WO2014014059A1 - Filtre en nid-d'abeilles - Google Patents

Filtre en nid-d'abeilles Download PDF

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Publication number
WO2014014059A1
WO2014014059A1 PCT/JP2013/069530 JP2013069530W WO2014014059A1 WO 2014014059 A1 WO2014014059 A1 WO 2014014059A1 JP 2013069530 W JP2013069530 W JP 2013069530W WO 2014014059 A1 WO2014014059 A1 WO 2014014059A1
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Prior art keywords
honeycomb filter
flow path
honeycomb
partition wall
powder
Prior art date
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Ceased
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PCT/JP2013/069530
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English (en)
Japanese (ja)
Inventor
康輔 魚江
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Sumitomo Chemical Co Ltd
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Sumitomo Chemical Co Ltd
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Publication date
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Priority to JP2014525864A priority Critical patent/JPWO2014014059A1/ja
Publication of WO2014014059A1 publication Critical patent/WO2014014059A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B01D46/24—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies
    • 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
    • B01D46/2451—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure
    • B01D46/247—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure of the cells
    • 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
    • C04B35/46—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 titanium oxides or titanates
    • C04B35/462—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 titanium oxides or titanates based on titanates
    • C04B35/478—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 titanium oxides or titanates based on titanates based on aluminium titanates
    • B—PERFORMING OPERATIONS; TRANSPORTING
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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
    • B01D53/9418—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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    • B01J29/723—CHA-type, e.g. Chabazite, LZ-218
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    • B01J37/346—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of microwave energy
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    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
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    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418—Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • 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
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6562—Heating rate
    • 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
    • F01N2330/00—Structure of catalyst support or particle filter
    • F01N2330/30—Honeycomb supports characterised by their structural details
    • F01N2330/34—Honeycomb supports characterised by their structural details with flow channels of polygonal cross section
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL-COMBUSTION ENGINES
    • F01N2510/00—Surface coverings
    • F01N2510/06—Surface coverings for exhaust purification, e.g. catalytic reaction
    • F01N2510/068—Surface coverings for exhaust purification, e.g. catalytic reaction characterised by the distribution of the catalytic coatings
    • F01N2510/0682—Surface coverings for exhaust purification, e.g. catalytic reaction characterised by the distribution of the catalytic coatings having a discontinuous, uneven or partially overlapping coating of catalytic material, e.g. higher amount of material upstream than downstream or vice versa
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
    • Y02T10/00—Road transport of goods or passengers
    • Y02T10/10—Internal combustion engine [ICE] based vehicles
    • Y02T10/12—Improving ICE efficiencies

Definitions

  • the present invention relates to a honeycomb filter.
  • the honeycomb filter is used to remove the collected matter from the fluid containing the collected matter.
  • the honeycomb filter collects fine particles such as carbon particles contained in exhaust gas discharged from an internal combustion engine such as a diesel engine. It is used as a ceramic filter (diesel particulate filter).
  • the honeycomb filter has a plurality of parallel flow paths partitioned by partition walls, and one end of a part of the plurality of flow paths and the other end of the remaining part of the plurality of flow paths are sealed. .
  • a honeycomb structure constituting such a honeycomb filter for example, structures described in Patent Documents 1 and 2 below are known.
  • the method of decomposing the NO X contained in the exhaust gas the method of decomposing the NO X by reaction such as the following formulas (2) to (4) are known from the ammonia.
  • This method is called SCR (Selective Catalytic Reduction) because NO x is selectively reduced by ammonia.
  • SCR Selective Catalytic Reduction
  • ammonia can be generated by hydrolyzing urea water at a high temperature.
  • a method of decomposing NO X in exhaust gas using ammonia generated from urea is called urea SCR.
  • a honeycomb structure was supported adsorbed easily zeolite ammonia is used. Further, as the zeolite, a metal ion exchanged zeolite ion-exchanged with a metal ion such as a copper ion is used in order to improve NO X reduction.
  • the honeycomb structure for SCR and the diesel particulate filter are arranged in series to construct an exhaust gas purification system.
  • the honeycomb filter having both the SCR function and the diesel particulate filter function has a problem that, when exposed to a high temperature, the metal ion exchange zeolite thermally decomposes the ceramics constituting the partition walls of the honeycomb filter. is there.
  • An object of the present invention is to provide a honeycomb filter having both an SCR function and a diesel particulate filter function that can suppress thermal decomposition of ceramics constituting the partition wall.
  • the present invention provides a honeycomb filter including partition walls that form a plurality of flow paths parallel to each other, wherein the honeycomb filter includes a first end surface and a side opposite to the first end surface. A plurality of first flow paths whose end portions on the second end face side are sealed, and ends on the first end face side.
  • the catalyst layer is selected from the group consisting of titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, rhodium, palladium, silver, and platinum.
  • Including at least one metal element and zeolite Serial septum, magnesium, calcium, strontium, yttrium, barium, aluminum titanate-based ceramics containing at least one element selected from the group consisting of lanthanoid, and bismuth, provides a honeycomb filter.
  • the partition wall is made of an aluminum titanate-based ceramic containing at least one element selected from the group consisting of magnesium, calcium, strontium, yttrium, barium, lanthanoid and bismuth. Thermal decomposition of the aluminum-based ceramics can be suppressed.
  • the honeycomb filter includes first and second flow paths whose opposite end faces are sealed, and a partition wall surface in the first flow path, a partition wall surface in the second flow path, and Since the catalyst layer (SCR catalyst layer) is formed in at least one of the pores in the partition wall, both the diesel particulate filter function and the SCR function are provided.
  • SCR catalyst layer catalyst layer
  • the partition wall preferably further contains silicon dioxide.
  • the partition walls of the honeycomb filter can contain silicon dioxide.
  • the silicon dioxide acts as a sintering aid when the honeycomb filter is fired, and is present at the interface between the aluminum titanate-based crystals.
  • the mechanical strength of the glass can be increased, and a glass phase is formed in the partition walls. This glass phase not only increases the strength of the partition walls by bonding the crystals, but also the metal element in the catalyst layer that comes into contact with the partition walls and the metal element contained in the ash remaining after the soot combustion is aluminum titanate. It has the effect of suppressing movement into the system crystal.
  • honeycomb filter having both the SCR function and the diesel particulate filter function that can suppress the thermal decomposition of ceramics constituting the partition wall.
  • FIG. 2 (a) is an enlarged view of the end face on the opposite side of Fig. 1 (b) in the honeycomb filter shown in Fig. 1
  • Fig. 2 (b) is an enlarged view of a partition wall cross section.
  • FIG. 3 is a view taken along arrow III-III in FIG. It is a figure which shows typically the honey-comb filter which concerns on 2nd Embodiment of this invention.
  • Fig.5 (a) is an enlarged view of the end surface on the opposite side to FIG.4 (b) in the honey-comb filter shown in FIG. 4,
  • FIG.5 (b) is an enlarged view of a partition cross section.
