WO2005033037A2 - High porosity honeycomb and method - Google Patents
High porosity honeycomb and method Download PDFInfo
- Publication number
- WO2005033037A2 WO2005033037A2 PCT/US2004/031019 US2004031019W WO2005033037A2 WO 2005033037 A2 WO2005033037 A2 WO 2005033037A2 US 2004031019 W US2004031019 W US 2004031019W WO 2005033037 A2 WO2005033037 A2 WO 2005033037A2
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- honeycomb
- pore former
- range
- oil
- micrometers
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims description 30
- 239000011148 porous material Substances 0.000 claims abstract description 53
- 239000000758 substrate Substances 0.000 claims abstract description 29
- 239000000919 ceramic Substances 0.000 claims abstract description 28
- 230000003197 catalytic effect Effects 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims description 33
- 239000011230 binding agent Substances 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 21
- 239000000843 powder Substances 0.000 claims description 20
- 239000001993 wax Substances 0.000 claims description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- 229910052878 cordierite Inorganic materials 0.000 claims description 16
- 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 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 14
- -1 polyethylene Polymers 0.000 claims description 14
- 239000004698 Polyethylene Substances 0.000 claims description 11
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 11
- 229910010293 ceramic material Inorganic materials 0.000 claims description 11
- 239000006185 dispersion Substances 0.000 claims description 11
- 229920000573 polyethylene Polymers 0.000 claims description 11
- 239000004094 surface-active agent Substances 0.000 claims description 10
- 239000004927 clay Substances 0.000 claims description 8
- 229910052570 clay Inorganic materials 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- 230000001413 cellular effect Effects 0.000 claims description 7
- 239000000454 talc Substances 0.000 claims description 6
- 229910052623 talc Inorganic materials 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229920003086 cellulose ether Polymers 0.000 claims description 4
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 4
- 229920000609 methyl cellulose Polymers 0.000 claims description 4
- 239000001923 methylcellulose Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- 239000005642 Oleic acid Substances 0.000 claims description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- 235000021355 Stearic acid Nutrition 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims description 2
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- 150000001340 alkali metals Chemical class 0.000 claims description 2
- 150000001408 amides Chemical class 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 239000011575 calcium Substances 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000001913 cellulose Substances 0.000 claims description 2
- 229920002678 cellulose Polymers 0.000 claims description 2
- 229910052732 germanium Inorganic materials 0.000 claims description 2
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 2
- 229910052622 kaolinite Inorganic materials 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000004200 microcrystalline wax Substances 0.000 claims description 2
- 235000019808 microcrystalline wax Nutrition 0.000 claims description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical group CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 2
- 239000012188 paraffin wax Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 229910052596 spinel Inorganic materials 0.000 claims description 2
- 239000011029 spinel Substances 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 239000008117 stearic acid Substances 0.000 claims description 2
- 229920002994 synthetic fiber Polymers 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 229910052723 transition metal Inorganic materials 0.000 claims description 2
- 150000003624 transition metals Chemical class 0.000 claims description 2
- 238000013329 compounding Methods 0.000 claims 3
- 229910052681 coesite Inorganic materials 0.000 claims 1
- 229910052593 corundum Inorganic materials 0.000 claims 1
- 229910052906 cristobalite Inorganic materials 0.000 claims 1
- 238000007580 dry-mixing Methods 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- 229910052500 inorganic mineral Inorganic materials 0.000 claims 1
- 239000011707 mineral Substances 0.000 claims 1
- 239000011236 particulate material Substances 0.000 claims 1
- 238000012216 screening Methods 0.000 claims 1
- 229910052682 stishovite Inorganic materials 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- 229910052905 tridymite Inorganic materials 0.000 claims 1
- 229910001845 yogo sapphire Inorganic materials 0.000 claims 1
- 241000264877 Hippospongia communis Species 0.000 description 26
- 210000004027 cell Anatomy 0.000 description 21
- 239000003921 oil Substances 0.000 description 9
- 238000010304 firing Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 5
- 238000001125 extrusion Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 150000004645 aluminates Chemical class 0.000 description 3
- 210000002421 cell wall Anatomy 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 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 3
- 239000007789 gas Substances 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052863 mullite Inorganic materials 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- 229910000951 Aluminide Inorganic materials 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001642 boronic acid derivatives Chemical class 0.000 description 2
- 238000009924 canning Methods 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 150000001247 metal acetylides Chemical class 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000002459 porosimetry Methods 0.000 description 2
