EP4126793A1 - Corps moulé, corps composite, procédé de production d'un corps moulé et procédé de production d'un corps composite - Google Patents

Corps moulé, corps composite, procédé de production d'un corps moulé et procédé de production d'un corps composite

Info

Publication number
EP4126793A1
EP4126793A1 EP21715574.6A EP21715574A EP4126793A1 EP 4126793 A1 EP4126793 A1 EP 4126793A1 EP 21715574 A EP21715574 A EP 21715574A EP 4126793 A1 EP4126793 A1 EP 4126793A1
Authority
EP
European Patent Office
Prior art keywords
approximately
shaped body
coating material
pore structure
particles
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP21715574.6A
Other languages
German (de)
English (en)
Inventor
Adrian MARBERGER
Andreas Klimera
Georg Vieweger
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hug Engineering AG
Original Assignee
Hug Engineering AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hug Engineering AG filed Critical Hug Engineering AG
Publication of EP4126793A1 publication Critical patent/EP4126793A1/fr
Pending legal-status Critical Current

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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—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 aluminium oxide
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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
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    • C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
    • C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
    • C04B35/185—Mullite 3Al2O3-2SiO2
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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
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3239—Vanadium oxides, vanadates or oxide forming salts thereof, e.g. magnesium vanadate
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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
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3258—Tungsten oxides, tungstates, or oxide-forming salts thereof
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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
    • C04B2235/34—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
    • C04B2235/3427—Silicates other than clay, e.g. water glass
    • C04B2235/3463—Alumino-silicates other than clay, e.g. mullite
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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
    • C04B2235/34—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
    • C04B2235/3427—Silicates other than clay, e.g. water glass
    • C04B2235/3463—Alumino-silicates other than clay, e.g. mullite
    • C04B2235/3481—Alkaline earth metal alumino-silicates other than clay, e.g. cordierite, beryl, micas such as margarite, plagioclase feldspars such as anorthite, zeolites such as chabazite
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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
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/616—Liquid infiltration of green bodies or pre-forms
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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
    • C04B2235/6567—Treatment time
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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
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density
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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
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient

Definitions

  • the present invention relates to a molded body.
  • the present invention also relates to a composite body.
  • the present invention further relates to a method for producing a molded body and a method for producing a composite body.
  • Shaped bodies are known from DE 10 2013 204276 A1.
  • the present invention is based on the object of providing a molded body which has good flea temperature resistance, a coating material permanently adheres to wel chem and which is easy to manufacture.
  • the shaped body is designed in particular as a carrier body for a coating mate rial.
  • the molded body comprises: a channel structure which is formed by shaping a material of the molded body; and a pore structure in the material of the molded body.
  • the material of the shaped body comprises a particulate base material or is at least partially formed therefrom.
  • the base material comprises, in particular, a cordierite material and / or a mullite material or is formed therefrom.
  • the cordierite material is a cordierite chamotte.
  • the mullite material is, for example, a mullite chamotte. It can be advantageous if particles of the base material are indirectly and / or directly connected to one another. In pores of the pore structure, approximately 5% by volume or more of a coating material, based on a total volume of the pore structure, can be absorbed and / or absorbed.
  • approximately 10% by volume of the coating material or more, based on the total volume of the pore structure, can be taken up or taken up in pores of the pore structure.
  • the inclusion of the coating material in pores of the pore structure can improve the adhesion properties of the coating material.
  • particulate base material By using particulate base material, a random orientation of the particles in the material of the shaped body can be formed. In this way, a preferred orientation can be avoided and / or the material of the molded body can have constant thermal conductivity properties in all spatial directions.
  • the coating material forms, in particular, an active material which acts, for example, as a catalyst material.
  • the shaped body is suitable as a support body for 3-way catalytic converter applications and / or diesel oxidation catalytic converter applications and / or SCR (selective catalytic reduction) applications.
  • the shaped body is preferably a ceramic body.
  • the particles of the base material are preferably connected to one another while retaining their particle properties.
  • the particulate base material is pre-burned and / or ground up.
  • the cordierite material is preferably a precalcined cordierite material, which was ground up in particular after calcining.
  • the cordierite material can be, for example, a cordierite chamot.
  • a pre-calcined mullite material is preferably used, which has been ground in particular after the calcination.
  • the mullite material can be, for example, mullite chamotte, sintered mullite and / or fused mullite.
  • Fireclay is to be understood as a fired or pre-fired and then ground material.
