claims description 30
- 239000003638 chemical reducing agent Substances 0.000 claims description 27
- 239000000919 ceramic Substances 0.000 claims description 17
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 15
- 229910021536 Zeolite Inorganic materials 0.000 claims description 9
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 9
- 239000010457 zeolite Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 238000011068 loading method Methods 0.000 claims description 7
- 230000001186 cumulative effect Effects 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 239000004745 nonwoven fabric Substances 0.000 claims description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 7
- 239000004615 ingredient Substances 0.000 abstract 2
- 229910002089 NOx Inorganic materials 0.000 description 42
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 32
- 239000007864 aqueous solution Substances 0.000 description 22
- 239000000084 colloidal system Substances 0.000 description 19
- 230000009467 reduction Effects 0.000 description 12
- 238000006722 reduction reaction Methods 0.000 description 12
- 230000003647 oxidation Effects 0.000 description 11
- 238000007254 oxidation reaction Methods 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 238000002360 preparation method Methods 0.000 description 8
- 239000002202 Polyethylene glycol Substances 0.000 description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 7
- 239000004202 carbamide Substances 0.000 description 7
- 229910052878 cordierite Inorganic materials 0.000 description 7
- 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 7
- 239000000203 mixture Substances 0.000 description 7
- 229920001223 polyethylene glycol Polymers 0.000 description 7
- 230000001603 reducing effect Effects 0.000 description 7
- 238000001179 sorption measurement Methods 0.000 description 7
- 230000009471 action Effects 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000000354 decomposition reaction Methods 0.000 description 6
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine hydrate Chemical compound O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 6
- 229930195733 hydrocarbon Natural products 0.000 description 6
- 150000002430 hydrocarbons Chemical class 0.000 description 6
- 150000003057 platinum Chemical class 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 5
- 239000012266 salt solution Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005470 impregnation Methods 0.000 description 4
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 description 4
- 239000003223 protective agent Substances 0.000 description 4
- 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 4
- 238000003756 stirring Methods 0.000 description 4
- IXSUHTFXKKBBJP-UHFFFAOYSA-L azanide;platinum(2+);dinitrite Chemical compound [NH2-].[NH2-].[Pt+2].[O-]N=O.[O-]N=O IXSUHTFXKKBBJP-UHFFFAOYSA-L 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 3
- 229910052703 rhodium Inorganic materials 0.000 description 3
- 239000010948 rhodium Substances 0.000 description 3
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229920002873 Polyethylenimine Polymers 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010531 catalytic reduction reaction Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000000366 colloid method Methods 0.000 description 2
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 2
- 239000002283 diesel fuel Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- HLMXWUYOTWZKHB-UHFFFAOYSA-N 2-aminoethanol;platinum Chemical compound [Pt].NCCO HLMXWUYOTWZKHB-UHFFFAOYSA-N 0.000 description 1
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000010718 Oxidation Activity Effects 0.000 description 1
- 230000010757 Reduction Activity Effects 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- FOSZYDNAURUMOT-UHFFFAOYSA-J azane;platinum(4+);tetrachloride Chemical compound N.N.N.N.[Cl-].[Cl-].[Cl-].[Cl-].[Pt+4] FOSZYDNAURUMOT-UHFFFAOYSA-J 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003925 fat Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- OAKJQQAXSVQMHS-UHFFFAOYSA-N hydrazine Substances NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 1
- -1 hydrazine compound Chemical class 0.000 description 1
- 150000002429 hydrazines Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- MUMZUERVLWJKNR-UHFFFAOYSA-N oxoplatinum Chemical compound [Pt]=O MUMZUERVLWJKNR-UHFFFAOYSA-N 0.000 description 1
- SJLOMQIUPFZJAN-UHFFFAOYSA-N oxorhodium Chemical compound [Rh]=O SJLOMQIUPFZJAN-UHFFFAOYSA-N 0.000 description 1
- 229910003446 platinum oxide Inorganic materials 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229910003450 rhodium oxide Inorganic materials 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 229930195735 unsaturated hydrocarbon Natural products 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- 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
