WO1993011087A1 - Structure pour un filtre ou un echangeur de chaleur et procede de fabrication de la structure - Google Patents

Structure pour un filtre ou un echangeur de chaleur et procede de fabrication de la structure Download PDF

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Publication number
WO1993011087A1
WO1993011087A1 PCT/US1992/010203 US9210203W WO9311087A1 WO 1993011087 A1 WO1993011087 A1 WO 1993011087A1 US 9210203 W US9210203 W US 9210203W WO 9311087 A1 WO9311087 A1 WO 9311087A1
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WO
WIPO (PCT)
Prior art keywords
support
fluid
porous
ceramic
end caps
Prior art date
Application number
PCT/US1992/010203
Other languages
English (en)
Inventor
John R. Moyer
Neal N. Hughes
Original Assignee
The Dow Chemical Company
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
Priority claimed from US07/803,292 external-priority patent/US5198007A/en
Priority claimed from US07/803,296 external-priority patent/US5194154A/en
Application filed by The Dow Chemical Company filed Critical The Dow Chemical Company
Priority to EP92925418A priority Critical patent/EP0615519A1/fr
Priority to JP5510245A priority patent/JPH07501783A/ja
Publication of WO1993011087A1 publication Critical patent/WO1993011087A1/fr

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Classifications

    • 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
    • B01D46/2476—Monolithic structures
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
    • B01D29/11—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with bag, cage, hose, tube, sleeve or like filtering elements
    • B01D29/31—Self-supporting filtering elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
    • B01D29/11—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with bag, cage, hose, tube, sleeve or like filtering elements
    • B01D29/31—Self-supporting filtering elements
    • B01D29/35—Self-supporting filtering elements arranged for outward flow filtration
    • B01D29/356—Self-supporting filtering elements arranged for outward flow filtration open-ended, the arrival of the mixture to be filtered and the discharge of the concentrated mixture are situated on both opposite sides of the filtering element
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
    • B01D29/50—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with multiple filtering elements, characterised by their mutual disposition
    • B01D29/52—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with multiple filtering elements, characterised by their mutual disposition in parallel connection
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2068—Other inorganic materials, e.g. ceramics
    • B01D39/2072—Other inorganic materials, e.g. ceramics the material being particulate or granular
    • B01D39/2075—Other inorganic materials, e.g. ceramics the material being particulate or granular sintered or bonded by inorganic agents
    • 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
    • B01D46/0039—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with flow guiding by feed or discharge devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
    • B01D63/06—Tubular membrane modules
    • B01D63/066—Tubular membrane modules with a porous block having membrane coated passages
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0039—Inorganic membrane manufacture
    • B01D67/0041—Inorganic membrane manufacture by agglomeration of particles in the dry state
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0039—Inorganic membrane manufacture
    • B01D67/0041—Inorganic membrane manufacture by agglomeration of particles in the dry state
    • B01D67/00411—Inorganic membrane manufacture by agglomeration of particles in the dry state by sintering
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0039—Inorganic membrane manufacture
    • B01D67/0046—Inorganic membrane manufacture by slurry techniques, e.g. die or slip-casting
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/10—Supported membranes; Membrane supports
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/10—Supported membranes; Membrane supports
    • B01D69/107—Organic support material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/02—Inorganic material
    • 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 monoliths
    • 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
    • C04B35/16—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
    • 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
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/0006—Honeycomb structures
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28—HEAT EXCHANGE IN GENERAL
    • F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
    • F28F21/00—Constructions of heat-exchange apparatus characterised by the selection of particular materials
    • F28F21/04—Constructions of heat-exchange apparatus characterised by the selection of particular materials of ceramic; of concrete; of natural stone
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2201/00—Details relating to filtering apparatus
    • B01D2201/46—Several filtrate discharge conduits each connected to one filter element or group of filter elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/04—Additives and treatments of the filtering material
    • B01D2239/0471—Surface coating material
    • B01D2239/0478—Surface coating material on a layer of the filter
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/10—Filtering material manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2323/00—Details relating to membrane preparation
    • B01D2323/08—Specific temperatures applied
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2323/00—Details relating to membrane preparation
    • B01D2323/08—Specific temperatures applied
    • B01D2323/081—Heating

Definitions

  • This invention relates generally to a ceramic structure for filtering of, or heat exchange between, fluids, either liquids or gases.
