WO2006027593A2 - Catalyse - Google Patents

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Publication number
WO2006027593A2
WO2006027593A2 PCT/GB2005/003472 GB2005003472W WO2006027593A2 WO 2006027593 A2 WO2006027593 A2 WO 2006027593A2 GB 2005003472 W GB2005003472 W GB 2005003472W WO 2006027593 A2 WO2006027593 A2 WO 2006027593A2
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WO
WIPO (PCT)
Prior art keywords
slurry
species
mould surface
catalyst
mould
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.)
Ceased
Application number
PCT/GB2005/003472
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English (en)
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WO2006027593A3 (fr
Inventor
Rodney Martin Sambrook
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Dytech Corp Ltd
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Dytech Corp Ltd
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Publication date
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Publication of WO2006027593A2 publication Critical patent/WO2006027593A2/fr
Publication of WO2006027593A3 publication Critical patent/WO2006027593A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
    • C04B35/634—Polymers
    • C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B35/63444—Nitrogen-containing polymers, e.g. polyacrylamides, polyacrylonitriles, polyvinylpyrrolidone [PVP], polyethylenimine [PEI]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B5/00—Producing shaped articles from the material in moulds or on moulding surfaces, carried or formed by, in or on conveyors irrespective of the manner of shaping
    • B28B5/02—Producing shaped articles from the material in moulds or on moulding surfaces, carried or formed by, in or on conveyors irrespective of the manner of shaping on conveyors of the endless-belt or chain type
    • B28B5/026—Producing shaped articles from the material in moulds or on moulding surfaces, carried or formed by, in or on conveyors irrespective of the manner of shaping on conveyors of the endless-belt or chain type the shaped articles being of indefinite length
    • B28B5/027—Producing shaped articles from the material in moulds or on moulding surfaces, carried or formed by, in or on conveyors irrespective of the manner of shaping on conveyors of the endless-belt or chain type the shaped articles being of indefinite length the moulding surfaces being of the indefinite length type, e.g. belts, and being continuously fed
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B7/00—Moulds; Cores; Mandrels
    • B28B7/0064—Moulds characterised by special surfaces for producing a desired surface of a moulded article, e.g. profiled or polished moulding surfaces
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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
    • C04B35/111—Fine ceramics
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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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    • C04B35/624—Sol-gel processing
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    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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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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    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
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    • C04B35/632—Organic additives
    • C04B35/634—Polymers
    • C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B35/63424—Polyacrylates; Polymethacrylates
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    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
    • C04B38/0615—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances the burned-out substance being a monolitic element having approximately the same dimensions as the final article, e.g. a porous polyurethane sheet or a prepreg obtained by bonding together resin particles
    • C04B38/062—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances the burned-out substance being a monolitic element having approximately the same dimensions as the final article, e.g. a porous polyurethane sheet or a prepreg obtained by bonding together resin particles the burned-out substance being formed in situ, e.g. by polymerisation of a prepolymer composition containing ceramic powder
    • C04B38/0625—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances the burned-out substance being a monolitic element having approximately the same dimensions as the final article, e.g. a porous polyurethane sheet or a prepreg obtained by bonding together resin particles the burned-out substance being formed in situ, e.g. by polymerisation of a prepolymer composition containing ceramic powder involving a foaming step of the burnable material
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL-COMBUSTION ENGINES
    • F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
    • F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
    • F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
    • F01N3/24—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by constructional aspects of converting apparatus
    • F01N3/28—Construction of catalytic reactors
    • F01N3/2803—Construction of catalytic reactors characterised by structure, by material or by manufacturing of catalyst support
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
    • B01J35/56—Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional [3D] monoliths
    • C—CHEMISTRY; METALLURGY
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    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/0081—Uses not provided for elsewhere in C04B2111/00 as catalysts or catalyst carriers
    • C—CHEMISTRY; METALLURGY
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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
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
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    • C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
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    • C04B2235/5463—Particle size distributions
    • C04B2235/5472—Bimodal, multi-modal or multi-fraction
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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
    • C04B2235/6023—Gel casting
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    • C04B2235/945—Products containing grooves, cuts, recesses or protusions

Definitions

  • This invention relates to catalysis, particularly, but not exclusively, to catalyst carriers and to catalyst carriers carrying catalyst.