- 150000004760 silicates Chemical class 0.000 description 2
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910001593 boehmite Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 238000007571 dilatometry Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000003502 gasoline Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
Classifications
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- 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
- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
- F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
- F01N3/24—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by constructional aspects of converting apparatus
- F01N3/28—Construction of catalytic reactors
- F01N3/2803—Construction of catalytic reactors characterised by structure, by material or by manufacturing of catalyst support
- F01N3/2825—Ceramics
- F01N3/2828—Ceramic multi-channel monoliths, e.g. honeycombs
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
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- B01D46/2418—Honeycomb filters
- B01D46/2425—Honeycomb filters characterized by parameters related to the physical properties of the honeycomb structure material
- B01D46/2429—Honeycomb filters characterized by parameters related to the physical properties of the honeycomb structure material of the honeycomb walls or cells
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- B01D46/2403—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies characterised by the physical shape or structure of the filtering element
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- B01D46/2425—Honeycomb filters characterized by parameters related to the physical properties of the honeycomb structure material
- B01D46/24491—Porosity
-
- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D46/24—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies
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- B01D46/2418—Honeycomb filters
- B01D46/2425—Honeycomb filters characterized by parameters related to the physical properties of the honeycomb structure material
- B01D46/24493—Modulus of rupture
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D46/2403—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies characterised by the physical shape or structure of the filtering element
- B01D46/2418—Honeycomb filters
- B01D46/2425—Honeycomb filters characterized by parameters related to the physical properties of the honeycomb structure material
- B01D46/24494—Thermal expansion coefficient, heat capacity or thermal conductivity
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- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
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- B01D46/2418—Honeycomb filters
- B01D46/2451—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure
- B01D46/2474—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure of the walls along the length of the honeycomb
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/56—Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional monoliths
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- 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
- B01J37/0009—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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- 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
- C04B35/195—Alkaline earth aluminosilicates, e.g. cordierite or anorthite
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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- F01N2330/06—Ceramic, e.g. monoliths
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Definitions
- the present invention relates to ceramic bodies for use in automotive catalytic converter systems, and in particular to high porosity honeycomb substrates having reduced thermal mass and offering faster light-off performance.
- hydrocarbon fuels such as hydrocarbon gases, gasoline or diesel fuel
- NOx nitrogen oxides
- CO carbon monoxide
- Cordierite substrates typically in the form of honeycomb structures, have long been preferred for use as substrates to support catalytically active components in part due to the high thermal shock resistance of such structures.
- Increasingly stringent regulations in recent years have been requiring higher conversion efficiencies in catalytic converters for the automotive market.
- Automobile emissions can be significantly reduced by controlling the light-off process. More than fifty percent of a vehicle's total emission is generated before light-off takes place.
- the light-off time of a substrate is controlled to a large degree by its thermal mass; specifically, a lower thermal mass results in faster light-off times.
- One way to achieve a lower thermal mass is to reduce the thickness of the cell webs. Accordingly, demand for substrates having very thin webs (i.e., less than 2.5 mil (0.0025 inch, 0.0635 mm)) has dramatically increased. In addition to reduced mass, such structures may possess higher geometric surface areas, as well as lower backpressures.
- reducing the thickness of cell webs significantly diminishes the strength of the body. This causes problems during the canning process of the catalytic converter substrate.
- An alternative way to reduce the thermal mass of a catalytic converter substrate is to increase the porosity while maintaining the cell density and wall thickness substantially constant. However, it is still important to maintain a low thermal expansion coefficient to prevent failures due to thermal shock. Unfortunately, high levels of porosity and low thermal expansion are known to reduce the strength of the honeycomb substrate.
- the invention is a high porosity ceramic honeycomb substrate for use in an automotive catalytic converter system which exhibits improved light-off performance.