  • Ceramic filter media are commonly used in a wide range of fluid handling procedures, including filtration, diffusion, recovery, transfer, mixing and foaming. Ceramic
  • filter media are also employed as catalysts themsel es, or as carriers for catalysts. Ceramics possess several advantages as media for fluid handling over alternatives such as organic or metallic filter media. One advantage is a superior resistance to deterioration from heat or chemical exposure.
  • Ceramic filter media are most often used in the form of an aggregation of .. ceramic particles, either loose or bound to one another.
  • the ceramic particles can be formed as spheres, platelets or needles.
  • the particles are routinely obtained by crushing and classifying (that is, sorting by size) a previously manufactured mass of the desired material. This method of manufacture is subject to some drawbacks, however. Crushing a formed material can degrade some desirable structural characteristics of the material, such as its impact strength,
  • Ceramic filter media have also been used as supports for discriminating layers such asfluorocarbon polymers or sintered ceramic membranes. These supports have typically been made from previously fired spherical particles of alpha-alumina ( ⁇ -A ⁇ O.) orcordierite. The particles have then been lightly sintered to bond them together and give them mechanical strength. Unfortunately, many of the resulting supports did not have possess sufficient strength, particularly against impact or against the pressure of fluid flowing through them. The resulting supports typically had a porosity of no more than about 30% (or 70% of theoretical density, defined as 100% minus the volume% porosity).
  • JP 63-103877A discloses a process for preparing a porous ceramic compact that may be useful for industrial filtering.
  • the compact is described as having fine porous structure with a relatively high deflection strength.
  • the compact consists of acicular mullite crystals formed by compression molding and sintering of stoichiometric mullite (3 A! 2 ⁇ 3-2Si ⁇ 2)-
  • the starting material includes additives so as to allowthe transfer of any unreacted or excess silica into a glass phase, which is then eluted with an acid such as hydrofluoric acid (HF). Acids such as HF require special handling procedures and degrade or attack any metal that may be used in a device.
  • HF hydrofluoric acid
  • U.S.-A 3,993,449 discloses a process for preparing single crystal mullite fibrils useful as fillers, catalysts, or catalyst supports.
  • the fibrils are made from aluminum suifate, a silica (Si0 2 ) source and an alkali metal salt (fluxing agent).
  • U.S.-A 4,894J60 discloses a honeycomb structure for fluid filtration.
  • the structure comprises a porous ceramic support having a multiplicity of parallel passageways formed through it by uniformly spaced porous partition walls.
  • the passageways permit pressurized fluid to flow through the support.
  • a selective membrane is coated onto the surface of the passageways to separate one or more components from the fluid.
  • the filtrate is carried through the partition walls to the exterior surface of the partition walls for collection.
  • the honeycomb structure is preferably contained within a cylindrical casing and held in place by a pair of support plates near the ends of the ceramic support element.
  • the external surface of the partition walls between the support plates is coated with a glaze, to direct the flow of filtrate into the discharge port.
  • the filter structure should be prepared by a process that avoids hazards associated with handling acids such as HF.
  • the process should also include a method for interlocking two or more pieces into a ceramic o body that has a uniform composition and structure. The uniform composition and structure should continue including throughoutthe locations pieces of the structure are joined. Disclosure of the Invention
  • One aspect of the present invention is a structure for filtering a fluid or for exchanging heat or a constituent or contaminant between two fluids passing through the 5 structure, comprising: a body composed of a fused, interlocked, single crystal acicular ceramic material, the body having porous partition walls defining at least one open channel extending entirely through the body; and means for collecting fluid exiting the body through the partition walls.
  • the body is preferably a honeycomb extrusion of porous partition walls that define a plurality of open parallel channels in fluid communication with one another. Any fluid not passing through the porous partition walls exits the body unhindered, through the open channel(s).
  • the means for collecting fluid exiting through the partition walls can include an impermeable coating, such as a glaze, substantially covering the exterior of the body so as to define an exit for the exiting fluid.
  • the structure can further comprise a membrane disposed on the partition walls, thereby lining the open channel(s).
  • the membrane can be a porous discriminating layer of sintered ceramic, a polymeric organic compound, a molecular sieve, a gel filtration, gel, or a microporous gaseous diffusion barrier. This makes the structure useful for cross-flow filtration.