  • the calcination can change the reaction and / or melting properties of the cordierite material and / or the mullite material.
  • the precalcined cordierite material and / or the precalcined mullite material of the base material can essentially retain their particle properties in a firing process to form the shaped body.
  • the cordierite material and / or the mullite material is calcined at approximately 1000 ° C. or more and / or at approximately 1700 ° C. or less.
  • particle property is to be understood in particular to mean that clear boundaries of the particles can be recognized in a scanning electron microscope image (SEM image) of the shaped body.
  • SEM image scanning electron microscope image
  • the particles are preferably embedded and / or networked with one another, for example glued.
  • the particles are preferably not completely melted and are fused with other particles to form a larger body.
  • the random orientation of the particles of the base material can be recorded and / or fixed.
  • a core part of the respective particle remote from the surface preferably remains physically and / or chemically unchanged.
  • a crystal structure of the particles of the base material preferably remains essentially unchanged.
  • the channel structure is preferably a macroscopic channel structure which can be seen in particular with the naked eye.
  • the pore structure is preferably a microscopic pore structure which cannot be seen with the naked eye and / or can only be seen in an electron microscope image.
  • the total volume of the pore structure is preferably an external volume of the pore structure.
  • the total volume of the pore structure is volume which is formed by a porosity of cavities formed and / or minus (macroscopic) cavities formed in the channel structure.
  • the shaped body and the coating material interlock in a coated state of the shaped body.
  • the shaped body and the coating material preferably form a composite body with the coating material in a coated state of the shaped body.
  • the surfaces of the pore structure and of the coating material are, in particular, interlaced with one another in the coated state of the molded body.
  • the pore structure is openly porous and / or has no closed surface and / or closed skin on surfaces facing the cavities of the channel structure.
  • the pore structure has a rough surface.
  • the shaped body Due to the pore structure in the material of the shaped body, the shaped body preferably has a sponge effect, so that the coating material can penetrate into the pore structure in the material of the shaped body during the production of the composite body.
  • the coating material is preferably arranged on the inside of walls which delimit cavities in the channel structure and / or completely covers the walls of the channel structure.
  • the material of the shaped body comprises a binding material by means of which particles of the base material are connected to one another, in particular in a materially bonded manner.
  • the binding material forms, for example, a matrix material in which particles of the base material are received and / or distributed.
  • the binding material or one or more precursors of the binding material comprises one or more of the following materials or are formed therefrom: one or more transition metal oxides, in particular titanium oxide; - one or more aluminum oxides; one or more alkaline earth oxides, in particular magnesium oxide; and one or more silicates.
  • aluminum hydroxide can form a material of the binding material or a precursor thereof.
  • the binding material preferably acts as an adhesive which holds the particles of the base material together.
  • a proportion of the binding material in the shaped body is approximately 10% by weight or more and / or approximately 40% by weight or less, based on a total mass of the shaped body.
  • the proportion of the binding material in the shaped body is in particular approximately 15% by weight or more and / or approximately 30% by weight or less, based on the total mass of the shaped body.
  • the shaped body is produced in a rapid firing process.
  • a chemical reaction of one or more precursors of the binding material can take place, while the particles of the base material for the most part, for example 50% by volume or more, based on a total volume of the respective particle, remain chemically unchanged.
  • the porosity of the pore structure is approximately 35% or more, in particular approximately 43% or more.
  • the porosity of the pore structure is approximately 54% or less, for example approximately 46% or less.
  • the porosity is preferably defined as a ratio of a cavity volume and the total volume of the pore structure of the shaped body. In particular Volumes formed by cavities in the channel structure of the molded body are not taken into account in the porosity.
  • a specific heat capacity of the material of the shaped body is reduced compared to materials of the same composition with lower porosity.
  • an average pore diameter of the pores of the pore structure is approximately 7 ⁇ m or more, in particular approximately 10 ⁇ m or more.
  • a mean pore diameter of the pores of the pore structure is preferably approximately 20 ⁇ m or less, in particular approximately 16 ⁇ m or less.
  • the mean pore diameter of the pores of the pore structure is approximately 12 ⁇ m or more and / or approximately 15 ⁇ m or less.
  • the molding can be loaded with the coating material to a greater extent.
  • the loading of the catalytically active coating material can be increased in this way without an open cross section of the cavities in the molded body being reduced. In this way, optimized activity can be achieved as SCR material.