- the honeycomb substrate which is defined by a body having an inlet end, an outlet end, and a multiplicity of cells, is further characterized by cell walls having a thickness of greater than 2.0 mil (0.0020 inch, 0.0508 mm), preferably in the range of 2.5 mil (0.0025 in., 0.0635 mm) to 7 mil (0.0070 in., 0.1778 mm).
- the inventive articles exhibit a total porosity in the range of 45 to 75 %, preferably 50 to 65%, and most preferably 55%; a median pore diameter in the range of 2 to 10 micrometers, preferably in the range of 2 to 4 micrometers, and most preferably 3 micrometers.
- the inventive articles exhibit a coefficient of thermal expansion (CTE) (25-800 °C) of less than 15 x 10 "7 /°C, preferably less than 10 x 10 "7 /°C.
- CTE coefficient of thermal expansion
- MOR modulus of rupture
- the invention is also a method for forming a high porosity ceramic honeycomb substrate for use in a catalytic converter system as described following herein.
- a batch of components is compounded, the batch being composed of ceramic powder material, a plasticizing binder system, and, a pore former having a mean particle diameter of 1 to 30 micrometers, preferably 2 to 18 micrometers.
- the components are batched to form a plasticized mixture.
- the plasticized mixture is then extruded through a die to form a green honeycomb body, and then the structure is fired at a temperature and for a time sufficient to form the desired properties.
- Preferred embodiments of the inventive forming method are further described below.
- FIG. 1 is a graph based on chemical reaction modeling illustrating the predicted improved light-off time in a high porosity cordierite honeycomb substrate according to the present invention
- FIG. 2 is a scanning electron micrograph taken at 487X magnification of a high porosity cordierite honeycomb substrate according to the present invention.
- FIG. 3 is a scanning electron micrograph taken at 487X magnification of a commercially available cordierite honeycomb substrate.
- the ceramic honeycomb substrate of the present invention combines the attractive attributes of a very thin-walled structure having a fast-light off time, as a virtue of high porosity in the range of 45 to 75 %, with a more conventional substrate geometry defining cell webs having a thickness of greater than 2.0 mil (0.0020 inch, O.0508 mm).
- the porosity is preferably in the range of 50 to 65%, and most preferably 55%.
- the wall thickness is between 2.5 mil (0.0025 in., 0.0635 mm) to 7 mil (0.0070 in., 0.1778 mm), and more preferably between 2.5 mil (0.0025 in., 0.0635 mm) to 3 mil (0.0030 in., 0.0762 mm).
- the cell density of the inventive honeycomb is not critical, but depends on particular applications. Generally, cell densities of 400 cells/in 2 (62 cells/cm 2 ) to 900 cells/in 2 (140 cells/cm 2 ) are suitable for purposes of the present invention. [0016] In an embodiment the inventive structure exhibits a low coefficient of thermal expansion (CTE) (25-800°C) of less than 15 x 10 "7 /°C, preferably less than 10 x 10 "7 /°C. The low thermal expansion imparts the honeycomb body with a high thermal shock resistance making it suitable for use in harsh environments.
- CTE coefficient of thermal expansion
- the inventive structure demonstrates high structural strength as provided by a modulus of rupture (MOR), as measured on a cellular bar sample, of 200-400 psi, preferably 350 psi.
- MOR modulus of rupture
- the ceramic material comprising the honeycomb of the present invention is not critical and can include anyone of silicates, oxides, aluminates, nitrides, borates, carbides, borides and aluminides.
- the invention is particularly suitable for ceramic honeycomb substrates which contain cordierite and/or mullite. Examples of such mixtures being 0-60% by weight mullite, and 30-100% by weight cordierite, with allowance for other phases, typically up to 10% by weight.
- FIG. 1 therein illustrated is a comparison between the light-off time of inventive and comparative cordierite substrates.
- Both substrates have a geometry of 900 cell/in 2 (140 cells/cm 2 ) and a cell wall thickness of 2.5 mil (0.0025 in., 0.0635 mm).
- the inventive substrate is modeled with a porosity of 63% and the comparative substrate with a porosity of 25%.
- an improvement of 5.5 seconds in light-off is predicted in the inventive substrate. This is significantly faster than the equivalent comparative substrate with lower porosity.
- the invention also relates to a method for forming the inventive structures.
- a batch of components is first compounded.
- the components of the batch include ceramic powder materials, a plasticizing binder system and a pore former.