  • the sintered ceramic material is desirably sintered C1-AI2O3.
  • the membrane can be impermeable, preventing a first fluid passing through the channels from mixing with a second fluid passing through the partition walls. This makes the structure useful for heat exchange between the fluids.
  • the structure can include a pair of porous end caps composed of the same acicular ceramic material as the body.
  • the end caps preferably abut and interlock with the partition walls.
  • Each end cap preferably includes a hole therethrough in fluid communication with the open channels.
  • Each end cap also preferably includes at least one recess that extends from the end cap external surface remote from, rather than proximate to, the partition walls only partway through the end cap.
  • the holes provide an entrance and exit for a fluid to pass through the open channels, while the recesses provide for eitherthe exit, orthe entrance and exit, of fluid passing through the porous partition walls.
  • the holes and recesses preferably have axes that parallel those of the open channels.
  • the collecting means can then include a pair of connecting tubes received in the end cap recesses to directthe flow of filtrate exiting the porous walls and end caps.
  • Another pair of connecting tubes can be received in the end cap holes to directthe flow of fluid into and out of the open channels in the ceramic body.
  • the body is desirably composed of non-stoichiometric acicular mullite, preferably of 76 percent by weight Al 2 0 3 and 24 percent by weight Si ⁇ 2-
  • the body is preferably formed as a honeycomb extrusion of plural parallel channels.
  • the body desirably further comprises plugs of porous, non-stoichiometric, acicular mullite that are disposed in, and interlocked with, single, alternating ends of the channels.
  • the body is preferably from 50 to 85 percent porous.
  • a second aspect of the present invention is a method of forming a structure useful for filtering a fluid or for exchanging heat or a constituent between two fluids passing through the structure, comprising the steps of: forming a green support composed of a ceramic material capable of being converted in situ into fused, interlocked, single crystal, acicular ceramic particles; converting said ceramic material in situ into such particles, thereby forming a rigid and porous ceramic support; and applying a membrane layer on at least part of the support.
  • the membrane layer is impermeable for heat exchanger applications and permeable forfiltering applications.
  • the green support is preferably a honeycomb extrusion having a plurality of open, parallel channels defined therein.
  • the support is desirably formed by abutting together at least two green support pieces, such as a honeycomb extrusion and either porous plugs or end caps or both.
  • Each piece is composed of a non-stoichiometric mixture of AI2O3 and Si ⁇ 2- The pieces become interlocked with each other when they are converted to acicular mullite.
  • a permeable membrane layer is desirably formed in two steps. First, at least one surface of the porous ceramic support, preferably surfaces of the open channels in a honeycomb extrusion, is coated with a slurry of C1-AI2O3. In the second step, the support and the -1-AI2O3 are sintered after removal of excess slurry. This provides a thin, continuous membrane of porous ⁇ -AI 2 03 on the surface of the support.
  • An impermeable layer may be formed in a similarmanner using a suitable material.
  • FIGURE 1 is a partial cut away side view of a structure prepared in accordance with the present invention
  • FIGURE 2 is a cross-sectional view taken along line 2-2 of Figure 1 showing how the end of the structure is cut to place outlet channels and inlet channels in fluid communication, respectively, with other outlet channels and inlet channels;
  • FIGURE 3 is a partial cross-sectional view similarto Figure 1 , more clearly showing the flow of fluid therethrough and the ⁇ -Al 2 03 or other membrane coating part of the interior of the structure;
  • FIGURE 4 is a cross-sectional view of a cross- flow filter incorporating the structure of the present invention.
  • FIGURE 5 is a cross-sectional view taken along line 5-5 in Figure 4
  • FIGURE 6 is a cross-sectional view taken along line 6-6 in Figure 4;
  • FIGURE 7 is an end view of a ceramic support used in making the cross-flow filter shown in Figure 4 disclosing how the end of the support is cut so as to yield the structure shown in Figure 6;
  • FIGURE 8 is an enlarged, partial cross- sectional view of the cross-flow filter of Figure 4, showing the flow of fluid through open filter channels and through porous support walls that define the open channels.
  • Filter 10 is useful for removing an entrained contaminant from a fluid, for example, for removing insoluble organic material from an aqueous slurry.
  • Filter 10 comprises a support 1 1 composed of a fused single crystal acicular ceramic of interlocked needles, whiskers or platelets (collectively, "whiskers” or “acicular particles”).