  • FIG. 5 (a) is an enlarged view of the end surface on the opposite side to FIG.4 (b) in the honey-comb filter shown in FIG. 4
  • FIG. 6 is a view taken along the line VI-VI in FIG. It is the schematic of the exhaust gas purification system provided with the honey-comb filter of this invention.
  • FIG. 8A is a scanning electron microscope (SEM) photograph of the partition wall cross section after the heat treatment of the honeycomb fired body obtained in Experimental Example 1, and FIG. 8B is a region R3 in FIG. 8A.
  • FIG. 8C is an enlarged photograph, and FIG. 8C is an enlarged photograph of the region R4 in FIG. 8B.
  • FIG. 9A is an EDX element mapping image of Al in the region R4, and FIG. 9B is an EDX element mapping image of Ti in the region R4.
  • FIG. 9A is an EDX element mapping image of Al in the region R4
  • FIG. 9B is an EDX element mapping image of Ti in the region R4.
  • FIG. 10 (a) is a scanning electron microscope (SEM) photograph of the cross section of the partition wall after the heat treatment of the honeycomb fired body obtained in Experimental Example 2
  • FIG. 10 (b) is a region R5 in FIG. 10 (a).
  • FIG. 11A is an EDX element mapping image of Al in the region R5
  • FIG. 11B is an EDX element mapping image of Ti in the region R5.
  • FIG. 12A is a scanning electron microscope (SEM) photograph of a cross section of the partition wall of the catalyst layer-supporting honeycomb filter A obtained in Example 1
  • FIG. 12B is an enlarged view of a region R6 in FIG. It is a photograph.
  • 2 is a scanning electron microscope (SEM) photograph of a partition wall cross section of a catalyst layer-supporting honeycomb filter B obtained in Example 1.
  • Fig. 1 is a diagram schematically showing a honeycomb filter according to the first embodiment.
  • Fig. 1 (a) is a perspective view and an enlarged view of an end face of the honeycomb filter
  • Fig. 1 (b) is a diagram of Fig. 1 (b). It is an enlarged view of area
  • Fig. 2 (a) is an enlarged view of the end face on the opposite side of Fig. 1 (b) in the honeycomb filter shown in Fig. 1, and Fig. 2 (b) is an enlarged view of a partition wall cross section.
  • FIG. 3 is a view taken in the direction of arrows III-III in FIG.
  • the honeycomb filter 100 has one end face (first end face) 100a and the other end face (second end face) 100b located on the opposite side of the end face 100a.
  • the honeycomb filter 100 is a cylindrical body having a plurality of flow paths 110 extending in parallel to each other.
  • the plurality of flow paths 110 are partitioned by partition walls 120 extending in parallel to the central axis of the honeycomb filter 100.
  • the plurality of channels 110 have a plurality of channels (first channels) 110a and a plurality of channels (second channels) 110b adjacent to the channels 110a.
  • the flow path 110a and the flow path 110b extend from the end face 100a to the end face 100b perpendicular to the end faces 100a and 100b.
  • One end of the flow path 110a constituting a part of the flow path 110 is opened at the end face 100a, and the other end of the flow path 110a is sealed by the sealing portion 130 at the end face 100b.
  • One end of the flow path 110b constituting the remaining part of the plurality of flow paths 110 is sealed by the sealing portion 130 at the end face 100a, and the other end of the flow path 110b is opened at the end face 100b.
  • an end portion on the end surface 100a side of the flow path 110a is opened as a gas inlet
  • an end portion on the end face 100b side of the flow path 110b is opened as a gas outlet.
  • the cross section perpendicular to the axial direction of the flow path 110a and the flow path 110b has a hexagonal shape.
  • the cross section of the flow path 110b is, for example, a regular hexagonal shape in which the lengths of the sides 140 forming the cross section are substantially equal to each other, but may be a flat hexagonal shape.
  • the cross section of the flow path 110a has, for example, a flat hexagonal shape, but may have a regular hexagonal shape.
  • the lengths of the sides facing each other in the cross section of the channel 110a are substantially equal to each other.
  • the cross section of the flow path 110a includes two long sides 150a having substantially the same length as the sides 150 forming the cross section, and four (two pairs) short sides 150b having substantially the same length. ,have.
  • the short side 150b is disposed on each side of the long side 150a.
  • the long sides 150a face each other in parallel, and the short sides 150b face each other in parallel.
  • the partition 120 has the partition 120a as a part which partitions off the flow path 110a and the flow path 110b. That is, the channel 110a and the channel 110b are adjacent to each other through the partition wall 120a. By arranging one channel 110a between adjacent channels 110b, the channels 110b are alternately arranged with the channels 110a in the arrangement direction of the channels 110b (a direction substantially orthogonal to the side 140). ing.
  • Each of the sides 140 of the flow channel 110b faces the long side 150a of any one of the plurality of flow channels 110a in parallel. That is, each of the wall surfaces forming the flow channel 110b faces the one wall surface forming the flow channel 110a in parallel in the partition wall 120a located between the flow channel 110a and the flow channel 110b.
  • the flow path 110 has a structural unit including one flow path 110b and six flow paths 110a surrounding the flow path 110b. In the structural unit, all the sides 140 of the flow path 110b are included. Opposite the long side 150a of the channel 110a.
  • at least one length of the side 140 of the flow path 110b may be substantially equal to the length of the opposed long side 150a, and each length of the side 140 is equal to the length of the opposed long side 150a. It may be substantially equal.
  • the partition wall 120 has a partition wall 120b as a part for partitioning the adjacent flow paths 110a. That is, the flow paths 110a surrounding the flow path 110b are adjacent to each other via the partition wall 120b.
  • Each of the short side 150b of the flow path 110a is facing in parallel with the short side 150b of the adjacent flow path 110a. That is, the wall surfaces forming the flow paths 110a face each other in parallel in the partition wall 120b located between the adjacent flow paths 110a.
  • at least one length of the short side 150b of the flow path 110a between the adjacent flow paths 110a may be substantially equal to the length of the opposing short side 150b. The length may be substantially equal to the length of the opposing short side 150b.
  • a catalyst layer 160 is formed on the surfaces of the partition walls 120a and 120b in the flow channel 110a, the surfaces of the partition walls 120a and 120b in the flow channel 110b, and inside the pores (inside the communication holes) of the partition walls 120a and 120b.
  • the catalyst layer 160 is formed on at least one of the surfaces of the partition walls 120a and 120b in the channel 110a, the surfaces of the partition walls 120a and 120b in the channel 110b, and the pores of the partition walls 120a and 120b.
  • it is preferably formed in all of the above-mentioned locations.
  • Fig. 4 is a diagram schematically showing the honeycomb filter according to the second embodiment.
  • Fig. 4 (a) is a perspective view and an enlarged view of the end face of the honeycomb filter
  • Fig. 4 (b) is a diagram of Fig. 4 (b). It is an enlarged view of area
  • Fig.5 (a) is an enlarged view of the end surface on the opposite side to FIG.4 (b) in the honey-comb filter shown in FIG. 4,
  • FIG.5 (b) is an enlarged view of a partition cross section. 6 is a view taken in the direction of arrows VI-VI in FIG.