- the invention works with a variety of inorganic ceramic powders including amorphous, crystalline or semi- crystalline material selected from the group consisting of silicate, borate or aluminate glasses or crystalline or semi-crystalline silicates, oxides, aluminates, borates, carbides, nitrides, borides and aluminides.
- Ceramic powder materials include cordierite, spinel, clay, talc, alumina, aluminurr ⁇ hydroxide, silica, and oxides of calcium, magnesium, boron, titanium, germanium, and the alkali and transition metals.
- Some ceramic batch material compositions for forming cordierite that are especially suited to the practice of the present invention are those disclosed in U.S. Pat. No. 6,506,336 Bl which is herein incorporated by reference in its entirety.
- One composition which ultimately forms cordierite upon firing is as follows in percent by weight: 33 to 41 aluminum oxide, 46 to 53 silica, and 11 to 17 magnesium oxide.
- Suitable cordierite-forming inorganic ceramic powder raw materials include high-purity clay, talc, silica, alumina, aluminum hydroxide, and magnesia (IVlgO)-yieldmg raw materials.
- the preferred cordierite-forming powder materials include kaolinite clay, talc, alumina and silica.
- Suitable clays are delaminated kaolinite raw clay having a mean particle size of less than 2 micrometers, such as KAOPAQUE-10TM (K10) clay and calcined clay having a mean particle size of less than 2 micrometers and a surface area of greater than 10 m 2 /g, such as Glomax LLTM, all available from Dry Branch Kaolin.
- KAOPAQUE-10TM K10
- calcined clay having a mean particle size of less than 2 micrometers and a surface area of greater than 10 m 2 /g, such as Glomax LLTM, all available from Dry Branch Kaolin.
- a suitable talc has a morphology index (refer to U.S. Pat. No.
- the alumina source has a mean particle size of 5 micrometers or less, preferably 1 micrometer or less.
- the alumina source can be any of alumina, aluminum hydroxide, aluminum oxyhydroxide, and combinations thereof, the source preferably comprising boehmite or pseudoboehmite.
- a suitable alumina source includes A1000SGDTM from Alcoa and/or DispalTM Alumina from Sasol jNorth America, Inc.
- a suitable silica has a mean particle size of less than 5 micrometers, and a surface area of about 4-6 m 2 /g, an example of which is LMSILTM sold by Unimin Corporation.
- the plasticizing binder system used in the present invention will depend in part on the composition and morphology of the ceramic powder materials of the batch.
- an aqueous binder system comprising a cellulose ether binder selected from the group consisting of methylcellulose, methylcellulose derivates and combinations thereof, a surfactant component such as stearic acid or oleic acid, an oil or oil-based component preferably a low molecular weight oil, such as polyalpholefin, and a water vehicle can provide highly plastic batches.
- the binder system comprises, based on 100 parts by weight of ceramic powder materials, 2 to 25 parts by weight of the cellulose ether binder, 0.5 to 10 parts by weight of the surfactant, 2 to 25 parts by weight of the oil, and 30 to 100 parts by weight of the water vehicle.
- the components of the binder system are added as super- additions such that the weight amount is computed as (mass of binder, surfactant, oil or water)/(mass of ceramic material) x 100%.
- the batch further comprises a large amount of pore former.
- the pore former is added as a supper-addition such that the weight amount is computed as (mass of binder, surfactant, oil or "water)/(mass of ceramic material) x 100%.
- the pore former is added in an amount of 15-85% by weight, preferably 30-70 % by weight, and has a mean particle size of 2 to 18 micrometers, preferably 3 to 8 micrometers. Pore formers with a mean particle size smaller than 2 micrometers are ineffective resulting in high shrinkage rather than creating the desired porosity.
- Pore former with a mean particle size larger than 18 micrometers decrease the strength of the resulting fired structure.
- the pore former may be any natural or synthetic material capable of forming relic pores by evaporation or degradation during firing, and can include materials such as carbon, graphite, starch, cellulose, natural and synthetic waxes.
- the pore former is a wax having a high melting point of at least 70° C, such as paraffin wax, microcrystalline wax, polyethylene wax, synthetic amides, chlorinated waxes, and dispersions thereof.
