WO2004035207A1 - 炭化珪素質触媒体及びその製造方法 - Google Patents
炭化珪素質触媒体及びその製造方法 Download PDFInfo
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- WO2004035207A1 WO2004035207A1 PCT/JP2003/013189 JP0313189W WO2004035207A1 WO 2004035207 A1 WO2004035207 A1 WO 2004035207A1 JP 0313189 W JP0313189 W JP 0313189W WO 2004035207 A1 WO2004035207 A1 WO 2004035207A1
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- Prior art keywords
- silicon carbide
- catalyst
- silicon
- carbide particles
- metal
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 103
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 94
- 239000000463 material Substances 0.000 title abstract description 14
- 230000003197 catalytic effect Effects 0.000 title abstract description 5
- 238000000034 method Methods 0.000 title description 7
- 239000003054 catalyst Substances 0.000 claims abstract description 121
- 239000002245 particle Substances 0.000 claims abstract description 53
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 15
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 15
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims abstract description 14
- 150000001342 alkaline earth metals Chemical class 0.000 claims abstract description 14
- 239000011248 coating agent Substances 0.000 claims abstract description 9
- 238000000576 coating method Methods 0.000 claims abstract description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 40
- 229910052710 silicon Inorganic materials 0.000 claims description 39
- 239000010703 silicon Substances 0.000 claims description 39
- 229910052751 metal Inorganic materials 0.000 claims description 23
- 239000002184 metal Substances 0.000 claims description 23
- 238000004519 manufacturing process Methods 0.000 claims description 15
- 239000011148 porous material Substances 0.000 claims description 12
- 210000002808 connective tissue Anatomy 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 229910052906 cristobalite Inorganic materials 0.000 claims 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 claims description 3
- 229910052863 mullite Inorganic materials 0.000 claims description 3
- 238000003763 carbonization Methods 0.000 claims description 2
- 150000002739 metals Chemical class 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 6
- 239000002585 base Substances 0.000 abstract 1
- 229910052700 potassium Inorganic materials 0.000 description 20
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 19
- 239000011591 potassium Substances 0.000 description 19
- 238000010304 firing Methods 0.000 description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 9
- 238000003860 storage Methods 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000001354 calcination Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000470 constituent Substances 0.000 description 5
- 238000009792 diffusion process Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- 238000011068 loading method Methods 0.000 description 4
- 229910052697 platinum Inorganic materials 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000004927 clay Substances 0.000 description 3
- 238000000635 electron micrograph Methods 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 229910021426 porous silicon Inorganic materials 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052809 inorganic oxide Inorganic materials 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000005192 partition Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 230000001629 suppression Effects 0.000 description 2
- 210000001519 tissue Anatomy 0.000 description 2
- 229910001148 Al-Li alloy Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000012264 purified product Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
Classifications
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/0006—Honeycomb structures
- C04B38/0012—Honeycomb structures characterised by the material used for sealing or plugging (some of) the channels of the honeycombs
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- 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
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
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- 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
- B01D53/9422—Processes characterised by a specific catalyst for removing nitrogen oxides by NOx storage or reduction by cyclic switching between lean and rich exhaust gases (LNT, NSC, NSR)
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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
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
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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
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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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- B01J37/02—Impregnation, coating or precipitation
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- B01J37/02—Impregnation, coating or precipitation
- B01J37/024—Multiple impregnation or coating
- B01J37/0248—Coatings comprising impregnated particles
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- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/0081—Uses not provided for elsewhere in C04B2111/00 as catalysts or catalyst carriers
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3817—Carbides
- C04B2235/3826—Silicon carbides
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
- C04B2235/6021—Extrusion moulding
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/80—Phases present in the sintered or melt-cast ceramic products other than the main phase
Definitions
- the present invention relates to a silicon carbide-based catalyst body and a method for producing the same.
- the present invention relates to a catalyst-supporting silicon carbide-based catalyst used for purifying automobile exhaust gas and a method for producing the same.
- a filter Diesel Particulate Filter (DPF)
- DPF Diesel Particulate Filter
- a catalyst partition for forming a composite of a plurality of adjacent cells, and a honeycomb outer wall surrounding and holding the outermost peripheral cell located at the outermost periphery of the cell composite.
- the porous honeycomb structure is widely used, and refractory silicon carbide (SiC) is used as a constituent material thereof.