  • the honeycomb filter 200 has one end face (first end face) 200a and the other end face (second end face) 200b located on the opposite side of the end face 200a.
  • the honeycomb filter 200 is a cylindrical body having a plurality of flow paths 210 extending in parallel to each other.
  • the plurality of flow paths 210 are partitioned by partition walls 220 extending in parallel with the central axis of the honeycomb filter 200.
  • the plurality of flow paths 210 include a plurality of flow paths (first flow paths) 210a and a plurality of flow paths (second flow paths) 210b adjacent to the flow paths 210a.
  • the channel 210a and the channel 210b extend from the end surface 200a to the end surface 200b perpendicular to the end surfaces 200a and 200b.
  • One end of the flow path 210a forming a part of the flow path 210 is open at the end face 200a, and the other end of the flow path 210a is sealed by the sealing portion 230 at the end face 200b.
  • One end of the flow path 210b forming the remaining part of the plurality of flow paths 210 is sealed by the sealing portion 230 at the end face 200a, and the other end of the flow path 210b is opened at the end face 200b.
  • an end portion on the end surface 200a side of the flow path 210a is opened as a gas inlet
  • an end portion of the flow path 210b on the end surface 200b side is opened as a gas outlet.
  • the cross section perpendicular to the axial direction of the flow path 210a and the flow path 210b has a hexagonal shape.
  • the cross section of the flow path 210b is, for example, a regular hexagonal shape in which the lengths of the sides 240 forming the cross section are substantially equal to each other, but may be a flat hexagonal shape.
  • the cross section of the flow path 210a is, for example, a flat hexagonal shape, but may be a regular hexagonal shape.
  • the lengths of the sides facing each other in the cross section of the flow path 210a are different from each other.
  • the cross section of the channel 210a has three long sides 250a having substantially the same length and three short sides 250b having substantially the same length as the sides 250 forming the cross section.
  • the long side 250a and the short side 250b face each other in parallel, and the short side 250b is disposed on each side of the long side 250a.
  • the partition 220 has the partition 220a as a part which partitions off the flow path 210a and the flow path 210b. That is, the flow path 210a and the flow path 210b are adjacent to each other through the partition wall 220a. Between the adjacent flow paths 210b, two flow paths 210a adjacent to each other in a direction substantially orthogonal to the arrangement direction of the flow paths 210b are arranged, and the two adjacent flow paths 210a are adjacent to each other. They are arranged symmetrically across a line connecting the centers of the cross sections of the paths 210b.
  • Each of the sides 240 of the flow path 210b faces the long side 250a of any one of the plurality of flow paths 210a in parallel. That is, each of the wall surfaces forming the flow path 210b faces the one wall surface forming the flow path 210a in parallel in the partition wall 220a positioned between the flow path 210a and the flow path 210b.
  • the flow path 210 includes a structural unit including one flow path 210b and six flow paths 210a surrounding the flow path 210b. In the structural unit, all the sides 240 of the flow path 210b are included. It faces the long side 250a of the flow path 210a.
  • each vertex of the cross section of the flow path 210b is opposed to the apex of the adjacent flow path 210b in the arrangement direction of the flow paths 210b.
  • at least one length of the side 240 of the flow path 210b may be substantially equal to the length of the opposed long side 250a, and each length of the side 240 is equal to the length of the opposed long side 250a. It may be substantially equal.
  • the partition 220 has the partition 220b as a part which partitions off the mutually adjacent flow paths 210a. That is, the flow paths 210a surrounding the flow path 210b are adjacent to each other through the partition 220b.
  • Each of the short side 250b of the flow path 210a is facing in parallel with the short side 250b of the adjacent flow path 210a.
  • the wall surfaces forming the flow path 210a face each other in parallel in the partition 220b located between the adjacent flow paths 210a.
  • One flow path 210a is surrounded by three flow paths 210b.
  • at least one length of the short side 250b of the flow path 210a may be substantially equal to the length of the opposing short side 250b.
  • the length may be substantially equal to the length of the opposing short side 250b.
  • a catalyst layer 260 is formed on the surfaces of the partition walls 220a and 220b in the flow path 210a, the surfaces of the partition walls 220a and 220b in the flow path 210b, and inside the pores (inside the communication holes) of the partition walls 220a and 220b.
  • the catalyst layer 260 is formed on at least one of the surfaces of the partition walls 220a and 220b in the channel 210a, the surfaces of the partition walls 220a and 220b in the channel 210b, and the pores of the partition walls 220a and 220b.
  • it is preferably formed at all of the above-described locations.
  • the length of the honeycomb filters 100 and 200 in the axial direction of the flow path is, for example, 50 to 300 mm.
  • the outer diameter of the honeycomb filters 100 and 200 is, for example, 50 to 250 mm.
  • the length of the side 140 is, for example, 0.4 to 2.0 mm.
  • the length of the long side 150a is, for example, 0.4 to 2.0 mm, and the length of the short side 150b is, for example, 0.3 to 2.0 mm.
  • the length of the side 240 is, for example, 0.4 to 2.0 mm.
  • the length of the long side 250a is, for example, 0.4 to 2.0 mm
  • the length of the short side 250b is, for example, 0.3 to 2.0 mm.
  • the thickness of the partition walls 120 and 220 is, for example, 0.1 to 0.8 mm.
  • the cell density in the honeycomb filters 100 and 200 is preferably 50 to 600 cpsi (cells per square inch), and more preferably 100 to 500 cpsi. preferable.
  • the sum total of the opening area of the some flow path 110a in the end surface 100a is larger than the sum total of the opening area of the flow path 110b in the end surface 100b.
  • the sum total of the opening area of the some flow path 210a in the end surface 200a is larger than the sum total of the opening area of the flow path 210b in the end surface 200b.
  • the hydraulic diameter of the flow paths 110a and 210a on the end faces 100a and 200a is preferably 1.4 mm or less.
  • the hydraulic diameters of the flow paths 110a and 210a are preferably 0.5 mm or more, and more preferably 0.7 mm or more, from the viewpoint of further suppressing accumulation of collected substances in the region on the end face side in the flow path.
  • the hydraulic diameter of the flow paths 110b and 210b on the end faces 100b and 200b is preferably larger than the hydraulic diameter of the flow paths 110a and 210a on the end faces 100a and 200a.
  • the hydraulic diameter of the flow paths 110b and 210b at the end faces 100b and 200b is preferably 1.7 mm or less, and more preferably 1.6 mm or less.
  • the hydraulic diameter of the channels 110b and 210b is preferably 0.5 mm or more, and more preferably 0.7 mm or more, from the viewpoint of reducing the pressure loss of exhaust gas ventilation.