  • Catalyst carriers used in highly exothermic or endothermic reactions must be made from materials with excellent thermal stability and high mechanical strength. Of necessity, this usually means carriers with relatively low surface area and high bulk volume. Because of the high volume to surface area ratio, the catalyst efficiency and activity is lowered and the pressure-drop across the carrier high.
  • US 6670305 discloses a tape casting method for making a monolithic catalyst with micro-scale flow channels for auto-thermal reforming of hydrocarbon fuels.
  • Catalyst layers and fugitive layers of polymeric nature are tape cast repeatedly onto a substrate layer, to form a multi-layer green form. After each casting the layers are allowed to dry.
  • the fugitive layer has a thickness of between 1 and 150 ⁇ m, and the catalyst layer a thickness of between 1 and 200 ⁇ m. Once the green form is dried, the free ⁇ standing catalyst is peeled from the substrate, cut into strips and rolled or folded into bulk shapes before firing to ensure fugitive layer burnout and final sintering.
  • US 4025462 discloses forming a slurry of ceramic particles, plastic supporting matrix, plasticizer, organic solvent and a deflocculant and ball milling the slurry.
  • the milled slurry is then cast to form a film and the solvent removed to provide a self-supporting green ceramic tape.
  • the tape is then moulded to form a corrugated first member and a flat second member and these are then stacked in alternating layers of tape cast first and second members.
  • the corrugated sheets therefore created the flow channels to form a ceramic cellular structure.
  • a sacrificial sheet for example made of wax or polymers
  • Catalyst slurry is then tape cast onto this arrangement.
  • the green tape is then cut into strips and rolled or stacked to form the catalyst shapes before burnout of the sacrificial sheets and binders and final sintering.
  • the binders used are thermosetting resins and harden, at room temperature, in about ten days.
  • the term catalyst carrier may relate to a carrier comprising a catalytic species ⁇ i.e. is provided in situ) or which carries a catalytic species (e.g. the catalyst is coated, impregnated, deposited onto the external and/or internal surface and/or within the pore structure of the carrier walls and/or within the voids of the carrier subsequent to formation of the carrier).
  • the finished catalyst carrier is, to all intents and purposes, a catalyst.
  • a first aspect of the invention provides a method of fabricating a catalyst carrier, the method comprising forming a slurry of ceramic particles in a liquid carrier, the carrier comprising a binder species, applying the dispersion to a mould surface having formations provided therein or thereon, causing the binder species to set to provide a green form, drying and firing the green form, wherein the setting of the binder species to provide a green form which is removeable from the mould surface takes less than 120 minutes.
  • a second aspect of the invention provides a method of fabricating a catalyst carrier, the method comprising forming a slurry of ceramic particles in a liquid carrier, the liquid carrier comprising a binder species, applying the dispersion to a non-sacrificial mould surface having formations provided therein or thereon, causing the binder species to set to provide a green form, removing the green form from the mould surface, drying and firing the green form, wherein the setting of the binder species to provide a green form which is removeable from the mould surface, preferably, takes less than 120 minutes.
  • the term 'non-sacrificial mould surface' is intended to mean a mould surface which may be used again subsequent to the removal of the green form therefrom. That is to say that it is also unnecessary to destroy the mould surface to remove the green form therefrom.
  • the ceramic particles may be or may comprise a catalytic species.
  • the binder species is preferably a polymerisable monomeric species which may be a bi-functional monomeric species or a poly-functional monomeric species. If the polymeric species is bi-functional, the liquid carrier may also comprise a poly-functional monomeric species, and vice versa.
  • the terms 'bi-functional monomer' and 'bi-functional monomeric species' are intended to relate to monomers which give two and only two linkages to other monomers to form, say, linear polymers.
  • the terms 'poly- functional monomer' and 'poly-functional monomeric species' are intended to relate to monomers which give more than two linkages and are therefore usually able to cross-link to other monomers to form a three-dimensional network.
  • Suitable polymers are alkenes, acrylates, methacrylates, esters, anhydrides, acrylamides, or other polymerisable substances such as agarose, cellulose and so on.
  • the polymerisable monomeric species may comprise homopolymer units or copolymers (including ter and higher polymers). A pre-mix of the polymerisable monomer(s) may be provided to which a species to cause polymerization may be added.