- honeycomb structure for example, silicon carbide powder having a predetermined specific surface area and containing impurities is used as a starting material, which is formed into a desired shape, dried, and then dried.
- a honeycomb-structured porous silicon carbide-based catalyst carrier obtained by firing in a temperature range of 200 ° C. is known (for example, see Japanese Patent Application Laid-Open No. Hei 6-182228).
- the silicon carbide component evaporates from the surface of the silicon carbide particles, and this is the contact portion between the particles (neck portion) ), The neck grows and a bonded state is obtained.
- a very high firing temperature is required to evaporate silicon carbide, which results in high costs, and a high thermal expansion material must be fired at a high temperature, which lowers the firing yield. There was a problem.
- a porous honeycomb structure containing refractory particles as an aggregate, particularly silicon carbide and metallic silicon, and a method for manufacturing the same are disclosed (for example, see Japanese Patent Application Laid-Open No. 20-210). 0 2—20 01 082 gazette).
- an alkali metal for example, potassium ( ⁇ )
- ⁇ ⁇
- the catalytic ability is rapidly deactivated. This is a problem that tends to occur when a porous body containing silicon carbide as a main component is used as a catalyst carrier regardless of the shape of the carrier that supports the catalyst. Disclosure of the invention
- the present invention has been made in view of the problems of the prior art, it is an object of tactile catalyst such as New Omicron chi storage catalyst can maintain passes connection its activity long term
- An object of the present invention is to provide a silicon carbide-based catalyst as a medium and a method for producing the same.
- a large number of silicon carbide particles as an aggregate are constituted by a first connecting structure formed by binding to each other while maintaining a large number of pores.
- a silicon carbide-based catalyst body in which a catalyst containing an alkali metal and / or an alkaline earth metal is supported on a porous body having a predetermined shape, wherein the catalyst forms the first connective tissue.
- a silicon carbide catalyst is provided, which is supported via a crystalline film made of an oxide formed on at least a part of the surface of the particle.
- a plurality of silicon carbide particles as an aggregate and metallic silicon as a binder are formed by bonding while holding a number of pores.
- a silicon carbide-based catalyst in which a catalyst containing an alkali metal and / or an alkaline earth metal is supported on a porous body having a predetermined shape, which is composed of a connective structure of No. 2;
- the carbonization material is supported via a crystalline film made of an oxide coated on at least a part of the surface of the silicon carbide particles forming the second connective structure and / or the metal silicon.
- a siliconaceous catalyst body is provided.
- the crystalline coating rather preferably be one containing S i 0 2
- further crystalline film is preferably made of cristobalite and / or mullite.
- the predetermined shape is preferably a honeycomb shape.
- a raw material mixture containing silicon carbide particles and metallic silicon is formed into a predetermined shape, and the obtained molded body is calcined and main-baked, and after being heat-treated in an oxygen-containing atmosphere, an alkali metal and A second connective tissue formed by supporting a catalyst containing Z or an alkaline earth metal, and bonding a large number of the silicon carbide particles and metallic silicon while holding a large number of pores.
- the catalyst is a crystalline body composed of an oxide coated and formed on at least a part of the surface of the silicon carbide particles and Z or the metal silicon forming the second connective tissue.
- the temperature of the heat treatment is preferably 800 to 140 ° C.
- the predetermined shape is preferably an 82-cam shape.
- FIG. 1 is an electron micrograph showing the microstructure of the silicon carbide-based catalyst of Example 1 before supporting the catalyst.
- FIG. 2 is an electron micrograph showing the microstructure of the silicon carbide-based catalyst of Comparative Example 1 before supporting the catalyst.
- the present inventors have found that when a porous honeycomb structure containing silicon carbide and metallic silicon carries a catalyst such as lithium (K), the catalytic ability is likely to be deactivated.
- a catalyst such as lithium (K)
- there porous body amorphous silica formed during the sintering and heating of the catalyst (S i 0 2) phases have found that it is liable to be absorbed 'spread. That is, it is considered that the catalyst life can be extended by modifying the amorphous silica (Si 2 ) phase, and the present invention has been achieved.
- Si 2 amorphous silica
- the first embodiment of the present invention comprises a first connecting structure formed by bonding a large number of silicon carbide particles as aggregates to each other while holding a large number of pores,
- a silicon carbide-based catalyst in which a catalyst containing an alkali metal and / or an alkaline earth metal is supported on a porous body having a predetermined shape, wherein the catalyst is formed of silicon carbide particles forming a first bonded structure. It is characterized in that it is supported via a crystalline film made of an oxide coated on at least a part of the surface. The details will be described below.