- dispenser is meant the pore former is present in a liquid environment wherein the solid loadings are less than 50 wt.%.
- the pore former is polyethylene wax or a dispersion thereof.
- the wax pore former is removed before firing by using a vacuum or an inert atmosphere.
- the batch components namely the ceramic powder material, the plasticizing binder system and the pore former are mixed to form a plasticized mixture.
- a portion of the powdered ceramic material is first mixed with a pore former dispersion to form a uniform mixture.
- the mixture is dried and screened to obtain a particulate pore forming material mixture having a composition consisting essentially of 60-85 wt.%, preferably 70 wt.%, pore former, 5-25 wt.%, preferably 15 wt.%, ceramic material and 2-20 wt.%, preferably 10 wt.% water.
- the remaining powdered ceramic material is then dry-blended with the binder, the resulting dry-blend then added to the particulate pore forming material mixture.
- the plasticizing binder system namely the surfactant component, the oil or oil-based component and the water vehicle.
- the water content can vary depending on the type of material to impart optimum handing properties and compatibility with other components in the mixture. From a practical standpoint the water content in the practice of this embodiment is usually about 30 to 100 parts, preferably 43 parts, based on 100 parts by weight of ceramic powder materials.
- the wet mix is then sheared in any suitable mixer in which the batch will be plasticized.
- a suitable pore former dispersion is polyethylene wax dispersion, available from Michelman Inc., sold under the brand name of Michem GuardTM 10, 15, 20, 25, 55, and 60.
- the sinterable ceramic material, the binder and powdered pore former are first dry-mixed to form a uniform blend. Thereafter, the surfactant, oil and water vehicle are added to the resulting dry blend.
- the mixture may be mixed in a mixer such as a LittlefordTM.
- the water vehicle is added in an amount that is needed to plasticize the batch, typically 30 to 100 parts, preferably 43 parts, based on 100 parts by weight of ceramic powder materials.
- the amount of water can vary from one batch of material to another and therefore is determined by pre-testing the particular batch for extrudability.
- the wet mixture is then plasticized by known means.
- Suitable pore formers are polyethylene wax powders available from Michelman Inc., sold under the brand name of MichemWaxTM 410, 411, 436, 437, 439 and 492.
- Other useful pore formers include micronized polyethylene wax powders available from Honeywell, sold under the brand name of ACumist A6, A12, A18, B6, B9, B12, B18, C5, C12, C18, D5, D9, E6. E12, 3105, 3205, 3305, 1106, 1109, 1112, 1204, 1306, and 1309.
- the resulting plasticized batch is then shaped, preferably by extrusion, into a green body, such as a honeycomb through a honeycomb extrusion die.
- honeycomb structure has an inlet and an outlet end or face, and a multiplicity of cells extending between the inlet and outlet ends.
- Inventive honeycomb bodies can be made with a variety of cellular densities tailored to the desired application.
- the present invention is particularly suitable for the formation of very high cellular densities range preferably as high as 900 cells/in 2 (140 cells/cm 2 ) with cell walls of greater than 2 mil (0.002O inch, 0.0508 mm) in thickness, preferably in the range of 2.5 mil (0.0025 in., 0.0635 mm) to 7 mil (0.0070 in., 0.1778 mm), and more preferably in the range of 2.5 mil (0.O025 in., 0.0635 mm) to 3 mil (0.0030 in., 0.0762 mm).
- the pore former Prior to firing the pore former is removed from the green bodies (which may be optionally first dried) by heating under a vacuum or in an inert atmosphere.
- a commercially available vacuum pyrolyzer may be used to heat up green bodies under vacuum to a temperature and for a time sufficient to substantially extract the pore former.
- the green bodies may be heated in nitrogen to a temperature and for a time to achieve substantially the same thing.
- a suitable temperature may be 500-600 °C or higher, for a period of 12 hours or longer.
- the bodies are fired in air to a maximum temperature of about 1400 °C, with a hold of 8 hours at the maximum temperature for a total cycle time of 48 hours, or longer as needed.
- a ceramic structure comprised predominately of a phase approximating the stoichiometry Mg 2 Al Si 5 O 18 .