  • the shape of the honeycomb filter is such that the cross section of the first channel perpendicular to the axial direction of the first channel (channels 110a and 210a) is the first side as in the honeycomb filters 100 and 200 described above. (Long sides 150a, 250a) and second sides (short sides 150b, 250b) respectively disposed on both sides of the first side, and a second channel (channels 110b, 210b). ) Each of the sides (sides 140 and 240) forming a cross section of the second flow path perpendicular to the axial direction of the first flow path are opposed to the first side of the first flow path. Each of the second sides may be in a form facing the second side of the adjacent first flow path, but is not necessarily limited to the shape described above.
  • the cross section of the channel perpendicular to the axial direction of the channel in the honeycomb filter is not limited to the hexagonal shape, and may be a triangular shape, a rectangular shape, an octagonal shape, a circular shape, an elliptical shape, or the like. .
  • those having different diameters may be mixed, or those having different cross-sectional shapes may be mixed.
  • the arrangement of the flow paths is not particularly limited, and the arrangement of the central axes of the flow paths may be an equilateral triangle arrangement, a staggered arrangement, or the like arranged at the apex of the equilateral triangle.
  • the honeycomb filter is not limited to a cylindrical body, and may be an elliptical column, a triangular column, a quadrangular column, a hexagonal column, an octagonal column, or the like.
  • the partition walls are porous, and include, for example, a porous ceramic sintered body.
  • the partition has a structure that allows fluid to pass therethrough. Specifically, a large number of communication holes (flow channels) through which fluid can pass are formed in the partition wall.
  • the porosity of the partition walls is preferably 20% by volume or more and more preferably 30% by volume or more from the viewpoint of improving the collection efficiency of the honeycomb filter and realizing a lower pressure loss.
  • the porosity of the partition walls is preferably 70% by volume or less, and more preferably 60% by volume or less.
  • the average pore diameter of the partition walls is preferably 5 ⁇ m or more, more preferably 10 ⁇ m or more, from the viewpoint of improving the collection efficiency of the honeycomb filter and realizing a lower pressure loss.
  • the average pore diameter of the partition walls is preferably 35 ⁇ m or less, and more preferably 30 ⁇ m or less.
  • the porosity and average pore diameter of the partition walls can be adjusted by the particle diameter of the raw material, the amount of pore former added, the kind of pore former, and the firing conditions, and can be measured by mercury porosimetry.
  • the partition includes an aluminum titanate ceramic containing at least one element selected from the group consisting of magnesium, calcium, strontium, yttrium, barium, lanthanoid and bismuth.
  • the aluminum titanate-based ceramics preferably contains at least one element selected from the group consisting of magnesium, calcium, strontium, barium and lanthanum from the viewpoint of sufficiently suppressing thermal decomposition by metal ion exchange zeolite. It is particularly preferable to contain magnesium.
  • the partition wall supporting the metal ion exchanged zeolite When the partition wall supporting the metal ion exchanged zeolite is exposed to high temperature, the metal in the zeolite promotes the movement of aluminum atoms and titanium atoms in the aluminum titanate ceramics and causes thermal decomposition.
  • magnesium magnesium titanate since magnesia exists in the lattice position of the crystal structure, the movement of aluminum atoms and titanium atoms can be inhibited, and thermal decomposition can be suppressed. Similarly, when the specific element other than magnesium is included, the movement of aluminum atoms and titanium atoms can be similarly inhibited to suppress thermal decomposition.
  • the oxide content of at least one element selected from the group consisting of magnesium, calcium, strontium, yttrium, barium, lanthanoid and bismuth in the partition wall is Al 2 O 3 in which aluminum and titanium are converted into oxides.
  • the total amount of TiO 2 is preferably 0.1 to 20 parts by mass, more preferably 1.0 to 15 parts by mass, and 4.0 to 10 parts by mass with respect to 100 parts by mass of the total amount of TiO 2. Particularly preferred.
  • the content of the specific element is equal to or higher than the lower limit, the thermal decomposition of the aluminum titanate-based ceramics tends to be more sufficiently suppressed, and when the content is lower than the upper limit, the mechanical strength is sufficiently increased. There is a tendency to be able to keep.
  • the molar ratio (aluminum: titanium) of aluminum converted to Al 2 O 3 and titanium converted to TiO 2 is preferably 35:65 to 45:55, and 40:60 to 45: 55 is more preferred.
  • the partition wall contains aluminum magnesium titanate
  • the composition formula of aluminum magnesium titanate is, for example, Al 2 (1-x) Mg x Ti (1 + x) O 5 , and the value of x is preferably 0.03 or more. 0.03-0.20 is more preferable, and 0.03-0.18 is still more preferable.
  • the partition wall containing the aluminum titanate-based ceramics is formed of, for example, porous ceramics mainly made of aluminum titanate-based crystals.
  • “Mainly composed of an aluminum titanate crystal” means that the main crystal phase constituting the ceramic fired body is an aluminum titanate crystal phase.
  • the aluminum titanate-based crystal phase contains at least one element selected from the group consisting of magnesium, calcium, strontium, yttrium, barium, lanthanoid and bismuth.
  • the partition containing the aluminum titanate ceramic may contain a glass phase derived from silicon source powder.
  • the glass phase refers to an amorphous phase in which SiO 2 (silicon dioxide) is a main component.
  • the partition containing an aluminum titanate ceramic may contain crystal phases other than an aluminum titanate crystal phase and a glass phase. Examples of such a crystal phase include a phase derived from a raw material used for producing a ceramic fired body.
  • the phase derived from the raw material is, for example, a phase derived from an aluminum source powder, a titanium source powder, a magnesium source powder, or the like remaining without forming an aluminum titanate-based crystal phase during the manufacture of the honeycomb filter, such as alumina, titania, magnesia. And the like.
  • the crystal phase forming the partition can be confirmed by an X-ray diffraction spectrum.
  • the content is preferably 0.5 to 30% by mass, more preferably 1.0 to 25% by mass, based on the total amount of the partition, 2.0 to It is especially preferable that it is 20 mass%.
  • the content of SiO 2 equal to or more than the above lower limit value, the mechanical strength after sintering can be increased compared to the case where the content is less than the above lower limit value, and the sintered honeycomb tends not to collapse.
  • the thermal expansion coefficient of the sintered honeycomb tends to be smaller than when the upper limit value is exceeded.
  • the catalyst layer is a layer mainly composed of porous zeolite, and is further selected from the group consisting of titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, rhodium, palladium, silver and platinum. It is a layer containing a kind of metal element. Since the zeolite is a metal ion-exchanged zeolite ion-exchanged with the ions of the above metal elements, the NO X reducing property is improved. In the metal ion exchanged zeolite, cations such as sodium ions contained in the zeolite are replaced with other metal ions.
  • the metal element is preferably at least one selected from the group consisting of copper, iron, vanadium, cobalt, nickel and silver, and particularly preferably copper.
  • the types of zeolite include ZSM-5, ⁇ zeolite, mordenite, ferrierite, chabazite, A-type zeolite, X-type zeolite, Y-type zeolite, and MCM-22.
  • zeolite is preferably one containing a ZSM-5 or chabazite since it is excellent in the NO X reducing.