- the silicon carbide-based catalyst of the present embodiment includes a large number of silicon carbide particles as an aggregate, and bonds to each other while holding a large number of pores to form a first connected structure. Therefore, it reflects the properties of silicon carbide as a constituent material, and has excellent properties such as oxidation resistance and heat resistance.
- the silicon carbide-based catalyst of the present embodiment has at least a part of the surface of silicon carbide particles forming the first connective tissue constituting the catalyst body, that is,
- At least a part of the surface in contact with the catalyst containing Z or the alkaline earth metal is covered with a crystalline film made of an oxide.
- the crystalline film made of this oxide is a film formed in place of the amorphous silica (Si 2 ) phase formed on the surface of the conventional silicon carbide porous silicon carbide particles.
- the supported catalyst is difficult to be absorbed and diffused, and This has the effect of extending the service life.
- the second embodiment of the present invention relates to a second bonding formed by bonding a large number of silicon carbide particles as an aggregate and metallic silicon as a binder while holding a large number of pores.
- a silicon carbide-based catalyst in which a catalyst containing an alkali metal and Z or an alkaline earth metal is supported on a porous body having a predetermined shape, the catalyst comprising a second connecting tissue Characterized by being supported via a crystalline film made of an oxide coated on at least a part of the surface of silicon carbide particles and / or metallic silicon forming the silicon carbide particles.
- the silicon carbide-based catalyst of the present embodiment contains silicon carbide particles as an aggregate and metallic silicon as a binder, and binds while holding a large number of pores to form a second connected tissue. are doing. Therefore, sintering can be performed at a relatively low firing temperature during manufacturing, which reduces manufacturing costs and improves manufacturing yield.
- metal silicon is used for bonding silicon carbide particles, which are refractory particles, they exhibit high thermal conductivity. Therefore, for example, when used for DPF, even if the particulates deposited for filter regeneration are burned, local temperature rise that would damage the filter is unlikely to occur, and excellent oxidation resistance and heat resistance It has characteristics such as sex. ,
- the silicon carbide-based catalyst body of the present embodiment has at least a portion of the surface of silicon carbide particles and / or metal silicon forming the second connective tissue constituting the catalyst body, At least a part of the surface in contact with the catalyst containing an alkaline earth metal is coated with a crystalline film made of an oxide.
- the oxide or Ranaru crystalline film is formed instead of the conventional porous body of silicon carbide particles and / or metallic silicon amorphous silica was formed on the surface of the silicon carbide (S i 0 2) Phase
- the silicon carbide-based catalyst body of the present embodiment supporting a catalyst containing Al-Li metal and Z or Al-earth metal via the crystalline film has the supported catalyst absorbed.
- “at least a part of the surface of silicon carbide particles” and “at least a part of the surface of silicon carbide particles and Z or metal silicon” refer to silicon carbide particles. And / or means that there may be a portion of the surface of the metallic silicon that is not covered by the crystalline film, but the catalyst contains a supported alkali metal and / or alkaline earth metal. It is particularly preferable that the entire surface of the silicon carbide particles and / or metallic silicon in contact with is covered with a crystalline film.
- the crystalline film made of an oxide according to the first and second embodiments of the present invention preferably contains a silicon (Si ⁇ ), and more specifically, Chris It is preferable that it is composed of tobarite and Z or muraite.
- a crystalline film composed of these materials is preferable because the catalyst can be stably supported for a longer period of time and can be easily formed by coating.
- the shape of the porous body is a honeycomb shape or a two-cam structure. That is, reflecting the characteristics of the silicon carbide porous body as a constituent material, it has excellent characteristics such as oxidation resistance and heat resistance, and can be used as a catalyst carrier under high SV (space velocity) conditions. .
- the type of the alkali metal and Z or the alkaline earth metal contained in the catalyst used in the present embodiment is, for example, K, Li, Na, Cs as the alkali metal, and C a as the alkaline earth metal. , Ba, Sr and the like.
- the catalyst in addition to N_ ⁇ x storage components such as alkali metals and alkaline earth metals, P t as a normal catalyst component, P d, may include a noble metal, such as R h.
- a general catalyst loading method for loading a catalyst on a honeycomb structure may be used.