  • Support 1 1 is distinguished from prior supports because it is composed of individual acicular ceramic particles that are rigidly interlocked at the locations where they cross rather than merely being interwoven as in prior supports.
  • the conversion of the ceramic into fused and interlocked acicular particles occurs in situ.
  • the fusion and interlocking of the whiskers yields a support that, in comparison to prior supports formed from preformed, lightly bonded whiskers, possesses significantly improved structural strength and resistance to high temperatures.
  • the acicular ceramic material is preferably a non-stoichiometric acicular mullite composed of about 76 percent by weight (wt-%) Al 2 0 3 and 2 wt-% Si0 2 .
  • Other ceramic materials that are capable of forming fused, interlocking, single crystal, acicular structures upon in situ formation are also useful. Such other ceramic materials are believed to include aluminum borate whiskers, alumina whiskers and ⁇ -AI 2 03 platelets, or other materials sharing these characteristics.
  • Support 1 1 can be formed in any of a variety of conventional shapes, including a disk, a barrel, a tube, a dead-end body, or a cross-flow body. Support 1 1 can also be formed into more complex shapes than prior filter supports. Support 1 1 can be a single piece or be formed from a plurality of pieces having a uniform composition and structure. Uniformity of composition is especially desirable through locations where pieces are joined together. The shape of support 1 1 should be appropriate for the function desired of the structure incorporating the support.
  • support 11 can be configured as a honeycomb extrusion for either a dead-end or cross-flow filter. In the dead-end configuration, half of the holes at each end of the honeycomb are plugged in a checkerboard arrangement.
  • honeycomb support shape is shown in U.S.-A 5,098,455.
  • support 11 comprises a honeycomb extrusion 12 having a 10 fluid inletend 14 and a fluid outlet end 16.
  • a pluralityof longitudinally extending inlet channels 18and parallel longitudinally extending outlet channels 20 extend from fluid inlet end 14to fluid outlet end 16.
  • Inlet channels 18 are formed by plugging their downstream ends adjacent outlet end 16 with downstream plugs 22.
  • Outlet channels 20 are formed by plugging their upstream ends adjacent inlet end 14 with upstream plugs 23. 15
  • the honeycomb extrusion 12 is allowed to dry to a self-sustaining green body. As more clearly shown in Figure 2, alternating single holes at opposing ends of inlet channels 18and outlet channels 20 are then plugged in checkerboard fashion.
  • Plugging occurs with green plugs 22 and 23 made of a paste of the same composition as honeycomb extrusion 12.
  • plugs 22 and 23 may possess the same amount of filler as the 20 composition making up extrusion 12.
  • it is preferred for handling purposes that green plugs 22 and 23 have a higher porosity than extrusion 12, for example, typically on the order of 70 % (30 % theoretical density). This higher porosity is achieved by mixing more filler or water with the mixture of alumina and either clay or silica.
  • Support 11 also comprises an inlet end cap 26 that is attached to inlet end 14 of honeycomb extrusion 12.
  • Inlet end cap 26 has a hole 28 formed through it, in fluid 5 communication with inlet channels 18 through spaces provided by saw cuts 24.
  • the surfaces of downstream plugs 22 and inlet channels 18, together with the interior surface of inlet end cap 26, define an inlet chamber 36 within filter 10.
  • Support 11 further comprises an outlet end cap 30 that is attached to outlet end 16 of honeycomb extrusion 12.
  • Outlet end cap 30 has a hole 32 (shown in Figure 3) formed through it, in fluid communication with outlet channels 20 through spaces provided by saw cuts 24.
  • the exterior of honeycomb extrusion 12, inlet end cap 26 and outlet end cap 30 are substantially covered with a fired glaze layer 34 (except for the inlet and outlet holes 28 and 32). Layer 34 is impermeable to, and nonreactive with, the fluid to be treated and its entrained contaminants.
  • filter 10 comprises a porous discriminating layer 38 on at least part of support 11.
  • Discriminating layer 38 is preferably disposed on the surfaces of downstream plugs 22, inlet channels 18, and the interior surface of the inlet end cap 26 that define inlet chamber 36.
  • Discriminating layer 38 is preferably a sintered ⁇ -AI 2 0 3 membrane. It can, however, be any conventional layer suitable for filtration, microfiltration, ultrafiltration (for example, sterilization, or purification of crystals), reverse osmosis (for example, desalination of sea water), or gas separation.