  • the shaped body preferably has a reduced bulk density (without cavities formed by the channel structure) due to the comparatively high porosity. In an application in exhaust gas aftertreatment, this can lead to optimized start-up behavior, especially since less mass has to be heated. In this way, a state of maximum turnover can be reached more quickly.
  • bulk density is preferably to be understood as a density of the corresponding body based on its volume, including the pore spaces it contains. In particular, cavities formed by the channel structure - unless explicitly stated - are not included in the bulk density.
  • the shaped body is preferably a honeycomb body, in particular a substrate for a catalytic coating.
  • the shaped body is suitable for use as a catalyst carrier.
  • a preform of the molded body can be shaped, for example, in a pressing process and / or an extrusion process.
  • a shaped body designed as a honeycomb body preferably has honeycombs arranged in a matrix shape.
  • the honeycomb body has a square cross section and comprises honeycombs (cells) which are arranged in the form of a matrix and are cylindrical, the honeycombs (cells) preferably also having a square cross section.
  • the molded body comprises 100 cells per square inch or more and / or 300 cells per square inch or less.
  • the molded body comprises 150 cells per square inch or 100 cells per square inch.
  • the shaped body has a mass concentration of approximately 450 g / l or less, in particular of approximately 360 g / l or less.
  • the mass concentration is preferably a bulk density of the shaped body, plus cavities formed by the channel structure.
  • the mass concentration is a volume weight of the shaped body.
  • Walls separating individual cavities of the channel structure of the shaped body preferably have a wall thickness of approximately 500 ⁇ m or less and / or approximately 200 ⁇ m or more.
  • a mean grain size (particle size) of the particles of the base material is preferably approximately 2/5 or less, in particular 1/3 or less, of a wall thickness of the walls of the molded body.
  • the wall thickness is preferably an average wall thickness.
  • the mean grain size (particle size) of the particles of the base material is approximately 1/20 or more of the mean wall thickness of the shaped body.
  • an average grain size of the particles of the base material is approximately 100 ⁇ m or less.
  • a grain size d o of the particles of the base material made of cordierite material and / or mullite material is in particular approximately 15 ⁇ m or more, in particular approximately 40 ⁇ m or more, and / or approximately 60 ⁇ m or less.
  • a grain size distribution (particle size distribution) of the particles of the cordierite material is preferably the following: dio about 1 ⁇ m or more and / or about 3 ⁇ m or less, for example 2 ⁇ m; and / or d o about 10 pm or more and / or about 28 pm or less, for example about 18 pm; and / or dgo about 30 pm or more and / or about 40 pm or less, for example 35 pm.
  • a dio value is to be understood as the particle size below which 10% of the particles of the respective substance fall below, while 90% of the particles of the respective substance are larger than the dio value.
  • a d 50 value is to be understood as the particle size below which 50% of the particles of the respective substance fall below, while 50% of the particles of the respective substance are larger than the do value.
  • a dgo value is to be understood as the particle size below which 90% of the particles of the respective substance fall below, while 10% of the particles of the respective substance are larger than the dgo value.
  • the grain size distribution can be obtained, for example, by sieving the particles.
  • the invention also relates to a composite body.
  • the invention is based on the object of providing a composite body which is easy to manufacture and has high temperature stability and high mechanical stability.
  • the composite body preferably comprises a shaped body according to the invention and a coating material.
  • the composite body according to the invention preferably has one or more features and / or one or more advantages of the molded body according to the invention.
  • the composite body is particularly suitable for use in the selective catalytic reduction of nitrous gases by means of ammonia (SCR applications) and / or in the oxidation of hydrocarbons by means of diesel oxidation catalysts.
  • the composite body can be used in exhaust gas aftertreatment.
  • the coating material extends into pores of the pore structure of the shaped body in a coated state of the shaped body.
  • the coating material is chemically and / or physically bonded to the material of the shaped body.
  • One or more constituents and / or one or more substances and / or one or more materials in chemically identical composition and / or chemically identical form are preferably contained both in the material of the molded body and in the coating material.
  • one or more crystal structures in the material of the molded body and the coating material match.
  • one or more compounds are contained in chemically and / or physically identical form both in the material of the molded body and in the coating material.
  • the coating material comprises or is formed from one or more of the following materials: titanium dioxide, vanadium oxide, in particular vanadium (V) oxide, tungsten oxide, in particular tungsten (VI) oxide.
  • a vanadium component is preferably less than a vanadium component in a full extrudate, based on a total mass of the composite body or the full extrudate.