- B01D53/9404—Removing only nitrogen compounds
- B01D53/9409—Nitrogen oxides
- B01D53/9413—Processes characterised by a specific catalyst
- B01D53/9418—Processes characterised by a specific catalyst for removing nitrogen oxides by selective catalytic reduction [SCR] using a reducing agent in a lean exhaust gas
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/42—Platinum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/391—Physical properties of the active metal ingredient
- B01J35/393—Metal or metal oxide crystallite size
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/10—Noble metals or compounds thereof
- B01D2255/102—Platinum group metals
- B01D2255/1021—Platinum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/20—Metals or compounds thereof
- B01D2255/209—Other metals
- B01D2255/2092—Aluminium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/50—Zeolites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/90—Physical characteristics of catalysts
- B01D2255/902—Multilayered catalyst
- B01D2255/9022—Two layers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/90—Physical characteristics of catalysts
- B01D2255/92—Dimensions
- B01D2255/9202—Linear dimensions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/01—Engine exhaust gases
- B01D2258/012—Diesel engines and lean burn gasoline engines
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
- F01N2510/00—Surface coverings
- F01N2510/06—Surface coverings for exhaust purification, e.g. catalytic reaction
- F01N2510/068—Surface coverings for exhaust purification, e.g. catalytic reaction characterised by the distribution of the catalytic coatings
- F01N2510/0684—Surface coverings for exhaust purification, e.g. catalytic reaction characterised by the distribution of the catalytic coatings having more than one coating layer, e.g. multi-layered coatings
Definitions
- the present invention relates to a catalyst and an exhaust gas purification method, and more particularly to a catalyst for purifying nitrogen oxides (hereinafter sometimes referred to as NOx) contained in exhaust gas.
- NOx nitrogen oxides
- Exhaust gas discharged from diesel engines, gasoline engines, etc. contains nitrogen oxides as a harmful substance, which causes adverse effects on the environment. For this reason, various studies have been made on catalysts for removing nitrogen oxides in exhaust gas.
- a method of reducing nitrogen oxides by using a urea SCR (selective catalytic reduction) catalyst or an SCR catalyst using light oil (hereinafter sometimes referred to as a light oil SCR catalyst) can be mentioned.
- NO 2 contained in the exhaust gas is first oxidized to NO 2 because NO 2 is superior to NO in the reduction action by the nitrogen oxide reduction catalyst due to selective reactivity with light oil or the like as a reducing agent. Because. Therefore, prior to the catalytic reduction of nitrogen oxides by oxidizing the pre-NO to NO 2, it is possible to increase the removal rate of NOx contained in the exhaust gas.
- the conventional diesel SCR catalyst has a low NOx purification rate.
- the purification rate remains at a maximum of about 20% under conditions of 200 ° C to 250 ° C (patents) Reference 2).
- the reducing agent even if the amount of the reducing agent (light oil) is increased, the reducing agent oxidizes and burns before reducing NOx and is not used for reaction with NOx, and the NOx purification rate does not improve.
- an object of the present invention is to provide a catalyst having a higher catalytic activity and higher NOx purification performance than before, and an exhaust gas purification method using the catalyst.
- the present invention relates to a catalyst for purifying nitrogen compounds in exhaust gas, comprising a first catalyst layer and a second catalyst layer, and the first catalyst layer is provided as a catalyst component on a carrier made of an oxide ceramic.
- the average particle size is 150 to 250 nm
- the particle size D 20 of the integrated distribution 20% from the small particle size side in the particle size distribution is 100 nm or more
- the particle size D 90 of the integrated distribution 90% is 350 nm or less.
- Platinum particles are supported
- the second catalyst layer has an average particle size of 300 to 500 nm as a catalyst component on a support made of an oxide-based ceramic, and an integrated distribution from the small particle size side in the particle size distribution.
- 20% particle size D 20 is 200nm or more and the cumulative distribution 90% particle size D 90 of being supported the following platinum particles 700 nm, it relates catalysts characterized by.
- the catalyst component of the first catalyst layer preferably has an average particle size of 150 to 250 nm, D 20 is 100 nm or more, and D 90 is 350 nm or less in order to enhance the oxidation action. It is more preferable.