- the method for producing the honeycomb structure silicon carbide-based catalyst
- the third embodiment of the present invention relates to a method for producing a silicon carbide-based catalyst body, comprising forming a raw material mixture containing silicon carbide particles and metal silicon into a predetermined shape, calcining the obtained molded body, and subjecting the formed body to a calcining process. After calcination and heat treatment in an oxygen-containing atmosphere, a large number of silicon carbide particles and a large number of pores are formed by a large number of silicon carbide particles and metallic silicon, carrying a catalyst containing Al-metal and Z or Al-earth metal.
- the catalyst is applied to the porous body composed of the second connective tissue formed by bonding while holding the surface of the silicon carbide particles and / or metallic silicon forming the second connective tissue.
- a catalyst body (silicon carbide-based catalyst body according to the second embodiment of the present invention) supported at least via a crystalline film made of an oxide that is partially coated and formed. is there.
- a raw material mixture containing silicon carbide particles and metallic silicon is prepared. If necessary, a molding aid such as an organic binder may be added to the raw material mixture.
- silicon carbide particles and metallic silicon may contain trace impurities such as Fe, A1, or Ca, they may be used as they are or subjected to chemical treatment such as chemical cleaning. A purified product may be used.
- the prepared raw material mixture is kneaded to obtain a forming clay.
- the obtained kneaded material is formed into a predetermined shape such as an 82 cam shape, and the obtained formed body is calcined to remove organic binders in the formed body (degreasing) to obtain a calcined body. .
- the calcination is preferably performed at a temperature lower than the temperature at which metallic silicon melts. Specifically, the temperature may be once held at a predetermined temperature of about 150 to 700 ° C., and the rate of temperature rise may be reduced to 50 ° C./hr or less in the predetermined temperature range, and then calcined. May be. Regarding the method of once holding at a predetermined temperature, depending on the type and amount of the organic binder used, holding at only one temperature level or holding at multiple temperature levels may be used.
- the holding times may be the same or different.
- the method of slowing down the heating rate may be slowed down only in one temperature zone or slowed down in multiple sections, and in multiple sections, even if the speeds are the same, they may be different. You may.
- This sintered body is composed of a large number of silicon carbide particles as an aggregate, which is a raw material, and metallic silicon as a binding material, in which pores are retained (second bonding structure).
- metallic silicon As a binding material, in which pores are retained (second bonding structure).
- the firing temperature in the final firing is preferably set to 140 ° C. or higher. Further, the optimal firing temperature is determined from the microstructure and characteristic values. However, if the temperature exceeds 160 O, evaporation of metal silicon proceeds, and it becomes difficult to bond through metal silicon. Therefore, a firing temperature of 140 to 160 ° C is appropriate.
- the temperature is preferably from 142 to 150 ° C.
- the fired body is heat-treated in an oxygen-containing atmosphere.
- an oxygen-containing atmosphere By performing this heat treatment, at least a part of the surface of the silicon carbide particles and Z or metallic silicon forming the second connective structure constituting the fired body is converted into a crystalline film made of an oxide, for example, Sio 2 3 ⁇ 4
- the coating can be coated with a coating, specifically, a coating composed of cristobalite and / or mullite, and a silicon carbide-based porous body serving as a catalyst carrier can be obtained.
- the temperature of the heat treatment performed in the above-described oxygen-containing atmosphere is preferably 800 to 140 ° C, and more preferably 110 to 135 ° C.
- the temperature is lower than 800 ° C, the degree of formation of crystals constituting the crystalline film is insufficient, and if the temperature is higher than 140 ° C, it approaches the melting point of metallic silicon and maintains a predetermined shape. It is not preferable because it may not be possible.
- a catalyst is supported on the porous body.
- the constituent material of the catalyst in order to carry the the NO x storage component and a noble metal, such as highly dispersed, ⁇ - it is preferable to use a large heat-resistant inorganic oxide of specific surface area, such as A 1 2 0 3 .
- a specific example of the method for supporting the catalyst will be described later.
- the SiC raw material powder having an average particle diameter of 47 ⁇ m and the Si powder having an average particle diameter of 5 / zm were blended so as to have a composition of 80:20 in terms of mass ratio. 6 parts by mass of an organic binder, 2.5 parts by mass of a surfactant, and 24 parts by mass of water were added to the parts by mass, and the mixture was uniformly mixed and kneaded to obtain a clay for molding.