  • the coating material is preferably a titanium dioxide-based material which comprises, for example, approximately 80% by weight or more, in particular approximately 85% by weight or more, titanium dioxide, based on a total mass of the coating material.
  • the coating material has approximately 95% by weight or less, in particular approximately 92% by weight or less, of titanium dioxide, based on the total mass of the coating material.
  • the coating material comprises approximately 0.5% by weight to approximately 3% by weight vanadium (V) oxide, for example approximately 2% by weight vanadium (V) oxide, based on a total mass of the coating material after calcination.
  • the coating material preferably comprises approximately 5% by weight to approximately 10% by weight tungsten (VI) oxide, based on the total mass of the coating material after calcination.
  • the coating material comprises approximately 88% by weight to approximately 93% by weight titanium dioxide, based on a total mass of the coating material after calcination.
  • the coating material is in powder form.
  • a coating material mixture comprises a liquid in an amount which essentially corresponds to a pore volume of the pore structure of the shaped body.
  • a NO x activity through the composite body at approximately 300 ° C. to approximately 500 ° C. is preferably approximately 30% higher than a NO x activity in a comparable full extrudate with the same composition and identical measurement conditions.
  • the invention also relates to a method for setting a shaped body, in particular a shaped body according to the invention.
  • the invention is based on the object of providing a method for producing a shaped body by means of which a shaped body with good high temperature resistance can be easily produced.
  • a mixture is preferably provided which comprises a particulate base material or is formed therefrom.
  • the particulate base material is preferably pre-burned and / or ground up.
  • the particulate base material comprises a cordierite material and / or a mullite material or is formed therefrom.
  • a preform is preferably produced by shaping the mixture, a channel structure in particular being formed.
  • the shaped body has, in particular, a pore structure.
  • pores of the pore structure are preferably approximately 5% by volume of a coating material or more, based on a total volume of the pore structure, can be absorbed.
  • the method according to the invention preferably has one or more features and / or one or more advantages of the molded body according to the invention and / or the composite body according to the invention:
  • the shaped body is preferably made in a rapid firing process with a temperature gradient of> 2300 ° C (more than 2300 ° C), in particular> 2200 K / m (more than 2200 K / m) and / or> 2200 K / h (more than 2200 K) / h), for example in the range between approximately 120 ° C and approximately 2000 ° C.
  • the shaped body is preferably fired at a temperature of at most approximately 1,400 ° C.
  • the particles of the base material can be bonded to one another while maintaining the particle property.
  • it can be prevented that an undesired conversion of the base material, for example complete melting of the particles of the base material, occurs at a temperature above approximately 1,400 ° C.
  • the temperature is preferably chosen so that solid-state reactions lead to the formation of the dimensionally stable molded body.
  • the shaped body is fired at a temperature of approximately 1,300.degree.
  • the preform is fired in a firing cycle with a duration of at least approximately 300 minutes and / or at most approximately 480 minutes, for example approximately 360 minutes.
  • the duration of the firing cycle is to be understood as the time between the beginning of the firing process of the preform and the end of the firing process, in particular removal of the shaped body formed during the firing process from a furnace. In particular, this is to be understood as the time between the start of the firing process and the cooling of the fired shaped body.
  • the base material is essentially formed from the cordierite material.
  • the base material comprises approximately 90% by weight of cordierite material or more, in particular approximately 95% by weight or more, based on a total mass of the base material.
  • the base material comprises approximately 10% by weight of mullite material or less, in particular approximately 5% by weight or less, based on the total mass of the base material.
  • the mixture comprises one or more precursors of a binding material and if the particles of the base material are absorbed by the binding material and / or by the binding material through chemical and / or physical reaction of the one or more precursors to the binding material get connected.
  • an average grain size of the particles of the base material is larger by a factor of 2 or more than a grain size of one or more precursors which form a binding material of the material of the shaped body through the firing.
  • one or more precursors of the binding material react chemically and / or physically during the firing of the preform, a cordierite material being formed.
  • the particles of the base material are preferably connected to one another.
  • the mixture comprises a pore-forming material.
  • the pore-forming material preferably comprises one or more of the following materials or is formed from them: potato starch, graphite, coconut flour, acrylic glass, acrylate.
  • the additional pore-forming material preferably burns with the formation of gaseous constituents which emerge from the material with the formation of the pore structure. It can be advantageous if a proportion of the pore-forming material is approximately 5% by weight or more, in particular approximately 10% by weight or more, based on a total mass of the mixture.
  • the proportion of the pore-forming material is approximately 20% by weight or less, in particular approximately 15% by weight or less, based on the total mass of the mixture.