- the catalyst component of the second catalyst layer preferably has an average particle size of 300 to 500 nm, D 20 is 200 nm or more, and D 90 is 700 nm or less in order to enhance the reduction action. Is more preferable.
- the maximum mode diameter (peak top) from the minimum particle diameter (Dmin) to the maximum particle diameter (Dmax) is preferably 180 to 220 nm in the case of the catalyst component of the first catalyst layer, and the catalyst of the second catalyst layer In the case of the component, it is preferably 380 to 420 nm.
- the supported amount of the catalyst component in the first catalyst layer is preferably a ratio of 0.1 g / L to 5.0 g / L in terms of platinum mass relative to the support. If the supported amount is less than 0.1 g / L, NO cannot be sufficiently oxidized, and if it is more than 5.0 g / L, the NO oxidation performance is improved by only increasing the number of platinum particles that do not perform the oxidation function. Because it does not.
- the supported amount of the catalyst component in the second catalyst layer is preferably in a ratio of 0.1 g / L to 5.0 g / L in terms of platinum mass relative to the support.
- the loading amount is less than 0.1 g / L, NOx cannot be reduced sufficiently, and if it is more than 5.0 g / L, the NO reduction performance is improved simply by increasing the number of platinum particles that do not perform the reduction function. Because it does not.
- the supported amount of the catalyst component in the first catalyst layer is 0.5 g / L to 3.0 g / L, and the supported amount of the catalyst component in the second catalyst layer is 0.5 g / L to 3. The rate is 0 g / L.
- the support made of an oxide-based ceramic is one in which at least a part of a ceramic honeycomb, metal honeycomb or nonwoven fabric structure is wash-coated. Wash coating is coating of an oxide ceramic with a large surface area. By doing this, the surface area of the support can be made sufficiently large, and the exhaust gas and the catalyst component can be sufficiently brought into contact with each other. Because.
- the carrier made of the oxide ceramic of the first catalyst layer is preferably any one of alumina, zeolite, and silica
- the carrier made of the oxide ceramic of the second catalyst layer is alumina or zeolite. It is preferable that In particular, it is preferable to use zeolite for the support of the second catalyst layer, and if ZSM-5 type zeolite is used, the exhaust gas purification performance is further enhanced.
- the carrier is preferably coated at 5 g / L to 150 g / L, more preferably 20 g / L to 80 g / L, with respect to the ceramic honeycomb, metal honeycomb or non-woven fabric structure. This is because, within this range, a sufficient surface area can be ensured without excessively increasing the pressure loss of the ceramic honeycomb or metal honeycomb structure.
- the first catalyst layer and the second catalyst layer NO is oxidized to NO 2 when exhaust gas passes through the first catalyst layer, and then NO 2 is reduced to N 2 by passing through the second catalyst layer.
- Any device may be used as long as it is configured.
- the first catalyst layer and the second catalyst layer may be constituted by one support that is wash-coated, and the first catalyst layer and the second catalyst layer are respectively formed on separate supports. And may be combined.
- the adsorption method is a method in which a carrier is adsorbed onto a carrier such as a platinum salt solution containing platinum that is less than the saturated adsorption amount of the carrier until equilibrium is reached, and then dried and calcined.
- a carrier such as a platinum salt solution containing platinum that is less than the saturated adsorption amount of the carrier until equilibrium is reached.
- platinum particles suitable for NO oxidation and NO 2 reduction cannot be obtained.
- the impregnation method is a method in which the support is immersed in a platinum salt solution containing platinum equal to or greater than the saturation adsorption amount of the support, the water in the platinum salt solution is evaporated, dried and fired to be supported.
- the amount of catalyst supported can be increased as compared with the adsorption method, but it is difficult to control the particle size of the platinum particles, and the adjacent platinum particles are brought into contact with each other during production and integrated.
- the particle size distribution is in a wide range of several nm to several ⁇ m. As a result, platinum particles that do not contribute to the reaction are present, and the NOx purification performance is reduced.