  • the catalyst layer has a structure that allows fluid to permeate. Specifically, a large number of communication holes (flow paths) through which fluid can pass are formed in the catalyst layer.
  • the catalyst layer is provided so as not to block the communication hole (flow path) of the partition wall so that the fluid can pass through both the catalyst layer and the partition wall.
  • the porosity of the catalyst layer is preferably 20% by volume or more, and more preferably 30% by volume or more.
  • the porosity of the catalyst layer is preferably 70% by volume or less, and more preferably 60% by volume or less, from the viewpoint of obtaining an excellent ammonia adsorption amount and NO X reduction ability.
  • the average pore diameter of the catalyst layer is preferably 5 ⁇ m or more, and more preferably 8 ⁇ m or more from the viewpoint of not impairing the function of the honeycomb filter as a diesel particulate filter.
  • the average pore diameter of the catalyst layer is preferably 30 ⁇ m or less, and more preferably 25 ⁇ m or less, from the viewpoint of obtaining excellent NO X reducing ability.
  • the porosity and average pore diameter of the catalyst layer can be adjusted by the type of zeolite used and the granulation of the zeolite powder, and can be measured by mercury porosimetry.
  • the content of at least one metal element selected from the group consisting of titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, rhodium, palladium, silver, and platinum in the catalyst layer is the aluminum titanate ceramics. while suppressing the thermal decomposition, from the viewpoint of obtaining excellent NO X reducing ability is preferably from 0.01 to 1.0 mass% of the catalyst layer based on the total amount of 0.05 to 0.5 mass% It is more preferable.
  • the molar ratio of silica (SiO 2 ) and alumina (Al 2 O 3 ) of zeolite in the catalyst layer has excellent NO X reduction ability while suppressing thermal decomposition of the aluminum titanate ceramics. From the viewpoint of obtaining, it is preferably 10 to 10,000, and more preferably 20 to 5,000.
  • the honeycomb filter 100, 200 for example, a diesel engine, as well as collecting the trapped material such as soot contained in exhaust gas from an internal combustion engine such as a gasoline engine, for purifying NO X in the exhaust gas, the exhaust gas purification filter Suitable as
  • the honeycomb filter 100 as shown in FIG. 3, the gas G supplied from the end face 100a to the flow path 110a passes through the communication holes in the catalyst layer 160 and the partition wall 120 and reaches the adjacent flow path 110b. And is discharged from the end face 100b.
  • NO X in the gas G is reduced by the catalyst layer 160 and decomposed into N 2 and H 2 O, and the trapped material is collected on the surface of the partition wall 120 and / or in the communication hole.
  • the honeycomb filter 100 functions as an exhaust gas purification filter.
  • the honeycomb filter 200 functions as an exhaust gas purification filter.
  • FIG. 7 is a schematic view showing an embodiment of an exhaust gas purification system.
  • the exhaust gas purification system of the present embodiment includes the honeycomb filter 100 described above.
  • the exhaust gas purification system may include a honeycomb filter 200 instead of the honeycomb filter 100.
  • the gas G discharged from the internal combustion engine 500 such as a diesel engine or a gasoline engine is first supplied to an oxidation catalyst (DOC: Diesel Oxidation Catalyst) 510.
  • DOC Diesel Oxidation Catalyst
  • a noble metal catalyst such as platinum or palladium is used. These noble metal catalysts are used, for example, supported on a honeycomb structure.
  • the oxidation catalyst 510 removes hydrocarbons, carbon monoxide and the like contained in the gas G. Further, the oxidation catalyst 510, also occurs conversion to NO 2 in the NO. Since NO 2 functions as a strong oxidant, soot can be oxidized (combusted) efficiently due to the presence of NO 2 when soot accumulated in the subsequent honeycomb filter 100 is combusted.
  • the gas G is supplied to the honeycomb filter 100, and removal of trapped substances such as soot and NO X purification are performed.
  • Ammonia as a reducing agent for purifying NO X is produced by ejecting from the urea water supply device 520 urea water U in the gas G.
  • NO X in the gas G is decomposed into N 2 and H 2 O.
  • the exhaust gas purification system may further include an oxidation catalyst (DOC) at the subsequent stage of the honeycomb filter 100.
  • DOC oxidation catalyst
  • the oxidation catalyst provided in the subsequent stage of the honeycomb filter 100 is effective for removing the remaining ammonia.
  • a method for manufacturing a honeycomb filter includes, for example, a raw material preparation step for preparing a raw material mixture containing an inorganic compound powder and an additive, a forming step for forming a raw material mixture to obtain a formed body having a flow path, and firing the formed body.
  • a firing step, and a sealing step of sealing one end of each flow path between the molding step and the firing step, or after the firing step, and a step of forming a catalyst layer after the firing step and the sealing step, Is further provided.
  • each step will be described.
  • the inorganic compound powder includes, for example, an aluminum source powder such as ⁇ -alumina powder, a titanium source powder such as anatase type or rutile type titania powder (titanium source powder), and magnesium, calcium, strontium, yttrium, barium, lanthanoid and A raw material powder of at least one element selected from the group consisting of bismuth is included, and a silicon source powder such as silicon oxide powder and glass frit can be further included as necessary.
  • the magnesium source powder include magnesia powder and magnesia spinel powder.
  • Examples of the calcium source powder include calcia powder, calcium carbonate powder, anorthite, and the like.
  • Examples of the strontium source powder include strontium oxide powder and strontium carbonate powder.
  • Examples of the yttrium source powder include yttrium oxide powder.
  • Examples of the barium source powder include barium oxide powder, barium carbonate powder, and feldspar.
  • Examples of the bismuth source powder include bismuth oxide powder.
  • Each raw material powder may be one type or two or more types. Each raw material powder may contain a trace component derived from the raw material or inevitably contained in the production process.
  • a volume-based cumulative particle size equivalent to 50% (center particle size, D50) measured by a laser diffraction method is preferably in the following range.
  • D50 of the aluminum source powder is, for example, 20 to 60 ⁇ m.
  • D50 of the titanium source powder is, for example, 0.1 to 25 ⁇ m.
  • the D50 of the magnesium source powder is, for example, 0.5 to 30 ⁇ m.
  • D50 of the silicon source powder is, for example, 0.5 to 30 ⁇ m.
  • the raw material mixture may contain aluminum titanate and / or aluminum magnesium titanate.
  • the aluminum magnesium titanate corresponds to a raw material mixture having an aluminum source, a titanium source, and a magnesium source.
  • additives examples include a pore-forming agent (pore-forming agent), a binder, a plasticizer, a dispersant, and a solvent.
  • the pore-forming agent one formed by a material that disappears at a temperature lower than the temperature at which the molded body is degreased or fired in the firing process can be used.
  • the pore forming agent disappears due to combustion or the like.
  • a space is created at the location where the pore-forming agent was present, and the communication hole through which the fluid can flow is formed in the partition wall by shrinking the inorganic compound powder located between the spaces during firing. Can be formed.