  • Classes of materials useful for discriminating layer 38 include sintered ceramics (of which C1-AI2O3 is an example), polymeric organic compounds, molecular sieves, gels, and microporous or ultraporous gaseous diffusion barriers.
  • Moiecular sieves include both zeolites and crystalline aluminophosphates derived from mixtures containing an organic amine or a quaternary ammonium salt.
  • Gels are simply those gels (such as dextran gels) that are useful in gel filtration.
  • Polymeric organic compounds include hydrocarbon, halogenated hydrocarbon, fluorocarbon, and chlorofluorocarbon resins and polymers, such as polytetra- fluoroethylene (PTFE), tetrafluoroethylene/hexafluoropropylene copolymer (FEP), tetrafluoroethylene/perchloro-alkylvinylether copolymer (PFA), polychlorotrifluoroethylene (PCTFE), polyvinyl- difluoride (PVDF), polypropylene resin, and polyvinylchloride resin.
  • PTFE polytetra- fluoroethylene
  • FEP tetrafluoroethylene/hexafluoropropylene copolymer
  • PFA tetrafluoroethylene/perchloro-alkylvinylether copolymer
  • PCTFE polychlorotrifluoroethylene
  • PVDF polyvinyl- difluoride
  • polypropylene resin and polyviny
  • the foregoing materials suitably provide, either singly or in combination, pore sizes within a useful range of 0.5 nanometers (nm) to 50 micrometers ( ⁇ m).
  • the material(s) chosen for discriminating layer 38 should also be compatible with the material of support 1 1.
  • Discriminating layer 38 can be formed by any fabrication process and any constituents that yield a layer useful for its intended purpose.
  • U.S. -A 4,874,516 discloses a method for applying a PTFE membrane filter to a ceramic substrate so as to permeate the surface layer of the substrate.
  • the substrate and PTFE are heat-treated to yield a supported membrane of a high polymer resinous material having a useful pore size as small as about OJ ⁇ m for ultra- or semiultra-filtration.
  • Appropriate fabrication processes for membranes of other materials are well known, and can be adapted for use in the present invention without undue experimentation.
  • fluid enters filter 10, as shown by unlabeled arrows in Figure 3, through inlet hole 28 and passes, via the inlet chamber 36, through discriminating layer 38 and the walls of honeycomb extrusion 12, into outlet channels 20.
  • the permeate fluid exits filter 10 through outlet hole 32.
  • cross-flow filter 100 comprises a body 1 11.
  • Body 111 is preferably composed of the same fused single crystal whiskers as support 11 of structure 10. Like support 11, body 111 can be a single piece or be formed from a plurality of pieces of uniform composition.
  • Body 1 11 is suitably configured as a honeycomb extrusion 1 13 having a number of continuously formed partition walls 1 12.
  • Walls 1 12 define a plurality of parallel open channels 114 that extend entirely through body 111.
  • Open channels 1 14 define a path for the flow of a first fluid through body 11 1.
  • open channels 1 14 are preferably circular in cross section, although they may have any convenient or desired cross-sectional shape.
  • All open channels 1 14 are preferably in fluid communication with one another. Fluid communication can be established in a variety of ways. One way includes positioning a hollow dome over each end of extrusion 1 13 so that all channels are open to the hollow dome. A preferred way is to form a plurality oftransverse clear openings 116 through partition walls 112. Openings 116 are desirably positioned at opposing ends of the open channels 114. Openings 116 are preferably recesses or channels formed by cuts that extend fully across the ends of extrusion 113 and intersect open channels 114. More particularly, as shown in Figure 7, when open channels 114 are arranged in a closest-packed (hexagonal) fashion, the cuts are made along every other row of open channels 1 14 in each of the three directions in which the rows run.
  • the cuts also known as saw cuts, can be made in any convenient fashion. They are usually made before extrusion 1 13 is converted into the preferred single crystal acicular ceramic.
  • One way to make the cuts is to draw a thread, wetted with water, across the ends of the extrusion 113 longitudinally in the directions of arrows A, B, and C.
  • Figure 6 shows howan end of extrusion 113 looks after the cuts are made.
  • body 11 1 further comprises a pair of porous end caps 118 that abut opposing ends of extrusion 113.