  • the mixture preferably comprises one or more precursors which react to form a binding material.
  • the binding material binds particles of the base material to one another.
  • the binding material comprises or is formed from one or more of the following materials: one or more transition metal oxides, in particular titanium dioxide; one or more aluminas; one or more alkaline earth oxides, in particular magnesium oxide; and one or more silicates.
  • Magnesium silicates are also suitable as silicates.
  • composition is particularly preferred for the precursors: titanium dioxide, several aluminum oxides, one or more kaolins, magnesium oxide, kaolin chamotte, aluminum hydroxide, one or more silicates.
  • a portion of the titanium dioxide is preferably about 1% by weight or more and / or about 5% by weight or less, based on the total mass of the binding material or based on the total mass of the mixture .
  • a composition of the precursors is preferably chosen such that cordierite is formed as a component of the binding material.
  • the present invention also relates to a method for producing a composite body, in particular a composite body according to the invention.
  • the invention is based on the object of providing a method for producing a composite body by means of which a composite body can be produced, which has a high temperature stability and a high mechanical stability.
  • a shaped body is preferably provided, in particular a shaped body according to the invention.
  • a coating material mixture is preferably applied to the shaped body and / or to the shaped body.
  • the coating material mixture preferably comprises a coating material and a liquid.
  • the shaped body and the coating material mixture applied to it and / or on it are preferably fired so that the coating material forms a coating on the shaped body and / or on the shaped body, with approximately 5 vol .-% of the coating material or more, based on a total volume of the pore structure, are taken up.
  • the method according to the invention for creating a composite body preferably has one or more features and / or one or more advantages of the method according to the invention for creating a molded body, the molded body according to the invention and / or the composite body according to the invention.
  • the liquid of the coating material mixture is water.
  • the coating material is powdery and / or is formed by calcining.
  • the shaped body and / or the composite body preferably also have the following features and / or advantages: through an enlarged uptake of the coating material in the pore structure of the shaped body, a pressure loss is reduced and / or an activity is increased with the same load; and or a weight of the shaped body reduced by approximately 20% to approximately 30% due to the porosity; and / or optimized adaptation of the material of the shaped body to the coating material; and / or through the improved adhesion of the coating material to the molded body, the connection between the coating material and the molded body is secured against mechanical abrasion and / or crumbling due to vibrations; and / or cracking in the coating material is minimized; and / or in comparison to a fully extruded catalyst material, a mechanical stability increased by a factor of 5 can be formed; and / or compared to a fully extruded catalyst material, the composite body is less brittle; and / or compared to a fully extruded catalyst material, the composite body has a coefficient of
  • 1 a first scanning electron microscope image of a section through a wall of an embodiment of a molded body in an uncoated state
  • 2 a comparison of a scanning electron microscope image of a section through a wall of a molded body and an EDX mapping of the same area
  • FIG. 3 shows a scanning electron microscope image of an embodiment of a composite body, a molded body having been coated with a coating material, in a section perpendicular to a direction in which a channel of the molded body extends;
  • FIG. 4 a scanning electron microscope image of the composite body from FIG. 3, magnified 800 times.
  • FIG. 1 of a molded body designated as a whole by 100 preferably forms a carrier body for a coating material 102 (cf. FIGS. 3 and 4).
  • the molded body 100 and the coating material 102 together form a composite body 104 in a coated state of the molded body 100.
  • the molded body 100 can have dimensions of up to 450 mm in all spatial directions.
  • the shaped body 100 preferably has regularly arranged flea spaces by shaping a material of the shaped body 100, through which a channel structure 106 of the shaped body 100 is formed.
  • the channel structure 106 is preferably a macroscopic channel structure.
  • the shaped body 100 preferably forms a honeycomb body which has channels with an at least approximately square cross section.
  • a wall thickness of the wall 108 of the channel structure 106 of the molded body 100 is preferably approximately 150 ⁇ m or more, in particular approximately 200 ⁇ m or more.
  • the wall thickness of the wall 108 is approximately 500 ⁇ m or less, for example approximately 300 ⁇ m or less.
  • a wall thickness of 290 ⁇ m has been found to be a particularly preferred wall thickness.
  • the wall thickness is preferably an average wall thickness.
  • the molded body 100 comprises 100 or 150 cells per square inch.
  • the shaped body 100 comprises a pore structure 110 which is formed in the material of the shaped body 100.
  • the pore structure 110 is preferably a microscopic pore structure.