  • Other binder species which may be used in addition or alternatively include polyvinyl alcohols (PVAs), alginates, starches and so on.
  • the slurry, and hence the green for, is preferably free from thermosetting resins.
  • the ceramic particles may comprise one or more of alumina, silica, hydroxyapatite, zirconia, silicon carbide, tin oxide, kyanite, cordierite, mullite, spinel, perovskites, titanium dioxide, zinc oxide, nickel aluminate, aluminium titanate, rare earth metal silicates, rare earth oxides, spinels and the like.
  • the dispersion may comprise 'active' catalytic species and/or the precursors thereof, for example one or more of molecular sieve, nickel oxide, iron oxide, manganese oxide, chromium oxide and other catalyst materials.
  • the particle size and size distribution should be chosen to meet the requirements of catalyst efficiency, sintered body strength, rheological property of the slurry and so on.
  • the usual particle size range is between 100nm to 100 ⁇ m, preferably between 300nm to 30 ⁇ m.
  • the slurry may also comprise one or more of solvents, dispersants, pore formers, plasticizers, viscosity modifiers and catalyst activity enhancers.
  • one or more dispersants may be added to introduce steric and/or electrostatic stabilisation.
  • Acrylic acid based polymers of specific molecular size range are most widely used dispersants although other phosphate based, non-ionic dispersants are also suitable for the present invention.
  • the selection of dispersants is still mainly based on experience and trial and error rather than scientific guidelines. Care must be taken to avoid or suppress chemical reactions between the monomers and dispersants or between the catalyst particles and dispersants.
  • Plasticizers may also be added if the process requires dry green form deformation.
  • plasticizers are those which are water soluble, environmentally friendly such as glycerol and polyethyleneglycol of various molecular sizes.
  • Viscosity modifiers may also be added to adjust the slurry viscosity to reduce the tendency of catalyst particle sedimentation or segregation, to reduce large air bubble entrapment, and to improve the casting conditions.
  • Sacrificial pore formers may also be added into the slurry if porosity is required within the catalyst body.
  • suitable pore formers widely used in the industry and the suitable one for this work include olive stone and almond shell powder of specific particle size and polymeric particles such as polyruric spheres. Pore formers should be carefully chosen so that after burnoff they do not leave residuals detrimental to the catalyst, that they burnoff well below the sintering temperature, that they do not deform (such as swelling) during slurry preparation and casting.
  • Porosity in the body may be provided by introducing air or another gas, for example by mechanical agitation, blowing or in situ gas generation into the slurry prior to casting.
  • Porosity in the body may also be introduced by emulsifying the slurry with low boiling point blowing agents such as cyclopentane and cyclohexane.
  • the blowing agent expands and evaporates, for example during and after the exothermic polymerization, and forms pores in the cast body.
  • the internal voids of the catalyst carrier may be filled with a foam material either catalytic or non-catalytic in nature either homogeneously or in zones to create differing reaction zones and/or control mass and heat transfer in local areas.
  • catalyst activity enhancers may also be added to improve the catalyst efficiency. These enhancers include those materials promoting the catalyst selectivity, avoiding the active catalyst particles forming agglomerate, and spacing the active catalyst particles more evenly in the catalyst body.
  • the catalyst slurry preparation generally includes the mixing of all the ingredients together or in preferred sequence with the monomers and solvents.
  • the prepared slurry will usually have a consistency of easy flowing or pouring, slow or no particles settling and segregation before and during casting, and uniform composition distribution throughout the slurry body.
  • the method may comprise the preliminary step of designing and preparing the mould surface and preparing a mould surface according to the design.
  • the mould surface will have intrinsic 'mould-releasing' characteristics.
  • the mould surface may be fabricated from a material comprising self- lubricating polymeric species, for example oil-filed Nylon 6 or MoS 2 -filled Nylon 6 (for example, those supplied by Bay Plastics Limited of North Shields, United Kingdom under the registered trademarks Nyloil and Nylatron respectively).
  • the mould surface may be formed from metal, wood or other polymeric species.
  • the mould may be formed as a discrete (i.e. stand-alone) mould member or may be formed as a continuous belt-type mould member.