- the colloid method is a method in which a platinum colloid obtained by reducing a platinum salt solution with a reducing agent is supported on a carrier, dried and fired. According to this method, it is possible to produce platinum particles having a particle diameter of several nanometers to several tens of nanometers and to control variation in the particle diameter of the platinum particles. However, it is difficult to produce platinum particles having a size suitable for the present invention by a general colloid manufacturing method.
- the catalyst according to the present invention comprising platinum particles having a predetermined average particle size with high oxidation performance or reduction performance is produced by the following steps. First, after adding a reducing agent and a protective agent to the platinum salt solution, the pH is adjusted, and further stirred with ultrasonic waves to prepare a colloidal solution. Next, the platinum colloid grown to a predetermined particle size is brought into contact with the carrier, dried and fired.
- platinum salts used for forming the platinum colloid include platinum chloride, platinum chloride, dinitroammine platinum, platinum oxide, ethanolamine platinum, acetylacetonatoplatinum, hexaammine platinum chloride, tetraammine platinum chloride, and the like. Can be used.
- a reducing agent in the step of forming a colloid in addition to sodium borohydride, ammonia, hydrazine compounds, etc., alcohol, hydrogen gas, carbon monoxide gas, saccharides, fats, ultrasonic reducing action, etc. should be used. However, it is particularly preferable to use a hydrazine compound.
- a surfactant as a protective agent.
- a surfactant polyvinyl pyrrolidone (PVP), polyacrylic acid (PAA), polyethyleneimine (PEI), polyethylene glycol (PEG) or the like having a molecular weight of 300 to 50,000 can be used.
- PVP polyvinyl pyrrolidone
- PAA polyacrylic acid
- PEI polyethyleneimine
- PEG polyethylene glycol
- polyethylene glycol having a molecular weight of 1000 to 20000 is preferred. Further, 4000 to 10,000 is more preferable.
- the PH in the colloid formation process is preferably 3.0 to 8.0. If the pH is lower than 3.0, the formation of nuclei is insufficient and a colloid cannot be generated. This is because when the pH is higher than 8.0, the colloid is precipitated and it is difficult to carry the colloid.
- the pH is preferably 3.0 to 5.0.
- the pH is 7.0 to 8. 0.0 is preferred.
- the ultrasonic wave is preferably performed at a frequency of 20 KHz to 400 KHz, more preferably a frequency of 30 KHz to 40 KHz.
- the irradiation time is preferably 1 minute to 120 minutes, more preferably 5 minutes to 40 minutes.
- the particle diameter of the platinum colloid can be adjusted to various platinum particles depending on the ratio of platinum to the reducing agent, and the mass ratio of platinum to the reducing agent is 4: 1 to 0.25: 1. Is preferred. In the present invention, it is particularly preferable that the mass ratio of platinum and reducing agent is in the range of 1: 1 to 0.5: 1. This is because when the platinum ratio is smaller than this, the platinum particle diameter is 600 nm or more, and when the platinum ratio is larger than this, the platinum particle diameter is 100 nm or less, which is not suitable for the present invention.
- the exhaust gas purification method using the catalyst and the reducing agent according to the present invention described above, wherein the exhaust gas is introduced into the first catalyst layer, and the first catalyst layer is
- the exhaust gas purification method is characterized by introducing the exhaust gas that has passed through the second catalyst layer. This is because a high NOx purification effect can be obtained by passing through the catalyst layers made of platinum particles having different average particle diameters and first oxidizing NO and then reducing NO 2 .
- the exhaust gas contains hydrocarbons composed of C 2 to C 14 unsaturated hydrocarbons in addition to NOx, and such hydrocarbons contribute to the decomposition reaction of NOx in the presence of a catalyst. It becomes.
- hydrocarbons in the exhaust gas are not sufficient. Therefore, it is necessary to add a reducing agent as a hydrocarbon source and sufficiently decompose it into NOx.
- the reducing agent to be used include gasoline, LPG, etc. in addition to light oil. Among these, it is preferable to use light oil in consideration of NOx decomposition efficiency.