  • the pore-forming agent is, for example, corn starch, barley starch, wheat starch, tapioca starch, bean starch, rice starch, pea starch, coral starch, canna starch, potato starch (potato starch).
  • the volume-based cumulative particle size (D50) measured by the laser diffraction method is 50 to 50 ⁇ m, for example.
  • the content of the pore-forming agent is, for example, 1 to 25 parts by mass with respect to 100 parts by mass of the inorganic compound powder.
  • the binder is, for example, celluloses such as methyl cellulose, hydroxypropyl methyl cellulose, carboxymethyl cellulose, sodium carboxymethyl cellulose; alcohols such as polyvinyl alcohol; salts such as lignin sulfonate; waxes such as paraffin wax and microcrystalline wax.
  • Content of the binder in a raw material mixture is 20 mass parts or less with respect to 100 mass parts of inorganic compound powder, for example.
  • plasticizer examples include alcohols such as glycerin; higher fatty acids such as caprylic acid, lauric acid, palmitic acid, alginic acid, oleic acid and stearic acid; stearic acid metal salts such as Al stearate, polyoxyalkylene alkyl ether ( For example, polyoxyethylene polyoxypropylene butyl ether).
  • Alcohols such as glycerin
  • higher fatty acids such as caprylic acid, lauric acid, palmitic acid, alginic acid, oleic acid and stearic acid
  • stearic acid metal salts such as Al stearate, polyoxyalkylene alkyl ether ( For example, polyoxyethylene polyoxypropylene butyl ether).
  • Content of the plasticizer in a raw material mixture is 10 mass parts or less with respect to 100 mass parts of inorganic compound powder, for example.
  • the dispersant examples include inorganic acids such as nitric acid, hydrochloric acid, and sulfuric acid; organic acids such as oxalic acid, citric acid, acetic acid, malic acid, and lactic acid; alcohols such as methanol, ethanol, and propanol; ammonium polycarboxylate.
  • Content of the dispersing agent in a raw material mixture is 20 mass parts or less with respect to 100 mass parts of inorganic compound powder, for example.
  • the solvent is, for example, water, and ion-exchanged water is preferable in terms of few impurities.
  • the content of the solvent is, for example, 10 to 100 parts by mass with respect to 100 parts by mass of the inorganic compound powder.
  • a green honeycomb formed body having a honeycomb structure is obtained.
  • a so-called extrusion molding method in which the raw material mixture is extruded from a die while being kneaded by a single screw extruder can be employed.
  • the honeycomb structured green honeycomb formed body obtained in the forming step is fired to obtain a honeycomb fired body.
  • calcination degreasing for removing a binder or the like contained in the molded body (in the raw material mixture) may be performed before the molded body is fired.
  • the firing temperature is usually 1300 ° C. or higher, preferably 1400 ° C. or higher.
  • a calcination temperature is 1650 degrees C or less normally, Preferably it is 1550 degrees C or less.
  • the temperature raising rate is not particularly limited, but is usually 1 to 500 ° C./hour.
  • the firing time may be a time sufficient for the inorganic compound powder to transition to the aluminum titanate-based crystal, and varies depending on the amount of raw material, type of firing furnace, firing temperature, firing atmosphere, etc., but usually 10 minutes to 24 hours.
  • the sealing step is performed between the molding step and the firing step or after the firing step.
  • a sealing step is performed between the forming step and the firing step, one end of each flow path of the green honeycomb molded body obtained in the forming step is sealed with a sealing material, and then green honeycomb forming is performed in the firing step.
  • a honeycomb structure including a sealing portion that seals one end of the flow path is obtained.
  • the sealing step after the firing step after sealing one end of each flow path of the honeycomb fired body obtained in the firing step with the sealing material, the flow path is obtained by firing the sealing material together with the honeycomb fired body.
  • a honeycomb structure provided with a sealing portion that seals one end of the above is obtained.
  • As the sealing material a mixture similar to the raw material mixture for obtaining the green honeycomb molded body can be used.
  • the catalyst layer forming step is performed after the firing step and the sealing step.
  • zeolite is wet-mixed with at least one metal element selected from the group consisting of titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, rhodium, palladium, silver and platinum, and dried and crushed. Then, if necessary, this is mixed with silica sol and / or alumina sol and water to prepare a slurry.
  • metal element selected from the group consisting of titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, rhodium, palladium, silver and platinum, and dried and crushed. Then, if necessary, this is mixed with silica sol and / or alumina sol and water to prepare a slurry.
  • copper can be exchanged into the pores of the zeolite by using copper acetate and iron as an ammine complex.
  • the produced slurry is subjected to the inside of the channel (first channel) in which the gas inlet side of the honeycomb structure is open and the channel (second channel) in which the gas outlet side is open. ) And apply to the partition wall surface.
  • the film is dried at 500 ° C. to 700 ° C. for about 1 hour to remove moisture.
  • a catalyst layer containing zeolite and the specific metal element is produced.
  • the catalyst layer also enters inside the pores of the partition walls (inside the communication holes), and is formed not only on the surface of the partition walls in the flow path but also on the surfaces inside the pores of the partition walls.
  • a honeycomb filter provided with a catalyst layer in the partition wall surfaces and partition pores in the first and second flow paths can be obtained.
  • Example 1 The following aluminum source powder, titanium source powder, magnesium source powder, silicon source powder, aluminum magnesium titanate powder and pore former were mixed to obtain a mixed powder.
  • the particle size (D50) corresponding to a volume-based cumulative percentage of 50% was measured using a laser diffraction particle size distribution analyzer (“Microtrac HRA (X-100)” manufactured by Nikkiso Co., Ltd.).
  • Aluminum source powder 37.5 parts by mass Aluminum oxide powder ( ⁇ -alumina powder) having a center particle size (D50) of 29 ⁇ m
  • Titanium source powder 36.8 parts by mass Titanium oxide powder having a D50 of 0.6 ⁇ m (rutile crystal)
  • Magnesium source powder 1.96 mass parts
  • Silicon source powder 3.18 mass parts Glass frit with D50 of 8.5 ⁇ m (deflection point: 642 ° C.)
  • Pore forming agent 11.7 parts by weight
  • Potato starch powder having a D50 of 31 ⁇ m
  • Aluminum magnesium titanate powder 8.83 parts by weight
  • As the aluminum magnesium titanate powder a sintered body of aluminum magnesium titanate is pulverized. The powder obtained was used.
  • the charged composition of each component in the mixed powder was [Al 2 O 3 ] / [TiO 2 in a molar ratio in terms of alumina [Al 2 O 3 ], titania [TiO 2 ], magnesia [MgO] and silica [SiO 2 ].
  • ] / [MgO] / [SiO 2 ] 35.1% / 51.3% / 9.6% / 4.0%.
  • content of the silicon source powder with respect to the total amount of aluminum source powder, titanium source powder, magnesium source powder, silicon source powder, and aluminum magnesium titanate powder was 3.6 mass%.