  • End caps 118 are preferably in physical contact with the ends of porous partition walls 1 12.
  • Each end cap 118 includes a hole 120 that extends fullythrough end cap 118 and is in fluid communication with open channels 1 14.
  • Each end cap 118 also includes a recess 122 that extends only partway through end cap 1 18 and is spaced apart from, and opposed to, partition walls 1 12Jn otherwords, recesses 122 do not communicate directly with open channels 1 14.
  • End caps 118 are desirably composed of the same single crystal acicular material as partition walls 112.
  • End caps 1 18 are also desirably interlocked with walls 122.
  • the material is preferably non-stoichiometric acicular mullite.
  • a first connecting tube 124 is received in, and operatively connected to, each end cap hole 120.
  • the first connecting tubes 124 fluidly communicate with all of the open channels 114, preferably by wayof openings 116. As such, they define a means for directing the flow of a first fluid from one first tube 124, into, through and out of the open channels 114, and through the other first tube 124.
  • First connecting tubes 124 can be made of a ceramic and may be co-fired with the conversion of body 1 1 1 to the preferred single crystal acicular ceramic.
  • First connecting tubes 124 are preferably made of, or coated with, a material that is impermeable to the fluids being handled.
  • Second connecting tubes 130 and 131 are received in, and operatively connected to, end cap recesses 122 of opposing end caps 1 18.
  • Second connecting tubes 130 and 131 are, I ike first connecting tubes 124 preferably made of, or coated with, a material that is impermeable to the fluids being handled.
  • An impermeable coati ng 134 substantially covers the exterior of the body 1 1 1 , 0 except for holes 120, recesses 122, and the open ends of connecting tubes 124, 130 and 131. Coating 134 may extend partway along connecting tubes 124, 130 and 131 in order to assure a good seal to body 1 1 1. Coating 134, preferably together with either of second connecting tubes 130 or 131 , defines a means for collecting fluid exiting body 1 1 1 through partition walls 1 12. The exiting fluid can be a second fluid supplied to filter 100, a filtrate derived from the 5 first fluid, or a combination of both. Similarly, coating 134, second connecting tubes 130 and 131 and end caps 1 18 define a means for directing the flow of the second fluid into, through, and out of partition walls 1 12.
  • the means for collecting fluid exiting body 1 1 1 is preferably formed integrally with body 1 1 1.
  • the collecting means and body 1 1 1 1 constitute a single piece. o This does not mean that the collecting means and body 1 1 1 are composed of the same material. To contrary, the body 1 1 1 1 is porous, while the collecting means is impermeable.
  • the integral formation of the collecting means and body 11 1 is most conveniently carried out by making coating 134 an impermeable glaze fired on exterior surfaces of body 1 1 1. Coating 134 is desirably formed from the same material as fired glaze layer 34 of structure 10.
  • porous partition walls 1 12 that define open channels 1 14, as well as any surfaces of end caps 1 18 exposed to the first fluid flowing through open channels 1 14, are preferably coated with a membrane 126 so as to line channels 1 14.
  • membrane 126 is a porous discriminating layer 128.
  • Discriminating layer 128 is preferably formed from the same classes of materials as discriminating layer 38 of structure 10. The use of cross-flow filter 100 is straightforward, as shown in Figure 8.
  • a flow of a first fluid is established through open channels 1 14 by supplying the first fluid through either of first connecting tubes 124 and withdrawing it through the other.
  • the flow of the first fluid is generally designated by long arrows 136.
  • a flow of a second fluid is established through porous walls 1 12 and porous end caps 118, preferably in a direction opposite to the flow of the first fluid.
  • the second fluid may be supplied by and withdrawn, respectively, through second connecting tubes 130 and 131.
  • the flow of the second fluid is generally designated by short, tailless arrows 138.
  • Impermeable coating 134 collects and directs the flow of the second fluid.
  • the transfer of a contaminant or constituent across membrane 126 is generally designated by short, tailed arrows 140. The flow ofthe contaminantor constituent is thereafter concurrent with the flow of the second fluid.
  • second connecting tubes 130 and 131 are merely a matter of convenience. Indeed, to save costs during assembly, end caps 118, first connecting tubes 124 10 and the second connecting tubes 130 and 131 are preferably composed as identical units. The use of body 1 1 1 in devices other than cross-flow filter 100 is also straightforward.