- the reducing agent it is desirable to introduce the reducing agent into the first catalyst layer together with the exhaust gas. This is because NOx purification efficiency is improved if the oxidation-reduction action of NOx is performed under conditions where hydrocarbons are sufficiently present. Note that if the amount of reducing agent introduced is 0.5 to 4 (more preferably 1 to 2) by weight with respect to NOx in the exhaust gas, the NOx purification efficiency can be stabilized.
- the catalyst according to the present invention has high catalytic activity for exhaust gas purification, and particularly has high NOx decomposition performance.
- Preparation of the first catalyst layer dilute by adding 368 g of water to 36.8 g of dinitrodiammine platinum aqueous solution with a platinum content of 8.5 wt%, and add 9.2 g of polyethylene glycol having a molecular weight of 10,000 until the polyethylene glycol is sufficiently dissolved. Stirred continuously.
- a colloidal honeycomb having a diameter of 28.5 mm, a length of 25.4 mm, and a capacity of 0.156 L was supported with platinum colloid, dried at 120 ° C. overnight, and then calcined at 500 ° C. for 2 hours to obtain a catalyst.
- a catalyst having a component loading of 2 g / L in terms of platinum mass relative to the support was prepared.
- the cordierite (ceramic) honeycomb was washed with either ⁇ -alumina, zeolite, or silica, dried at 120 ° C. overnight, and then fired at 500 ° C. for 2 hours to deposit 40 g / L. A thing was used.
- the NOx oxidation catalyst thus prepared was observed with SEM photographs, and the particle size distribution on the basis of the number of particles of about 500 platinum particles was measured. As a result, the catalyst layers indicated by 200A, 200B, and 200C in Table 1 I confirmed that there was.
- Second catalyst layer 36.8 g of dinitrodiammine platinum aqueous solution having a platinum content of 8.5 wt% was diluted by adding 368 g of water, and 4.6 g of polyethylene glycol having a molecular weight of 4000 was used as the protective agent, and 98 was used as the reducing agent. A 5.5% aqueous solution of hydrazine monohydrate was added with stirring, colloids were formed under the condition of pH 7.0, and the mixture was treated with ultrasonic waves at 30 KHz for 10 minutes.
- the cordierite (ceramic) honeycomb was washed with either ⁇ -alumina, zeolite, or silica, dried at 120 ° C. overnight, and then fired at 500 ° C. for 2 hours to deposit 40 g / L. A thing was used. Other conditions were the same as those for the first catalyst, and a second catalyst having a catalyst component loading amount of 2 g / L in terms of platinum mass relative to the carrier was produced. As a result of observation with an SEM photograph, it was confirmed that the catalyst layers were 400A, 400B and 400C in Table 2.
- Preparation of catalyst layer by impregnation method A platinum solution obtained by adding 10 g of water to 2.08 g of platinum chloride aqueous solution having a platinum content of 15 wt% is absorbed by a cordierite (ceramic) honeycomb that has been coated with water at 120 ° C. overnight. After drying, it was calcined at 900 ° C. for 2 hours to prepare a catalyst layer in which the supported amount of the catalyst component was 2 g / L of platinum with respect to the support. Observation with an SEM photograph confirmed that the catalyst layers indicated by D to G in Table 3 were obtained.
- Preparation of catalyst layer by adsorption method Wash-coated cordierite (ceramic) honeycomb was immersed in a platinum solution obtained by adding 200 g of water to 3.67 g of dinitrodiamine platinum aqueous solution with a platinum content of 8.5 wt%, and stirred for 4 hours. As a result, the entire amount of platinum was adsorbed on the washcoat.
- the honeycomb taken out from the aqueous solution was dried at 120 ° C. overnight and then fired at 500 ° C. for 2 hours to prepare a catalyst layer in which the amount of the catalyst component supported was 2 g / L of platinum with respect to the carrier. Observation with an SEM photograph confirmed that the catalyst layers indicated by HK in Table 4 were obtained.