  • Methyl cellulose 5.49 parts by mass, hydroxypropyl methylcellulose 2.35 parts by mass, glycerol 0.40 parts by mass and polyoxyethylene polyoxypropylene butyl ether 4.64 parts by mass were added to 100 parts by mass of the mixed powder. Furthermore, after adding 28.44 parts by mass of water, the mixture was extruded using a kneading extruder and dried by microwave drying to obtain a dried honeycomb structure having a number of through holes in the longitudinal direction. The dried honeycomb structure was fired in an air atmosphere including a calcination (degreasing) step of removing the organic binder. The maximum temperature during firing was 1500 ° C., and the holding time at the maximum temperature was 5 hours.
  • honeycomb fired body having the honeycomb structure shown in FIGS. 4 to 6 (however, the catalyst layer and the sealing portion are not formed) (the shape of the fired body: columnar, the cross-sectional shape of the through hole: regular hexagonal shape and flat hexagonal shape) Shape, diameter of fired body: 25 mm, height of fired body: 50 mm, cell density: 300 cpsi, cell wall thickness: 0.3 mm).
  • Example 2 As a ceramic powder, a powder obtained by pulverizing an aluminum titanate-based ceramic containing strontium as a constituent element with a mortar was prepared. When the chemical composition of this ceramic powder was analyzed by XRF (fluorescence X-ray analysis), the ceramic powder was found to be 38.4% by mass of Al in terms of Al 2 O 3 , 35.4% by mass of Ti in terms of TiO 2 , SiO 2 It was confirmed that 16.3% by mass of Si in terms of 2 and 8.29% by mass of Sr in terms of SrO were confirmed.
  • XRF fluorescence X-ray analysis
  • the mixed powder was obtained by mixing 88.3 parts by mass of the ceramic powder and 11.7 parts by mass of a pore-forming agent (potato starch powder having a D50 of 31 ⁇ m). 5.49 parts by mass of methylcellulose, 2.35 parts by mass of hydroxypropylmethylcellulose, 0.40 parts by mass of glycerin and 4.64 parts by mass of polyoxyethylene polyoxypropylene butyl ether were added to 100 parts by mass of the mixed powder. Furthermore, after adding 28.44 parts by mass of water, the mixture was extruded using a kneading extruder and dried by microwave drying to obtain a dried honeycomb structure having a number of through holes in the longitudinal direction.
  • a pore-forming agent potato starch powder having a D50 of 31 ⁇ m
  • the dried honeycomb structure was fired in an air atmosphere including a calcination (degreasing) step of removing the organic binder.
  • the maximum temperature during firing was 1500 ° C., and the holding time at the maximum temperature was 5 hours.
  • a honeycomb fired body having the honeycomb structure shown in FIGS. 4 to 6 (however, the catalyst layer and the sealing portion are not formed) (the shape of the fired body: columnar, the cross-sectional shape of the through hole: regular hexagonal shape and flat hexagonal shape) Shape, diameter of fired body: 25 mm, height of fired body: 50 mm, cell density: 300 cpsi, cell wall thickness: 0.3 mm).
  • Aluminum source powder 46.9 parts by mass Aluminum oxide powder ( ⁇ -alumina powder) having a center particle size (D50) of 29 ⁇ m
  • Titanium source powder 37.6 parts by mass Titanium oxide powder having a D50 of 0.6 ⁇ m (rutile crystal)
  • Silicon source powder 3.5 parts by weight
  • Light anhydrous silicic acid having a D50 of 3.5 ⁇ m (bending point: 642 ° C.)
  • Pore forming agent 12 parts by mass Potato starch powder having a D50 of 31 ⁇ m
  • honeycomb fired body having the honeycomb structure shown in FIGS. 4 to 6 (however, the catalyst layer and the sealing portion are not formed) (the shape of the fired body: columnar, the cross-sectional shape of the through hole: regular hexagonal shape and flat hexagonal shape) Shape, diameter of fired body: 25 mm, height of fired body: 50 mm, cell density: 300 cpsi, cell wall thickness: 0.3 mm).
  • partition X-ray diffraction XRD
  • SEM scanning electron microscope
  • EDX energy dispersive X-ray analysis
  • Powder X-ray diffraction measurement of the partition walls was performed using a powder X-ray diffractometer (manufactured by Rigaku, trade name “RINT-2200HL”). Peaks attributed to aluminum titanate, titania and alumina are detected by powder X-ray diffraction measurement, and the ratio of the peak area of aluminum titanate to the total peak area of aluminum titanate, titania and alumina from those peak areas (%) was calculated.
  • the measurement results of Experimental Example 1 are shown in Table 1
  • the measurement results of Experimental Example 2 are shown in Table 2
  • the measurement results of Comparative Experimental Example 1 are shown in Table 3, respectively. In this measurement result, the smaller the decrease from the control experiment result, the more the thermal decomposition is suppressed.
  • FIG. 8B is an enlarged photograph of the region R3 in FIG. 8A
  • FIG. 8C is an enlarged photograph of the region R4 in FIG. 8B.
  • FIGS. 10A to 10B are SEM photographs of the section of the partition walls of the honeycomb fired body when the concentration of the Cu (NO 3 ) 2 aqueous solution in Experimental Example 2 is 30000 ppm and the heating condition is 900 ° C. for 5 hours.
  • EDX element mapping images are shown in FIGS.
  • FIG. 10B is an enlarged photograph of the region R5 in FIG. 11A is an element mapping image of Al in the region R5, and
  • FIG. 11B is an element mapping image of Ti in the region R5.
  • the whiter (brighter) portion means that the concentration of the element to be measured is higher.
  • the degree of thermal decomposition of aluminum titanate can be grasped. That is, the portion (AT in the figure) that can be confirmed by both the Al element mapping image and the Ti element mapping image is a portion where the aluminum titanate is maintained without being thermally decomposed.
  • the part that can be confirmed only (Al in the figure) is Al 2 O 3
  • the part that can be confirmed only by the element mapping image of Ti is TiO 2 . It can be said that the thermal decomposition of aluminum titanate is suppressed as there are more AT parts and fewer Al and Ti parts.
  • the part (Si in the figure) that cannot be confirmed in the element mapping image while the image is shown in the SEM photograph is the glass phase part.
  • Example 1 In the same manner as in Experimental Example 1, a dried honeycomb structure in which the catalyst layer and the sealing portion were not formed was produced. The dry honeycomb structure was sealed in the following procedure.
  • As the sealing material a mixture of aluminum titanate powder (powder obtained by pulverizing the honeycomb fired body obtained in Experimental Example 1), an organic binder (hydroxypropylmethylcellulose), a lubricant (glycerin), and water (solvent) was used. .
  • a film is previously applied to both end faces of the gas outlet of the dried honeycomb structure, and a sealing material is introduced into one end of each flow path through an opening in which the film is melted and perforated with a soldering iron. Dried.
  • the dried honeycomb structure into which the sealing material was introduced was fired in an air atmosphere including a calcination (degreasing) step of removing the organic binder.
