JP6204751B2 - ハニカム触媒及び排ガス浄化装置 - Google Patents
ハニカム触媒及び排ガス浄化装置 Download PDFInfo
- Publication number
- JP6204751B2 JP6204751B2 JP2013175928A JP2013175928A JP6204751B2 JP 6204751 B2 JP6204751 B2 JP 6204751B2 JP 2013175928 A JP2013175928 A JP 2013175928A JP 2013175928 A JP2013175928 A JP 2013175928A JP 6204751 B2 JP6204751 B2 JP 6204751B2
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- Prior art keywords
- honeycomb
- zeolite
- honeycomb unit
- honeycomb catalyst
- inorganic particles
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000003054 catalyst Substances 0.000 title claims description 82
- 238000000746 purification Methods 0.000 title claims description 58
- 239000011148 porous material Substances 0.000 claims description 93
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 72
- 229910021536 Zeolite Inorganic materials 0.000 claims description 66
- 239000010457 zeolite Substances 0.000 claims description 66
- 239000002245 particle Substances 0.000 claims description 61
- 239000010954 inorganic particle Substances 0.000 claims description 53
- 238000005192 partition Methods 0.000 claims description 42
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 36
- 239000011230 binding agent Substances 0.000 claims description 32
- 239000000126 substance Substances 0.000 claims description 30
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 26
- 239000012784 inorganic fiber Substances 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 16
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 11
- 229910001431 copper ion Inorganic materials 0.000 claims description 11
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 10
- 229910000323 aluminium silicate Inorganic materials 0.000 claims description 6
- 229910002089 NOx Inorganic materials 0.000 description 48
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 38
- 239000007789 gas Substances 0.000 description 37
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 23
- 229910021529 ammonia Inorganic materials 0.000 description 19
- 239000010410 layer Substances 0.000 description 18
- 230000002093 peripheral effect Effects 0.000 description 18
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- 238000007254 oxidation reaction Methods 0.000 description 9
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- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 6
- 229910052753 mercury Inorganic materials 0.000 description 6
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 6
- 238000006073 displacement reaction Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 4
- 229910001593 boehmite Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000470 constituent Substances 0.000 description 4
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 4
- 229910000174 eucryptite Inorganic materials 0.000 description 4
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 4
- 229920000609 methyl cellulose Polymers 0.000 description 4
- 239000001923 methylcellulose Substances 0.000 description 4
- 235000010981 methylcellulose Nutrition 0.000 description 4
- 229910052863 mullite Inorganic materials 0.000 description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 4