- Preparation of catalyst layer using PVP colloid Wash-coated cordierite (ceramic) honeycomb was immersed in 200 g of platinum-PVP colloid aqueous solution having an average platinum particle diameter of 2 nm and a platinum content of 0.16 wt% for 4 hours. By stirring, the entire amount of the platinum-PVP colloid was adsorbed on the washcoat. The honeycomb taken out from the aqueous solution was dried at 120 ° C. overnight and then fired at 500 ° C. for 2 hours to prepare a catalyst layer in which the amount of the catalyst component supported was 2 g / L of platinum with respect to the carrier. Observation with an SEM photograph confirmed that the catalyst layer was indicated by L in Table 5.
- comparative catalyst layer dilute by adding 184 g of water to 36.8 g of dinitrodiammine platinum aqueous solution with a platinum content of 8.5 wt%, use 4.6 g of polyethylene glycol having a molecular weight of 4000 as a protective agent, and 98% as a reducing agent. 9.0 g of hydrazine monohydrate aqueous solution was added with stirring to form a colloid under the condition of pH 8.0. The colloid is supported on a wash-coated cordierite (ceramic) honeycomb, dried at 120 ° C. overnight, then calcined at 500 ° C. for 2 hours, and a comparative catalyst having a catalyst loading of 2 g / L of platinum on the support. 5 was produced. Observation with an SEM photograph confirmed that the catalyst layer was indicated by M in Table 6.
- the honeycomb taken out from the aqueous solution was dried at 120 ° C. overnight and then reduced at 450 ° C. for 1 hour under a hydrogen stream to prepare a catalyst having a catalyst component loading of 2 g / L in terms of the copper mass relative to the support.
- the measurement result of the NOx purification rate using such a catalyst corresponds to Conventional Example 8 in Table 9.
- rhodium nitrate having a rhodium content of 8.21 wt% 0.64 g was dissolved in 100 ml of ion-exchanged water.
- 100 ml of ⁇ -alumina having an average particle diameter of 3 mm which had been dried at 120 ° C. for 24 hours in advance, was added to the above rhodium nitrate aqueous solution and stirred for 30 minutes to sufficiently impregnate the pores of alumina with the rhodium nitrate aqueous solution.
- ⁇ -alumina is separated from the aqueous rhodium nitrate solution, and after removing the excess aqueous solution adhering to the surface, it is dried at 100 ° C.
- First Embodiment The prepared catalysts are arranged in series, and a mixture obtained by adding a reducing agent to exhaust gas in advance is passed from the first catalyst layer to the second catalyst layer by a fixed bed circulation device, and the purification rate of NOx in the exhaust gas was measured.
- the results of Examples, Comparative Examples, and Conventional Examples are shown in Table 7, Table 8, and Table 9, respectively.
- the NOx purification performance was remarkably improved as compared with the comparative example and the conventional example due to the NOx oxidation effect of the first catalyst layer and the NOx reduction effect of the second catalyst layer according to the present invention.
- zeolite is used for the washcoat of the second catalyst layer, it is clear that the purification performance is higher.
- Second Embodiment Here, the influence of the reducing agent introduction sequence on the NOx purification rate was evaluated.
- the difference from the first embodiment is that the reducing agent (light oil) is not mixed with the exhaust gas in advance, but is mixed with the exhaust gas discharged through the first catalyst layer, and the mixture is introduced into the second catalyst layer (implementation).
- Example 10 The arrangement of the first catalyst layer and the second catalyst layer, and the measurement conditions such as the gas composition, the reaction temperature, and the space velocity at the time of measurement were the same as in the first embodiment.
- Table 10 shows the results of comparison of the NOx purification rate in the case of the above with the case where the mixture obtained by previously adding the reducing agent to the exhaust gas was passed from the first catalyst layer to the second catalyst layer (Example 1). Shown in
- the catalyst according to the present invention has high catalytic activity for exhaust gas purification, and particularly has high NOx decomposition performance. Therefore, if this is used, nitrogen oxides contained in the exhaust gas as harmful substances that adversely affect the environment can be effectively decomposed.