- Comparative (non-inventive) and inventive examples are prepared by mixing together selected raw materials from Table 1 in the proportions listed in Table 2.
- Comparative example 1 is prepared according to the teachings of U.S. Pat. No. 6,506,336 and is absent a pore former.
- Inventive examples 1-4 are prepared by using a polyethylene wax dispersion to form a particulate pore forming material mixture as described above.
- Inventive example 5 is prepared by using a powdered polyethylene wax as the pore former.
- the plasticized mixtures are extruded through a honeycomb-forming die under conditions suitable to form monoliths having a cellular density of between about 640-960 cells/in 2 (99-149 cells/cm 2 ) and a wall thickness of between about 2.8-4.2 mil (0.0028- 0.0042 inch).
- the green ceramic honeycombs were sufficiently dried to remove water or other liquid phases that might be present and thereafter, first subjected to a heating in a commercially-available vacuum pyrolizer from room temperature to 500 °C over a period of 12 hours to remove the pore former, followed by a second firing from room temperature to 1400°C with a hold of 8 hours for a cycle total time of 48 hours or longer to sinter and form the final product structure; i.e., firing conditions suitable for forming cordierite ceramic bodies.
- cordierite honeycomb structures having cell with a wall thickness of greater than 2.0 mil (0.0020 inch, 0.0508 mm), a total porosity in the range of 45 to 75 %, a median pore diameter in the range of 2-10 micrometers, a coefficient of thermal expansion (CTE) (25-800°C) of less than 15 x 10 "7 /°C, and a modulus of rupture (MOR) honeycomb strength in the range of 200-400 psi have been obtained.
- CTE coefficient of thermal expansion
- MOR modulus of rupture
- FIG. 3 is a scanning electron micrograph taken at a magnification of 487X of a polished web section of a commercially available cordierite honeycomb body having a porosity of 33% and a median pore size of 1.3 micrometers.
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Geometry (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Thermal Sciences (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Combustion & Propulsion (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
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- Exhaust Gas After Treatment (AREA)
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Abstract
Description
Claims
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2006533959A JP4795958B2 (en) | 2003-09-30 | 2004-09-21 | Highly porous honeycomb and manufacturing method thereof |
EP04788899.5A EP1667942B1 (en) | 2003-09-30 | 2004-09-21 | High porosity honeycomb and method |
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US10/676,863 | 2003-09-30 | ||
US10/676,863 US7442425B2 (en) | 2003-09-30 | 2003-09-30 | High porosity honeycomb and method |
Publications (2)
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WO2005033037A2 true WO2005033037A2 (en) | 2005-04-14 |
WO2005033037A3 WO2005033037A3 (en) | 2006-05-11 |
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PCT/US2004/031019 WO2005033037A2 (en) | 2003-09-30 | 2004-09-21 | High porosity honeycomb and method |
Country Status (5)
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US (2) | US7442425B2 (en) |
EP (1) | EP1667942B1 (en) |
JP (1) | JP4795958B2 (en) |
CN (1) | CN100537213C (en) |
WO (1) | WO2005033037A2 (en) |
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- 2004-09-21 EP EP04788899.5A patent/EP1667942B1/en not_active Expired - Lifetime
- 2004-09-21 JP JP2006533959A patent/JP4795958B2/en not_active Expired - Fee Related
- 2004-09-21 CN CNB2004800279264A patent/CN100537213C/en not_active Expired - Fee Related
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US8389101B2 (en) | 2009-05-29 | 2013-03-05 | Corning Incorporated | Lanthanum-containing cordierite body and method of manufacture |
Also Published As
Publication number | Publication date |
---|---|
CN100537213C (en) | 2009-09-09 |
EP1667942A2 (en) | 2006-06-14 |
US20090041976A1 (en) | 2009-02-12 |
WO2005033037A3 (en) | 2006-05-11 |
EP1667942B1 (en) | 2018-06-13 |
US8697222B2 (en) | 2014-04-15 |
US20050069469A1 (en) | 2005-03-31 |
US7442425B2 (en) | 2008-10-28 |
EP1667942A4 (en) | 2010-07-28 |
JP2007507667A (en) | 2007-03-29 |
CN1856398A (en) | 2006-11-01 |
JP4795958B2 (en) | 2011-10-19 |
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