- 229910010271 silicon carbide Inorganic materials 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000004793 Polystyrene Substances 0.000 description 3
- 229910052581 Si3N4 Inorganic materials 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- 239000001768 carboxy methyl cellulose Substances 0.000 description 3
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 3
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 3
- 235000014113 dietary fatty acids Nutrition 0.000 description 3
- 239000000194 fatty acid Substances 0.000 description 3
- 229930195729 fatty acid Natural products 0.000 description 3
- 150000004665 fatty acids Chemical class 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
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- 229920002223 polystyrene Polymers 0.000 description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 3
- LNAZSHAWQACDHT-XIYTZBAFSA-N (2r,3r,4s,5r,6s)-4,5-dimethoxy-2-(methoxymethyl)-3-[(2s,3r,4s,5r,6r)-3,4,5-trimethoxy-6-(methoxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6r)-4,5,6-trimethoxy-2-(methoxymethyl)oxan-3-yl]oxyoxane Chemical compound CO[C@@H]1[C@@H](OC)[C@H](OC)[C@@H](COC)O[C@H]1O[C@H]1[C@H](OC)[C@@H](OC)[C@H](O[C@H]2[C@@H]([C@@H](OC)[C@H](OC)O[C@@H]2COC)OC)O[C@@H]1COC LNAZSHAWQACDHT-XIYTZBAFSA-N 0.000 description 2
- 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 2
- 229910052582 BN Inorganic materials 0.000 description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 2
- FIPWRIJSWJWJAI-UHFFFAOYSA-N Butyl carbitol 6-propylpiperonyl ether Chemical compound C1=C(CCC)C(COCCOCCOCCCC)=CC2=C1OCO2 FIPWRIJSWJWJAI-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000001856 Ethyl cellulose Substances 0.000 description 2
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 239000004113 Sepiolite Substances 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000002671 adjuvant Substances 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- OJMOMXZKOWKUTA-UHFFFAOYSA-N aluminum;borate Chemical compound [Al+3].[O-]B([O-])[O-] OJMOMXZKOWKUTA-UHFFFAOYSA-N 0.000 description 2
- 229960000892 attapulgite Drugs 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 2
- 239000002612 dispersion medium Substances 0.000 description 2
- 229920001249 ethyl cellulose Polymers 0.000 description 2
- 235000019325 ethyl cellulose Nutrition 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000010881 fly ash Substances 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 2
- 229910052574 oxide ceramic Inorganic materials 0.000 description 2
- 239000011224 oxide ceramic Substances 0.000 description 2
- 229910052625 palygorskite Inorganic materials 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 2
- 235000019353 potassium silicate Nutrition 0.000 description 2
- 239000003566 sealing material Substances 0.000 description 2
- 229910052624 sepiolite Inorganic materials 0.000 description 2
- 235000019355 sepiolite Nutrition 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000000344 soap Substances 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 230000008646 thermal stress Effects 0.000 description 2