- the obtained clay was extruded using an extruder to an outer diameter of 45 mm, a length of 120 mm, a partition wall thickness of 0.43 mm, and a cell density of 100 cells / square inch (16 cells / cm2). 2 ), and then calcined for 5 hours at 500 ° C for 5 hours, and then calcined for 2 hours at 1450 ° C in a non-oxidizing atmosphere. A fired body was produced.
- the fired body thus produced was heat-treated under the heat treatment conditions shown in Table 1 (however, Comparative Example 1 was not heat-treated) to produce a silicon carbide porous body (honeycomb structure) having an 82-cam structure.
- the state of coating of each porous body with the (crystalline) film was evaluated by observing with an electron microscope.
- Table 1 shows the results. The evaluation is based on the table of the carrier in contact with the catalyst. ⁇ indicates that the surface of silicon carbide (SiC) particles and metallic silicon (Si) constituting the surface is sufficiently covered, ⁇ indicates that the surface is covered to some extent (approximately 50%), and ⁇ ⁇ indicates that the surface is covered. If no, X is used.
- FIGS. 1 and 2 show electron micrographs showing the microstructure of the silicon carbide-based catalyst body of the working example and comparative example 1 before supporting the catalyst.
- 0 308/0 cells (1.06 g / L)) (per honeycomb volume, platinum (Pt) element-based mass), potassium (K) is 20 g / L (honeycomb volume per potassium (K) the Hare by the element-based mass) was adjusted at the stage of mixing immersion.
- a honeycomb structure serving as a catalyst carrier was immersed in the obtained slurry for wet coating, and excess liquid in the cell was blown off and dried.
- the amount of potassium (K) supported was adjusted to be 20 g / liter (L) (mass of potassium (K) per volume of catalyst support) after calcination. If there is a shortage of the desired loading amount after one immersion and drying In that case, the immersion and drying steps were repeated until reaching.
- the obtained potassium (K) carrier was calcined at 600 in an electric furnace for 1 hour to prepare a silicon carbide-based catalyst.
- the catalyst has the first connective tissue Because it is made are carried through the crystalline film ing an oxide which is at least partially coat forming the surface of the silicon carbide particles forming the, over a catalyst for a long time, such as the NO x storage catalyst It is a catalyst that can maintain its activity.
- the catalyst is a crystalline film formed of oxide coated on at least a part of the surface of silicon carbide particles and / or metal silicon forming the second connective tissue. Because it is made are carried through a catalyst capable of maintaining its activity catalyst such as N_ ⁇ x storage catalyst over a long period of time.
- the catalyst is formed on the surface of silicon carbide particles and / or metal silicon forming a predetermined connective tissue. It is possible to easily produce a catalyst body that is supported via a crystalline film made of an oxide that is at least partially coated.
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- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Ceramic Engineering (AREA)
- Structural Engineering (AREA)
- Environmental & Geological Engineering (AREA)
- Biomedical Technology (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Combustion & Propulsion (AREA)
- Manufacturing & Machinery (AREA)
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Abstract
Description
Claims
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
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EP03754135A EP1552882A4 (en) | 2002-10-18 | 2003-10-15 | CATALYTIC MATERIAL BASED ON SILICON CARBIDE AND PROCESS FOR PRODUCING THE SAME |