  • the pores of the pore structure 110 are shown darker than the material of the molded body 100.
  • a porosity of the pore structure 110 is preferably approximately 35% or more, in particular approximately 43% or more.
  • the porosity of the pore structure 110 is approximately 54% or less, in particular approximately 46% or less. “Porosity” is preferably to be understood as a ratio of a cavity volume and a total volume of the pore structure 110. Cavities formed by shaping the material into the channel structure 106 are excluded from the total volume of the pore structure 110.
  • An average pore diameter of the pores of the pore structure 110 of the molded body 100 is preferably approximately 10 ⁇ m or more, in particular approximately 12 ⁇ m or more.
  • the mean pore diameter of the pore structure 110 of the molded body 100 is approximately 20 ⁇ m or less, for example approximately 16 ⁇ m or less.
  • the porosity of the pore structure 110 is preferably an open porosity.
  • the coating material 102 can penetrate into pores of the pore structure 110 of the molded body 100 during the production of the composite body 104.
  • a mass concentration and / or density of the molded body 100 is preferably approximately 300 g / l or more and / or approximately 450 g / l or less.
  • the mass concentration and / or bulk density plus cavities of the molded body 100 formed by the channel structure is approximately 350 g / l.
  • outer surfaces of the walls 108 of the channel structure 106 of the molded body 100 have a rough surface.
  • an extrusion skin of the molded body 100 is designed to be rough and / or spatially structured.
  • the material of the molded body 100 preferably comprises base material which comprises or is formed from a cordierite material and / or a mullite material.
  • the base material of the material of the molded body 100 is preferably in powder form and / or in particulate form.
  • particles of the base material are connected to one another by means of a binding material 112, in particular cohesively, and / or are glued to one another by means of the binding material 112.
  • the particles of the base material are preferably surrounded in the molded body 100 by the binding material 112 (cf. FIG. 4).
  • a mixture is preferably provided or produced, which is shaped into a preform and then burned in a rapid firing.
  • the mixture preferably comprises the base material and precursors of the binding material 112.
  • titanium dioxide, one or more aluminum oxides, one or more magnesium oxides, one or more silicates and aluminum hydroxide are used as precursors of the binding material 112.
  • one or more of the following materials are used as precursors for the binding material: titanium dioxide, several aluminum oxides, one or more kaolins, magnesium oxide, kaolin chamotte, aluminum hydroxide, one or more silicates.
  • Magnesium silicates for example a product from the Finntalc series from Mondo Minerals B.V., 1041 AR Amsterdam, Netherlands, are also suitable as silicates.
  • Examples of aluminum oxides are the product NABALOX® NO 715-10 from Nabaltec AG, 92409 Schwandorf; one of the products of the range of aluminum oxide CT from GÜPO GmbH, 77694
  • a proportion of the one or more precursors of the binding material 112 is approximately 10% by weight or more and / or approximately 35% by weight or less, based on a total mass of the mixture.
  • a proportion of the titanium dioxide is preferably approximately 1% by weight or more and / or approximately 5% by weight or less, based on the total mass of the binding material 112 or based on the total mass of the mixture.
  • the mixture contains a pore-forming material in addition to the base material and the precursors of the binding material.
  • the pore-forming material serves in particular to form pores in the material of the molded body 100.
  • the pore-forming material is added, for example, before and / or during the formation of the preform.
  • the pore-forming material comprises or is formed from one or more of the following materials: potato starch, graphite, coconut flour, acrylic glass, acrylate.
  • a proportion of the pore-forming material is preferably approximately 5% by weight or more and / or approximately 20% by weight or less, based on the total mass of the mixture.
  • the base material is preferably powdery and / or particulate.
  • a grain size distribution (particle size distribution) of the particles of the cordierite material and / or of the mullite material is preferably the following: dio about 1 gm or more and / or about 3 gm or less, for example 2 ⁇ m; and / or d o about 10 pm or more and / or about 28 pm or less, for example about 18 pm; and / or dgo about 30 pm or more and / or about 40 pm or less, for example 35 pm.
  • a dio value is to be understood as the particle size below which 10% of the particles of the respective substance fall below, while 90% of the particles of the respective substance are larger than the dio value.
  • a do value is to be understood as the particle size below which 50% of the particles of the respective substance fall below, while 50% of the particles of the respective substance are larger than the do value.
  • a dgo value is to be understood as the particle size below which 90% of the particles of the respective substance fall below, while 10% of the particles of the respective substance are larger than the dgo value.