- WTHDKMILWLGDKL-UHFFFAOYSA-N urea;hydrate Chemical compound O.NC(N)=O WTHDKMILWLGDKL-UHFFFAOYSA-N 0.000 description 2
- 238000007088 Archimedes method Methods 0.000 description 1
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
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- 239000002253 acid Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- UNYSKUBLZGJSLV-UHFFFAOYSA-L calcium;1,3,5,2,4,6$l^{2}-trioxadisilaluminane 2,4-dioxide;dihydroxide;hexahydrate Chemical compound O.O.O.O.O.O.[OH-].[OH-].[Ca+2].O=[Si]1O[Al]O[Si](=O)O1.O=[Si]1O[Al]O[Si](=O)O1 UNYSKUBLZGJSLV-UHFFFAOYSA-L 0.000 description 1
- 238000009924 canning Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 229910052676 chabazite Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
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- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- YGANSGVIUGARFR-UHFFFAOYSA-N dipotassium dioxosilane oxo(oxoalumanyloxy)alumane oxygen(2-) Chemical compound [O--].[K+].[K+].O=[Si]=O.O=[Al]O[Al]=O YGANSGVIUGARFR-UHFFFAOYSA-N 0.000 description 1
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- 150000002500 ions Chemical class 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
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- 229910052627 muscovite Inorganic materials 0.000 description 1
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- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
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Images
Classifications
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- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
- B01J29/72—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing iron group metals, noble metals or copper
- B01J29/76—Iron group metals or copper
- B01J29/763—CHA-type, e.g. Chabazite, LZ-218
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- 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
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- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
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- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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- B01J2229/10—After treatment, characterised by the effect to be obtained
- B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
- B01J2229/186—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself not in framework positions
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Description
なお、CHAの平均粒子径は、走査型電子顕微鏡(SEM)を用いて測定した一次粒子の平均粒子径である。
なお、無機粒子の平均粒子径は、レーザー回折・散乱法によって求めた粒度分布(体積基準)における積算値50%での粒径(Dv50)である。
上記の組み合わせの中で、無機粒子の平均粒子径は、CHAの平均粒子径の1/5〜50倍であることが望ましく、1/3〜30倍であることがより望ましく、1/2〜10倍であることがさらに望ましい。
特に、無機粒子の平均粒子径は、CHAの平均粒子径より大きく、CHAの平均粒子径の4倍以下であることが望ましい。
まず、ゼオライトと無機バインダとを含み、必要に応じて、無機繊維、鱗片状物質、テトラポット状物質及び三次元針状物質からなる群より選択される一種以上や無機粒子をさらに含む原料ペーストを用いて押出成形し、複数の貫通孔が隔壁を隔てて長手方向に並設されている円柱状のハニカム成形体を作製する。
造孔材としては、特に限定されないが、ポリスチレン粒子、アクリル粒子、澱粉等が挙げられ、二種以上併用してもよい。これらの中では、ポリスチレン粒子が望ましい。
例えば、CHAの平均粒子径が0.1μmである場合、平均粒子径が0.1〜3μmである造孔材をCHA体積添加量に対して10〜30%添加することにより、隔壁の平均気孔径を0.05〜0.2μmとすることができる。なお、CHAの平均粒子径が1.2μmである場合には、造孔材を添加しなくてもよい。