  • the maximum temperature during firing was 1500 ° C., and the holding time at the maximum temperature was 5 hours.
  • a honeycomb fired body having a first flow path and a second flow path (the shape of the fired body: a columnar shape, a cross-sectional shape of a through hole: a regular hexagonal shape and a flat hexagonal shape, a diameter of the fired body: 25 mm, The height of the fired body: 50 mm, cell density: 300 cpsi, cell wall thickness: 0.3 mm) was obtained. Two honeycomb fired bodies were produced.
  • the formation of the catalyst layer was performed on each of the separate honeycomb fired bodies by the following two methods.
  • the first method is as follows. To a 100 mL poly beaker, 70 parts by mass of pure water and 30 parts by mass of the zeolite catalyst supporting the copper ions were added and stirred for 30 minutes. Furthermore, 6 parts by mass of a dispersant (made by NOF Corporation, trade name “Marialim”) was added and stirred for 1 hour. The honeycomb fired body was immediately dipped in this suspension solution until the gas inlet side of the honeycomb fired body was on the bottom, and the end surface on the gas outlet side was not soaked. Air was blown from the gas inlet side, and the excess suspension solution that blocked the first channel and the second channel was discharged to the outside of the honeycomb fired body. This honeycomb fired body was dried at 500 ° C.
  • FIG. 12A is a scanning electron microscope (SEM) photograph of the partition wall cross section of the catalyst layer-supporting honeycomb filter A
  • FIG. 12B is an enlarged photograph of the region R6 in FIG.
  • AT is aluminum titanate constituting the partition
  • CL is a catalyst layer.
  • the second method is as follows. To a 100 mL poly beaker, 70 parts by mass of pure water and 30 parts by mass of the zeolite catalyst supporting the copper ions were added and stirred for 30 minutes. Furthermore, 2.85 parts by mass of a viscosity modifier (manufactured by Ashland, ethyl cellulose) was added and stirred for 1 hour. A negative pressure was applied to the gas outlet side of the honeycomb fired body, and 8 parts by mass of this suspension solution was sucked from the gas inlet side. It dried at 500 degreeC for about 1 hour, and the catalyst layer carrying honeycomb filter B was obtained. As an evaluation of the catalyst layer, a scanning electron microscope (SEM) observation of the partition wall cross section was performed. FIG. 13 is a scanning electron microscope (SEM) photograph of the partition wall cross section of the catalyst layer-supporting honeycomb filter B. As shown in FIG. 13, it was confirmed that the catalyst layer was filled in the surfaces of the partition walls and the pores of the porous structure.
  • a viscosity modifier
  • Example 2 In the same manner as in Experimental Example 2, a dried honeycomb structure in which the catalyst layer and the sealing portion were not formed was produced. The dry honeycomb structure was sealed in the following procedure.
  • a film is previously applied to both end faces of the gas outlet of the dried honeycomb structure, and a sealing material is introduced into one end of each flow path through an opening in which the film is melted and perforated with a soldering iron. Dried.
  • the dried honeycomb structure into which the sealing material was introduced was fired in an air atmosphere including a calcination (degreasing) step of removing the organic binder.
  • the maximum temperature during firing was 1500 ° C., and the holding time at the maximum temperature was 5 hours.
  • a honeycomb fired body having a first flow path and a second flow path (the shape of the fired body: a columnar shape, a cross-sectional shape of a through hole: a regular hexagonal shape and a flat hexagonal shape, a diameter of the fired body: 25 mm, The height of the fired body: 50 mm, cell density: 300 cpsi, cell wall thickness: 0.3 mm) was obtained.
  • Comparative Example 1 In the same manner as in Comparative Experimental Example 1, a dried honeycomb structure in which the catalyst layer and the sealing portion were not formed was produced. The dry honeycomb structure was sealed in the following procedure.
  • a film is previously applied to both end faces of the gas outlet of the dried honeycomb structure, and a sealing material is introduced into one end of each flow path through an opening in which the film is melted and perforated with a soldering iron. Dried.
  • the dried honeycomb structure into which the sealing material was introduced was fired in an air atmosphere including a calcination (degreasing) step of removing the organic binder.
  • the maximum temperature during firing was 1500 ° C., and the holding time at the maximum temperature was 5 hours.
  • a honeycomb fired body having a first flow path and a second flow path (the shape of the fired body: a columnar shape, a cross-sectional shape of a through hole: a regular hexagonal shape and a flat hexagonal shape, a diameter of the fired body: 25 mm, The height of the fired body: 50 mm, cell density: 300 cpsi, cell wall thickness: 0.3 mm) was obtained.
  • ⁇ Evaluation 2 of thermal decomposition resistance> The catalyst layer-supporting honeycomb filters B to D obtained in Examples 1 and 2 and Comparative Example 1 are heat-treated at a predetermined temperature and time, and the thermal decomposition resistance is evaluated by evaluating the state of the partition walls after the heat treatment. did.
  • the heating conditions were 850 ° C. for 5 hours, 900 ° C. for 5 hours, 950 ° C. for 5 hours, 1000 ° C. for 5 hours, 1000 ° C. for 1 hour, or 1100 ° C. for 0.5 hour.
  • honeycomb filter having both an SCR function and a diesel particulate filter function that can suppress thermal decomposition of ceramics constituting the partition wall.

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  • Chemical Kinetics & Catalysis (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Porous Artificial Stone Or Porous Ceramic Products (AREA)
  • Compositions Of Oxide Ceramics (AREA)
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  • Exhaust Gas Treatment By Means Of Catalyst (AREA)

Abstract

La présente invention a pour but de proposer un filtre en nid-d'abeilles dans lequel la décomposition thermique d'une céramique constituant la paroi de séparation est rendue minimale et qui combine une fonction SCR et une fonction de filtre de particule diesel. L'invention concerne un filtre en nid-d'abeilles qui comprend une paroi de séparation qui forme de multiples canaux d'écoulement et qui a une première et une seconde face d'extrémité, dans lequel : les multiples canaux d'écoulement comprennent de multiples premiers canaux d'écoulement qui sont chacun scellés à l'extrémité sur le côté de seconde face d'extrémité et de multiples seconds canaux d'écoulement qui sont chacun scellés à l'extrémité sur le côté de première face d'extrémité ; le filtre en nid-d'abeilles comprend une couche de catalyseur qui est formée sur les surfaces de la paroi de séparation dans les premiers canaux d'écoulement, sur les surfaces de la paroi de séparation dans les seconds canaux d'écoulement et/ou dans les pores dans la paroi de séparation et qui contient à la fois de la zéolite et un ou plusieurs éléments métalliques choisis parmi Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Rh, Pd, Ag et Pt ; et la paroi de séparation comprend une céramique à base de titanate d'aluminium qui contient un ou plusieurs éléments choisis parmi Mg, Ca, Sr, Y, Ba, les lanthanoïdes et Bi.
PCT/JP2013/069530 2012-07-20 2013-07-18 Filtre en nid-d'abeilles Ceased WO2014014059A1 (fr)

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