  • the mould or at least the mould surface, will preferably be fabricated from a readily machinable material (the materials disclosed above satisfying the requirement) so that the mould surface can be provided with, for example, one or more of a series of shaped holes in say staggered or linear fashion, channels in linear, curved, zig-zagged, swirled or other shapes, notched diamond-shaped channels and so on or a combination thereof, which, in the finished catalyst carrier, will allow for interconnectivity for fluid flow whilst also providing a degree of control over direction of flow.
  • the mould surface may also be provided with formations or projections thereon corresponding to the above- identified holes or channels. In either case the projections, ridges, holes, channels efc.
  • the mould surface will preferably have a smooth, preferably substantially planar, finish to facilitate removal of the green form therefrom.
  • the slurry is cast directly on to the mould surface.
  • a further and/or more specific aspect of the invention provides a method of fabricating a catalyst carrier, the method comprising forming a mould surface having a desired arrangement of formations therein or thereon, forming a slurry of ceramic particles in a liquid carrier, the carrier comprising a polymerisable monomeric species, applying the dispersion to the mould surface, causing the monomeric species to polymerise to provide a green form, removing the green form from the mould surface, preferably within 120 minutes of commencement of the polymerization of the monomeric species, drying and firing the green form.
  • the green form may be achieved in less than 60 minutes, preferably less than 30 minutes and most preferably less than 15 minutes.
  • the method or methods may comprise the subsequent step of cutting the green form into sheets which may be stacked above one another or rolled into a cylinder to provide the catalyst carrier. It will be appreciated that the fired ceramic article will have formations along its length corresponding to a 'positive' or 'negative' of the formations formed in or on the mould surface respectively.
  • the body and/or walls of the catalyst carriers typically have a porosity of from 5 to 90%. They may typically have a thickness of from 0.3 to 3 mm with spacings between the walls of from 0.1 to 2.5 mm i.e. the longest projections will have a length between 0.1 and 2.5 mm.
  • a further aspect of the invention provides tape casting apparatus for providing a catalyst carrier, the apparatus comprising slurry mixing means and slurry delivery means to deliver slurry from said slurry mixing means to a mould surface, a doctor blade to spread slurry delivered from said slurry delivery means onto a mould surface and in-line mixing means located upstream of the doctor blade in said slurry delivery means, said in ⁇ line mixing means being arranged to mix a initiator and/or polymerization catalyst into slurry delivered through said slurry delivery means, the initiator and/or polymerization catalyst polymerizing a monomeric polymerisable species provided in the slurry delivered through said slurry delivery means.
  • a yet further aspect of the invention provides a method of casting a ceramic slurry on to a mould, the method comprising mixing ceramic particles and a binder species, for example a monomeric polymerisable species, to provide a slurry; delivering the slurry to a mould surface and spreading the slurry onto the mould surface using a doctor blade; and comprising mixing an initiator and/or polyermization catalyst into and with the slurry at a point upstream of the doctor blade to commence setting of the binder species, for example polymerization of the polymerisable monomeric species.
  • a binder species for example a monomeric polymerisable species
  • the mould is a shaped mould surface, for example one comprising an array of formations thereon or therein, arranged to provide a cast ceramic article having corresponding formations in or on a surface thereof.
  • Figure 1 is a plan view of a part of a first embodiment of catalyst carrier made by the method of the invention
  • Figure 1 A is a perspective view of the part of the carrier of Figure 1 ;
  • Figure 2 is a plan view of a part of a second embodiment of catalyst carrier made by the method of the invention.
  • Figure 2A is a perspective view of the part of the carrier of Figure 2;
  • Figure 3 is a perspective view of a mould surface used in the method of the invention.
  • Figure 4 is a schematic representation of a tape-casting apparatus useful in the method of the invention.
  • Figure 5 is a perspective view of the carrier of Figure 1 and 1 A, configured for use;
  • Figure 6 is a perspective view of a stack of the carriers of Figures 2 and 2A, configured for use.
  • a catalyst carrier 1 comprising a ceramic body 2 from which a plurality of integral cylindrical projections 3 extend.
  • a catalyst carrier 11 comprising a ceramic body 12 having an integral saw-tooth formation 13 on, or as, an upper surface.
  • the bodies 2, 12 of the carriers 1 , 11 may be dense or may have a defined priority
  • FIG. 3 shows a part of a non-sacrificial mould 20 used to fabricate a catalyst carrier 1.