  • Comparatively coarse-grained cordierite material and / or mullite material is preferably used as the base material.
  • an average grain size of the particles of the cordierite material and / or mullite material used in the base material is, for example, approximately 100 ⁇ m or less.
  • the cordierite material and / or the mullite material are preferably burned, for example calcined.
  • the cordierite material and / or the mullite material are preferably ground and, for example, sieved.
  • cordierite material and no mullite material is used in or as the base material.
  • a proportion of approximately 10% by weight or less of mullite material, based on a total mass of the base material is used.
  • a proportion of the cordierite material is then in particular approximately 90% by weight, based on the total mass of the base material.
  • a preform is preferably first formed from the mixture for producing the molded body 100. This is preferably done by pressing and / or extrusion. In particular, the channel structure 106 of the molded body 100 is created here.
  • the preform is preferably dried, for example by means of microwave heating in a continuous oven.
  • the preform is then preferably fired, the molded body 100 being formed.
  • the firing is preferably carried out in a rapid firing continuous furnace.
  • a pushing speed is, for example, in a range from about 3 cm / min to about 10 cm / min.
  • the molded body 100 is preferably produced in a rapid firing process, with a preform with a temperature gradient of more than 2300 ° C., in particular more than 2200 K / m and / or more than 2200 K / h, for example in the range between approximately 120 ° C. and approximately 2000 ° C, fired.
  • the shaped body 100 is preferably produced when the preform is fired at temperatures of at most approximately 1,400 ° C. In this way, it is possible to connect the particles of the base material to one another while maintaining the particle property.
  • the preform is preferably fired at a temperature of approximately 1,300 ° C., the shaped body 100 being produced.
  • the preform is fired in a firing cycle with a duration of at least approximately 300 minutes and / or at most approximately 480 minutes, for example approximately 430 minutes to approximately 450 minutes.
  • the duration of the firing cycle is to be understood as the time between the beginning of the firing process of the preform and the end of the firing process, in particular removal of the molded body 100 formed during the firing process from a furnace. In particular, this is to be understood as the time between the start of the firing process and the cooling of the fired molded body 100.
  • the one or more non-pre-fired precursors of the binding material 112 preferably react, for example to form a cordierite material and other substances, while particles of the base material are only melted on the surface and / or only react with the constituents of the surface on their surface Binding material 112 enter.
  • the resulting molded body 100 preferably forms a carrier body for the coating material 102 (cf. FIGS. 3 and 4).
  • the coating material 102 is applied to and / or on the molded body 100, for example by means of dip coating.
  • the coating material 102 has one or more substances and / or constituents and / or materials which are chemically identical in composition and / or or chemically identical form are also contained in the material of the molded body 100.
  • titanium dioxide is used both as a precursor of the binding material 112 and as a component of the coating material 102.
  • the presence of titanium dioxide in the shaped body can be seen from the comparison, shown in FIG. 2, of an SEM image and an EDX (energy dispersive X-ray spectroscopy) mapping of the same area.
  • FIG. 2 shows an SEM image which was recorded with a magnification of 1,500 times and an acceleration voltage of 15.00 kV. A backscattered electron detector was used.
  • the SEM image shows that dark particles are recorded in a lighter material. These dark particles are the particles of the base material which also continue to have particle properties in the fired molded body 100. The lighter material surrounding the particles is the binding material 112.
  • Inclusions shown in white can be seen in the lighter material. These inclusions include titanium, since in the EDX (energy dispersive X-ray spectroscopy) mapping of the same area shown on the right, a signal is detected at energy that is characteristic of titanium. Since titanium was only contained in titanium dioxide in the starting materials, it can be assumed that the white inclusions are made of titanium dioxide.
  • the material has a porosity, with cavities being shown comparatively dark.
  • the coating material 102 shown in FIGS. 3 and 4 preferably comprises titanium dioxide and / or vanadium oxide, in particular vanadium (V) oxide, and / or tungsten oxide, in particular tungsten (VI) oxide.
  • FIG. 3 and 4 show SEM recordings of a section through the molded body 100 coated with the coating material 102.
  • the acceleration voltage for the recordings is 12.50 kV in each case.
  • the photograph shown in FIG. 3 was taken at a magnification of 110 times and shows a honeycomb of the shaped body 100.
  • the coating material 102 is applied to an inside facing the flea space.
  • FIG 4 shows the transition between the coating material 102 and the wall 108 of the molded body 100 at an 800-fold magnification.