まず、ハニカム触媒10を構成するハニカムユニット11と同様にして、扇柱状のハニカムユニット11´を作製する。次に、ハニカムユニット11´の円弧側を除く外周面に接着層用ペーストを塗布して、ハニカムユニット11´を接着させ、乾燥固化することにより、ハニカムユニット11´の集合体を作製する。
ゼオライトとして平均粒子径が0.1μmのCHAを27質量%、無機粒子として平均粒子径が0.2μmのチタニアを13質量%、無機バインダとしてベーマイトを5質量%、平均繊維径が6.5μm、平均繊維長が100μmのガラス繊維を8質量%、造孔材として平均粒子径が0.8μmのポリスチレン粒子を6質量%、メチルセルロースを5質量%、成形助剤として脂肪酸石鹸を4質量%及びイオン交換水を32質量%混合混練して、原料ペースト1を作製した。なお、ゼオライトとしては、比重2.02、組成比Si/Al:32、比表面積600m2/g、銅イオンでイオン交換されているCHAを用いた。
実施例1において、ゼオライト及び無機粒子の体積比(CHA:チタニア)は、80:20である。
また、ハニカムユニット11´は、ハニカムユニット11´の見掛けの体積当たり、ゼオライトを197g/L含有しており、銅イオンを6.4g/L含有している。
ゼオライト及び無機粒子の体積比(CHA:チタニア)をそれぞれ70:30、60:40に変更した以外は、実施例1と同様にして、ハニカムユニット11´を作製した。
ゼオライト及び無機粒子の体積比(CHA:チタニア)を100:0に変更した以外は、実施例1と同様にして、ハニカムユニット11´を作製した。つまり、比較例1では、無機粒子(チタニア)を用いなかった。
ゼオライト及び無機粒子の体積比(CHA:チタニア)を40:60、20:80に変更した以外は、実施例1と同様にして、ハニカムユニット11´を作製した。
ゼオライト及び無機粒子の体積比(CHA:チタニア)を0:100に変更した以外は、実施例1と同様にして、ハニカムユニット11´を作製した。つまり、参考例3では、ゼオライト(CHA)を用いなかった。
実施例1〜3、参考例1〜3及び比較例1で作製したハニカムユニットについて、水銀圧入法を用いて平均気孔径及び気孔径分布を測定した。
水銀圧入法による具体的な測定手順としては、各ハニカムユニットを0.8cm程度の立方体に切断し、イオン交換水で超音波洗浄し、十分乾燥して測定用サンプルとした。次に、測定用サンプルの気孔径を、水銀ポロシメーター(島津製作所製、オートポアIII9405)を用いて接触角を130°、表面張力を485mN/mとして測定した。測定範囲は、0.005〜350μmとした。
さらに、全気孔の容積に対する0.05μm以下の気孔径を有する気孔の容積の割合[%]を算出した。
これらの測定結果を表1に示す。表1では、全気孔の容積に対する0.05μm以下の気孔径を有する気孔の容積の割合を「気孔径0.05μm以下の気孔の割合[%]」と記載している。
実施例1〜3、参考例1及び比較例1で作製したハニカムユニットを一辺38mm、長さ10mmに切り出し、水に浸漬し、含水率を80%としたときの体積変化率[%]を求め、その値を吸水変位とした。結果を表1に示す。
なお、ハニカムユニットの含水率は、電子天秤(A&D製 HR202i)を用いて絶乾時の重量と含水時の重量を測定し算出した。
図5より、気孔径0.05μm以下の気孔の割合が25%以下であると、吸水変位が急激に減少することが分かる。なお、上記割合が25%以下である場合、室温から700℃まで昇温し、その後50℃まで降温する吸脱水試験を行っても、ハニカムユニットにクラックが発生しないことが確認されている。したがって、気孔径0.05μm以下の気孔の割合を25%以下とすることにより、吸水によるクラックの発生を好適に防ぐことができると考えられる。
実施例1〜3及び参考例1で作製したハニカムユニットから、ダイヤモンドカッターを用いて、直径:1インチ、長さ:3インチの円柱状試験片を切り出した。これらの試験片に、200℃又は525℃の模擬ガスを空間速度(SV)40000/hr(200℃)、100000(525℃)で流しながら、触媒評価装置(堀場製作所社製、SIGU−2000/MEXA−6000FT)を用いて、試料から流出するNOxの流出量を測定し、式
(NOxの流入量−NOxの流出量)/(NOxの流入量)×100
で表されるNOxの浄化率[%]を算出した。算出結果を表2に示す。なお、模擬ガスの構成成分は、一酸化窒素260ppm、二酸化窒素90ppm、アンモニア350ppm(200℃)、一酸化窒素315ppm、二酸化窒素35ppm、アンモニア385ppm(525℃)、酸素10%、二酸化炭素5%、水5%、窒素(balance)である。
係る必須の構成要件に、本発明の詳細な説明で詳述した種々の構成(例えば、ゼオライトの構成、無機バインダの構成、ハニカムユニットの構成、ハニカム触媒の製造条件、排ガス浄化装置の構成等)を適宜組み合わせることにより所望の効果を得ることができる。
11、11´ ハニカムユニット
11a 貫通孔
11b 隔壁
12 外周コート層
13 接着層
20 保持シール材
30 金属容器
100 排ガス浄化装置
G 排ガス
Claims (11)
- 複数の貫通孔が隔壁を隔てて長手方向に並設されたハニカムユニットを備えたハニカム触媒であって、
前記ハニカムユニットは、ゼオライトと無機バインダとを含み、
前記ゼオライトは、CHA構造を有するアルミノケイ酸塩で、その組成比Si/Alが15〜50であり、
前記隔壁の平均気孔径が、0.05〜0.2μmであり、
0.05μm以下の気孔径を有する気孔の容積が、全気孔の容積の25%以下であることを特徴とするハニカム触媒。 - 前記ハニカムユニットは、無機粒子をさらに含む請求項1に記載のハニカム触媒。
- 前記ゼオライトの平均粒子径は、0.1〜2.0μmであり、前記無機粒子の平均粒子径は、0.1〜5.0μmである請求項2に記載のハニカム触媒。
- 前記無機粒子の平均粒子径は、前記ゼオライトの平均粒子径の1/5〜50倍である請求項3に記載のハニカム触媒。
- 前記ゼオライト及び前記無機粒子の体積比(ゼオライト:無機粒子)が、50:50〜90:10である請求項2〜4のいずれかに記載のハニカム触媒。
- 前記無機粒子は、アルミナ、チタニア及びジルコニアからなる群より選択される一種以上である請求項2〜5のいずれかに記載のハニカム触媒。
- 前記ゼオライトは、銅イオンでイオン交換されている請求項1〜6のいずれかに記載のハニカム触媒。
- 前記ハニカムユニットは、前記銅イオンを前記ハニカムユニットの見掛けの体積当たり5.5〜7.5g/L含有する請求項7に記載のハニカム触媒。
- 前記ハニカムユニットは、前記ゼオライトを前記ハニカムユニットの見掛けの体積当たり150〜250g/L含有する請求項1〜8のいずれかに記載のハニカム触媒。
- 前記ハニカムユニットは、無機繊維、鱗片状物質、テトラポット状物質及び三次元針状物質からなる群より選択される一種以上をさらに含む請求項1〜9のいずれかに記載のハニカム触媒。
- 請求項1〜10のいずれかに記載のハニカム触媒を備えることを特徴とする排ガス浄化装置。
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