  • the mould 20 has an array of cylindrical indentations 21 formed in a mould surface 22 and is provided with a peripheral wall 23 which bounds and defines the edge of the mould surface 22 (only one wall 23 being shown for the sake of clarity).
  • the mould surface 22 of the mould 20 is delimited at points along its length by transverse walls 24.
  • the mould 20 may be fabricated from oil-filled Nylon 6 or MoS 2 -filled Nylon 6, both of which may be supplied by Bay Polymers of North Shields, United Kingdom, under the registered trademarks Nyloil and Nylatron respectively.
  • the material is machined to provide the desired configuration and shape of mould surface 22.
  • a modified tape-casting apparatus may be used, as shown in Figure 4.
  • a slurry or dispersion of a ceramic material in a medium is provided in a slurry mixing system 51 and a slurry delivery system 52.
  • the medium also comprises a polymerisable monomeric species and may comprise a catalyst material to provide the catalytic action for the carrier.
  • An in-line mixer 53 mixes an initiator and polymerization catalyst into the slurry 54 as it passes through or along the slurry delivery system 52.
  • the in-line mixer 53 is provided immediately upstream of a doctor blade 55 which spreads the dispersion 54, with added initiator and polymerization catalyst, onto a mould
  • the mould 20 is formed as a continuous belt-type mould and the doctor blade 55 continuously applies the dispersion directly to the mould surface 22 as it passes the blade.
  • the green form is then shaped to the required shape, two of which are shown in Figures 5 and 6.
  • the green form 30 is formed into a roll 31 and, in the latter, the green form 40 is stacked with other green forms to provide a stack of sheets 41.
  • the stack may allow co-current, counter-current or cross-flow configurations.
  • the form of the upper surface of the mould ensures that there are gaps, and hence flow channels, between adjacent surfaces.
  • the shaped green forms 30, 40 are then dried at either room temperature or at elevated temperatures followed by binder burnout (at, say, 200 to 700 0 C) followed by sintering (at, say, 500 to 1600 0 C).
  • pore formers such as olivestone, almond shell powder, polymeric thermoplastics spheres and so on may be provided in the dispersion to provide corresponding macroporous voids in the sintered material.
  • the main requirement is that the pore-formers do not affect or react with any catalyst which is provided in the dispersion or leave any residues which would or could likewise affect the catalyst.
  • a mould was prepared by drilling 5mm diameter holes about 5mm deep into a thermoplastic part.
  • the holes are arranged as shown in Figure 3.
  • a slurry of the following composition was prepared by thorough mixing (parts in weight) • fine alumina powder (average particle size 0.5 ⁇ m) 75;
  • ammonium acrylate dispersant 2.5 • ammonium acrylate dispersant 2.5.
  • a 30ml slurry batch 1mJ! of 25% ammonium persulphate solution (initiator) and 50 ⁇ l of N, N, N', N'-tetramethylethylenediamine (catalyst) are mixed into the slurry and cast onto the mould surface to a height of about 1-2 mm.
  • the slurry gels within about 1 minute and the gelled green form is peeled off of the mould and rolled into a cylinder shape, as shown in Figure 5. It is then dried and fired to 152O 0 C for 2 hours.
  • the shape formed in this way is very strong and has a dense body (micro density >90%).
  • a slurry was prepared as per Example 1 , with the exception that 10 parts of olivestone powder (-100 mesh) was added to the slurry as a pore former.
  • the rolled cylinders were fired to 135O 0 C for 2 hours.
  • the measured pore volume of the micro-pores is 0.2 ml/g, equivalent to a 45% micro- porosity.
  • Example 4 A slurry was prepared as per Example 1 , with the exception that instead of 75 parts of the disclosed fine alumina powder, only 70 was added. A further 5 parts of coarser alumina (average particle size 6 ⁇ m) was added as well as 13 parts of olivestone powder (-100 mesh). The rolled cylinders were fired to 132O 0 C for 2 hours. The measured micro- porosity is 0.25 ml/g, equivalent to a 50% micro-porosity.