  • a backscattered electron detector was used both for the recording in FIG. 3 and for the recording shown in FIG.
  • the coating material 102 comprises or is formed from the following materials: titanium dioxide, vanadium (V) oxide and tungsten (VI) oxide.
  • a proportion of the titanium dioxide in the coating material 102 is preferably approximately 80% by weight or more, based on a total mass of the coating material 102.
  • V vanadium
  • VI tungsten
  • Monoethanolamine and / or a colloidal silicon dioxide dispersion are suitable as one or more additives.
  • a proportion of the silicon dioxide dispersion is preferably approximately 2% by weight or more and / or approximately 5% by weight or less, based on a total mass of the mixture.
  • a proportion of the silicon dioxide in the silicon dioxide The dispersion is preferably 30% by weight, based on a total mass of the silicon dioxide dispersion.
  • the mixture is preferably dried in an oven and then calcined at about 400 ° C to about 600 ° C.
  • the coating material 102 is preferably dissolved and / or dispersed in a liquid.
  • An amount of the liquid preferably corresponds to a pore volume of the molded body 100.
  • the composite body 104 is preferably produced by firing.
  • the molded body 100 and / or the composite body 104 are particularly suitable for use in exhaust gas aftertreatment, for example as catalysts and / or as diesel particulate filters.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Nanotechnology (AREA)
  • Dispersion Chemistry (AREA)
  • Catalysts (AREA)

Abstract

Afin de fournir un corps moulé qui présente une bonne résistance à des températures élevées, auquel un matériau de revêtement adhère de manière permanente et qui est simple à produire, un corps moulé est proposé, qui présente une structure de canal, formée par la mise en forme d'un matériau du corps moulé, et une structure poreuse dans le matériau du corps moulé, le matériau du corps moulé comprenant un matériau de base particulaire ou étant au moins partiellement formé à partir de ce dernier, le matériau de base comprenant un matériau cordiérite et/ou un matériau mullite, les particules du matériau de base étant interconnectées indirectement et/ou directement, et approximativement 5 % en volume d'un matériau de revêtement ou plus, par rapport à un volume global de la structure poreuse, peuvent être reçus ou sont reçus dans des pores de la structure poreuse.
EP21715574.6A 2020-03-26 2021-03-26 Corps moulé, corps composite, procédé de production d'un corps moulé et procédé de production d'un corps composite Pending EP4126793A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102020203924.0A DE102020203924A1 (de) 2020-03-26 2020-03-26 Formkörper, Verbundkörper, Verfahren zur Herstellung eines Formkörpers und Verfahren zur Herstellung eines Verbundkörpers
PCT/EP2021/058013 WO2021191444A1 (fr) 2020-03-26 2021-03-26 Corps moulé, corps composite, procédé de production d'un corps moulé et procédé de production d'un corps composite

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EP4126793A1 true EP4126793A1 (fr) 2023-02-08

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US (1) US20240010565A1 (fr)
EP (1) EP4126793A1 (fr)
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Publication number Priority date Publication date Assignee Title
US5334570A (en) 1991-07-25 1994-08-02 Corning Incorporated Pore impregnated catalyst device
JP3874270B2 (ja) * 2002-09-13 2007-01-31 トヨタ自動車株式会社 排ガス浄化フィルタ触媒及びその製造方法
DE102005062317B4 (de) 2005-12-24 2008-08-21 Umicore Ag & Co. Kg Verfahren zur katalytischen Beschichtung von keramischen Wabenkörpern
US7575794B2 (en) * 2006-08-29 2009-08-18 Corning Incorporated High strength substantially non-microcracked cordierite honeycomb body and manufacturing method
JP5997025B2 (ja) * 2012-12-03 2016-09-21 日本碍子株式会社 ハニカム触媒体
DE102013204276A1 (de) 2013-03-12 2014-09-18 Hug Engineering Ag Verfahren zur Herstellung eines Formkörpers und Formkörper
DE102014104582A1 (de) 2014-04-01 2015-10-01 Denk Aqua GmbH Porenkörper
JP6906468B2 (ja) 2018-03-30 2021-07-21 日本碍子株式会社 セラミックス多孔体及びその製造方法、並びに集塵用フィルタ
DE102018127955A1 (de) 2018-11-08 2020-05-14 Umicore Ag & Co. Kg Katalytisch aktiver Partikelfilter mit hoher Filtrationseffizienz

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US20240010565A1 (en) 2024-01-11
WO2021191444A1 (fr) 2021-09-30

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