US10/531,048 US7253134B2 (en) | 2002-10-18 | 2003-10-15 | Silicon carbide-based catalytic body and process for producing the same |
AU2003273013A AU2003273013A1 (en) | 2002-10-18 | 2003-10-15 | Silicon carbide-based catalytic material and process for producing the same |
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JP2002303923A JP4404538B2 (ja) | 2002-10-18 | 2002-10-18 | 排ガス浄化用炭化珪素質触媒体及びその製造方法 |
JP2002-303923 | 2002-10-18 |
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PCT/JP2003/013189 WO2004035207A1 (ja) | 2002-10-18 | 2003-10-15 | 炭化珪素質触媒体及びその製造方法 |
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US (1) | US7253134B2 (ja) |
EP (1) | EP1552882A4 (ja) |
JP (1) | JP4404538B2 (ja) |
KR (1) | KR100739409B1 (ja) |
AU (1) | AU2003273013A1 (ja) |
PL (1) | PL215617B1 (ja) |
WO (1) | WO2004035207A1 (ja) |
Cited By (1)
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CN115124347A (zh) * | 2021-03-25 | 2022-09-30 | 日本碍子株式会社 | 碳化硅质多孔体、蜂窝结构体、电加热催化器及碳化硅质多孔体的制造方法 |
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JP4567285B2 (ja) * | 2002-11-22 | 2010-10-20 | 日本碍子株式会社 | 排ガス浄化用触媒体 |
FR2889080B1 (fr) * | 2005-07-28 | 2007-11-23 | Saint Gobain Ct Recherches | Support et filtre catalytique a base de carbure de silicium et a haute surface specifique |
FR2891472B1 (fr) * | 2005-09-30 | 2008-04-18 | Saint Gobain Ct Recherches | Methode d'obtention d'une structure de filtration homogene pour une application catalytique |
KR101383352B1 (ko) | 2007-10-10 | 2014-04-10 | 주식회사 칸세라 | 탄화규소질 다공체 제조용 조성물, 이를 이용한 탄화규소질다공체, 촉매 담체 및 분진 필터 |
BRPI0817413A2 (pt) * | 2007-12-21 | 2015-06-16 | Dow Global Technologies Inc | Catalisador de fuligem, filtro de fuligem catalisador e método para formar um filtro de fuligem catalisador |
JP4997090B2 (ja) | 2007-12-26 | 2012-08-08 | 日本碍子株式会社 | 多孔質焼成体及びその製造方法 |
JP5228788B2 (ja) * | 2008-10-21 | 2013-07-03 | 住友大阪セメント株式会社 | 金属触媒担持粒子とその製造方法及び金属触媒担持粒子分散液並びに触媒 |
DE102009052308B3 (de) * | 2009-11-09 | 2011-02-10 | Heraeus Quarzglas Gmbh & Co. Kg | Verfahren zur Herstellung eines Quarzglaszylinders sowie Träger zur Durchführung des Verfahrens |
JP6654085B2 (ja) * | 2016-03-31 | 2020-02-26 | 日本碍子株式会社 | 多孔質材料、及び多孔質材料の製造方法並びにハニカム構造体 |
US11428138B2 (en) | 2016-10-24 | 2022-08-30 | Ngk Insulators, Ltd. | Porous material, honeycomb structure, and method of producing porous material |
JP6996914B2 (ja) * | 2016-10-24 | 2022-01-17 | 日本碍子株式会社 | 多孔質材料、ハニカム構造体、及び多孔質材料の製造方法 |
JP7051524B2 (ja) * | 2018-03-26 | 2022-04-11 | 日本碍子株式会社 | 多孔質材料、セル構造体および多孔質材料の製造方法 |
JP7025969B2 (ja) * | 2018-03-26 | 2022-02-25 | 日本碍子株式会社 | 多孔質材料、セル構造体および多孔質材料の製造方法 |
JP6912412B2 (ja) * | 2018-03-30 | 2021-08-04 | 日本碍子株式会社 | 炭化珪素質多孔体及びその製造方法 |
JP7390272B2 (ja) | 2020-09-30 | 2023-12-01 | 日本碍子株式会社 | 焼成用セッター |
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- 2002-10-18 JP JP2002303923A patent/JP4404538B2/ja not_active Expired - Fee Related
-
2003
- 2003-10-15 WO PCT/JP2003/013189 patent/WO2004035207A1/ja active Application Filing
- 2003-10-15 KR KR1020057006690A patent/KR100739409B1/ko not_active IP Right Cessation
- 2003-10-15 EP EP03754135A patent/EP1552882A4/en not_active Withdrawn
- 2003-10-15 AU AU2003273013A patent/AU2003273013A1/en not_active Abandoned
- 2003-10-15 PL PL375547A patent/PL215617B1/pl unknown
- 2003-10-15 US US10/531,048 patent/US7253134B2/en not_active Expired - Lifetime
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Also Published As
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KR100739409B1 (ko) | 2007-07-18 |
PL215617B1 (pl) | 2014-01-31 |
PL375547A1 (en) | 2005-11-28 |
EP1552882A4 (en) | 2009-07-01 |
JP4404538B2 (ja) | 2010-01-27 |
EP1552882A1 (en) | 2005-07-13 |
US20060003889A1 (en) | 2006-01-05 |
AU2003273013A1 (en) | 2004-05-04 |
US7253134B2 (en) | 2007-08-07 |
KR20050065607A (ko) | 2005-06-29 |
JP2004136216A (ja) | 2004-05-13 |
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