  • Example 4 A slurry was prepared as per Example 1 , with the exception that instead of 75 parts of the disclosed fine alumina powder, only 70 was added. A further 5 parts of coarser alumina (average particle size 6 ⁇ m) was added as well as 13 parts of olivestone powder (-100 mesh). The rolled cylinders were fired to 132O 0 C for 2 hours. The measured micro- porosity is 0.25 ml/g, equivalent to a 50% micro-porosity.
  • Example 4 A slurry was prepared as per Example 1 , with the
  • a slurry was prepared as per Example 3 but instead of 13 parts of (-100 mesh) olivestone 8 parts of olivestone (-100 mesh) and 10 parts of olivestone (-100, +125 mesh) are added to form a bi-modal pore structure.
  • Two sets of rolled cylinders were made with the slurry and were fired to 132O 0 C and 135O 0 C respectively.
  • the measured micro-pore volumes were 0.36 and 0.30 ml/g respectively, equivalent to 58% and 54% micro-porosity.
  • the so-formed catalyst carriers were found to be suitable as catalyst carriers in steam reforming, autothermal reforming, partial oxidation, or in other fixed bed reactors involving endothermic or exothermic reactions.
  • the carriers may be used in heat exchangers, filters, catalytic filters and so on, as will be appreciated by the skilled man.
  • the catalyst carriers were found to show much increased surface area and a lower pressure drop than other catalyst carriers known in the art. Specific geometric areas and measured pressure drops of the catalyst carriers made according to Example 1 are compared with various catalyst carriers in Table 1. Table 1
  • Catalyst carriers made in the same manner as Example 1 but with different mould formations. On one surface there are random channels of 0.3mm width and depth. Green form thickness about 1mm, carrier size 16mm diameter and 16mm length;
  • Example 1 Comparing with the spheres of the same diameter the specific geometric surface area of the catalyst carriers given in Example 1 is almost 3 times as high and the sample with finer formations (No.5 in Table 1) has a specific area of 7 times as that of the equivalent spheres.
  • the pressure drop in the case of Example 1 is only about half of that of the spheres.
  • the pressure drop data given in Table 1 were measured in a 64mm diameter 140mm length miniature reactor with nitrogen as the flow medium. Flow rate was fixed at 30i.min "1 .
  • the green form tapes formed using the tape casting apparatus may be combined with other catalyst tapes made using the apparatus (or otherwise) to provide a dual (or multi) purpose catalyst carrier. For example, tapes of different compositions may be rolled or stacked together to provide a catalyst carrier having a combined physical and/or catalytic properties of the tapes.
  • the mould need not be of a continuous belt-type mould and may be any suitable mould surface.
  • the form and pattern of the formations therein or thereon may be any chosen for a particular task, for example the indentations may be shaped to provide a carrier having hemispherical projections, elongate, curved or other shaped projections.
  • the carrier is formed from a non catalytic ceramic material (i.e. a ceramic material having no or little catalytic activity)
  • a catalytic material may be coated, impregnated and/or deposited over some or all of the shaped surface of the carrier either prior to or after binder burnout and final sintering.
  • the invention can offer the possibility of ceramic microchannel heat exchangers or chemical reactors for high and low temperature applications for liquid and gaseous feeds or a combination of both.
  • Other applications include absorption of gases in liquids in co-current and counter current flow systems.
  • the polymersible monover may be pre-mixed with an initiator and the pre-mix solution added to the ceramic material.

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Abstract

La présente invention concerne un procédé permettant de fabriquer un support catalytique, lequel procédé consiste à former une boue de particules de céramique dans un support liquide, lequel support comprend une espèce de liant; à appliquer la dispersion sur la surface d'un moule non sacrificiel présentant des formations dessus et à l'intérieur; à permettre au liant de sécher de manière à obtenir une ébauche; à retirer l'ébauche de la surface du moule; à sécher et à cuire l'ébauche. La durée du séchage du liant qui permet d'obtenir l'ébauche est, de préférence, inférieure à 120 minutes. Cette invention concerne également des supports catalytiques ainsi qu'un dispositif de coulée en bande permettant de réaliser de tels supports catalytiques.
PCT/GB2005/003472 2004-09-10 2005-09-08 Catalyse Ceased WO2006027593A2 (fr)

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GB0420156A GB2417921A (en) 2004-09-10 2004-09-10 A method of fabricating a catalyst carrier
GB0420156.2 2004-09-10

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