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Abstract
Description
Claims (7)
- 排ガス中の窒素化合物を浄化させるための触媒において、
第1触媒層と第2触媒層とからなり、
前記第1触媒層は、酸化物系セラミックからなる担体に、触媒成分として、平均粒径が150~250nmであり、粒子径分布における小粒径側からの積算分布20%の粒径D20が100nm以上で、且つ、積算分布90%の粒径D90が350nm以下の白金粒子が担持されており、
前記第2触媒層は、酸化物系セラミックからなる担体に、触媒成分として、平均粒径が300~500nmであり、粒子径分布における小粒径側からの積算分布20%の粒径D20が200nm以上で、且つ、積算分布90%の粒径D90が700nm以下の白金粒子が担持されていることを特徴とする排ガス浄化触媒。 - 第1触媒層の触媒成分の担持量は、担体に対する白金質量で0.1g~5.0g/Lの割合であり、
第2触媒層の触媒成分の担持量は、担体に対する白金質量で0.1g~5.0g/Lの割合である請求項1に記載の排ガス浄化触媒。 - 酸化物系セラミックからなる担体は、セラミックハニカム、メタルハニカム又は不織布の構造体の少なくとも一部にウォッシュコートされたものである請求項1又は請求項2に記載の排ガス浄化触媒。
- 第1触媒層の酸化物系セラミックからなる担体は、アルミナ、ゼオライト、シリカのいずれか1つである請求項1~請求項3のいずれかに記載の排ガス浄化触媒。
- 第2触媒層の酸化物系セラミックからなる担体は、アルミナ、又はゼオライトである請求項1~請求項4のいずれかに記載の排ガス浄化触媒。
- 請求項1~請求項5のいずれかに記載の触媒と還元剤を用いた排ガス浄化方法であって、
排ガスを第1触媒層に導入し、第1触媒層を通過した排ガスを第2触媒層に導入することを特徴とする排ガス浄化方法。 - 還元剤は、排ガスとともに第1触媒層に導入する請求項6に記載の排ガス浄化方法。
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CN104174393A (zh) * | 2014-09-05 | 2014-12-03 | 中国科学院福建物质结构研究所 | 一种用于CO气相氧化偶联生产草酸酯的Pd/ZnO高效纳米催化剂及其制备方法和应用 |
WO2020001840A1 (en) * | 2018-06-27 | 2020-01-02 | Rhodia Operations | Catalyst for base-free aerobic oxidation of glucose to glucaric acid; said process and said catalyst's preparation |
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CN105617857B (zh) * | 2016-01-06 | 2017-12-01 | 昆明理工大学 | 一种ph3选择性低温催化还原no的方法 |
CN109248681A (zh) * | 2018-09-06 | 2019-01-22 | 南京蔚岚环境技术研究院有限公司 | 一种一氧化碳氧化催化剂及其制备方法和涂覆该催化剂在载体上的方法 |
EP3912718A4 (en) * | 2019-01-15 | 2022-10-12 | Hitachi Zosen Corporation | CATALYST FOR EXHAUST GAS PURIFICATION USE, AND METHOD OF PRODUCING CATALYST FOR EXHAUST GAS PURIFICATION USE |
EP3782727A1 (de) | 2019-08-20 | 2021-02-24 | Umicore Ag & Co. Kg | Katalysator zur reduzierung von ammoniak-emissionen |
JP6921261B1 (ja) * | 2020-03-26 | 2021-08-18 | 株式会社キャタラー | 排ガス浄化触媒装置 |
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EP1020223A3 (en) * | 1999-01-12 | 2001-09-12 | Kabushiki Kaisha Toyota Chuo Kenkyusho | Porous material and production process thereof, catalyst comprising the porous material and process for purifying exhaust gas |
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JPH08229356A (ja) * | 1995-03-01 | 1996-09-10 | Toyota Motor Corp | 排ガス浄化装置 |
JPH0919626A (ja) * | 1995-07-05 | 1997-01-21 | Nippon Soken Inc | 窒素酸化物の浄化装置 |
JPH09103651A (ja) * | 1995-10-11 | 1997-04-22 | Toyota Central Res & Dev Lab Inc | 排ガス浄化装置及び排ガス浄化方法 |
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WO2020001840A1 (en) * | 2018-06-27 | 2020-01-02 | Rhodia Operations | Catalyst for base-free aerobic oxidation of glucose to glucaric acid; said process and said catalyst's preparation |
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