  • body 111 is useful in a heat exchanger for exchanging heat between two preferably opposed fluid flows.
  • the construction of such a heat exchanger is identical to that of cross-flow filter 100, except forthe specific nature of membrane 126.
  • membrane 126 of a heat exchanger must be an impermeable layer. Many such impermeable layers are known and would be useful in the practice of the present invention.
  • an impermeable membrane 126 can be made thinner than past dividing 0 walls or septa for heat exchange.
  • Q Body 111 is also useful in a simple filter, presenting generally unimpeded flow of a fluid through open channels 1 14, but having a cross-flow ofthe filtrate.
  • the construction of such a filter can be identical to that of filter 100, except that membrane 126 is only optionally applied to porous walls 1 12.
  • the flow path through the simple filter is essentially the same as that of the cross-flow filter 100, except, of course, that there is no second fluid. Filtrate from the flow ofthe first fluid passes through walls 112 and end caps 118JS collected and directed by impermeable coating 134, and exits the body 111 through either of the second connecting tubes 130 and 131.
  • Filter 10 and cross-flow filter 100 are preferably constructed as follows: a mixture containing AI2O3 and Si0 2 in a molar ratio of about 2 to 1 (an atomic ratio of aluminum to silicon of about 4 to 1) is first prepared.
  • the mixture can be prepared by combining clay and AI2O3, having a net composition of about 76 wt-% AI2O3 and 24 wt-% Si0 2 , the clay and Al 2 0 3 being mixed according to the amount of AI2O3 and Si ⁇ 2 in the clay. All of the foil owing percentages, unless indicated otherwise, are also by weight.
  • Suitable clays typically contain about 35 % Si ⁇ 2 and about 50 % AI 2 ⁇ 3 # so that a typical starting composition prepared from AI2O3 and clay can include about 60 percent clay and about 40 percent Al 2 0 3 .
  • the mixture is advantageously and preferably prepared directly from Al 2 0 3 and fused (amorphous) Si ⁇ 2 powders of high purity.
  • the mixture of AI2O3 and clay or Si0 2 may be blended with a conventional filler for ceramics, such as wood flour or saw dust, and a convenient amount of water for handling.
  • the filler provides porosity to the mixture upon conversion to acicular mullite, for example, by combustion of an organic filler, or by evolution of water from a hydrated form of AI2O3 or Si ⁇ 2-
  • the non-stoichiometric mullite will retain its overall dimensions and its theoretical density upon conversion to its acicular form.
  • the mixture of AI 2 ⁇ 3, filler and either S1O2 or clay is formed into any convenient or desired shape for support 1 1 or body 1 1 1.
  • a first portion of the mixture can be extruded in a honeycomb shape to yield honeycomb extrusions 12 and 1 13.
  • the remainder of the mixture can then be used to form other pieces of support 1 1 or body 1 1 1 in a similar fashion.
  • the theoretical density of support 1 1 and body 1 1 1 1 will vary upon the volume percentage of filler employed in the mixture and the amount of pressure applied during the shape-forming process. Typically, a honeycomb extrusion can be made having sufficient green strength at 40 to 50 % theoretical density. The inclusion of a greater volume percentage of filler allows other shapes to be obtained having theoretical densities as low as 15 %, that is, having 85 % porosity.
  • the shape and theoretical density of support 1 1 and body 1 1 1 are selected to match, respectively, the needs to which filter 10 and cross-flow filter 100 will be put.
  • the shape and theoretical density of support 1 1 and body 1 1 1 are also selected to match, respectively, discriminating layer 38 and membrane 126.
  • Honeycomb extrusion 113 is suitably allowed to dry to a self-sustaining body in the same manner as honeycomb extrusion 12.
  • the open ends of all open channels 1 14 are then placed in fluid communication with each other, preferably by the cuts 16 across said open channel ends, in the diagonal directions shown by arrows A, B and C in Figure 7.
  • End caps 1 18 can be fastened to honeycomb extrusion 1 13 in the same manner as end caps 26 and 30 are fastened to honeycomb extrusion 12.
  • connecting tubes 124, 130 and 131 can be inserted into end cap holes 120 and recesses 122 and co-fired with extrusion 113 and end caps 118.
  • connecting tubes 124, 130 and 131 can be previouslyformed orfired.
  • conversion of end caps 118 desirably affixes connecting tubes 124, 130 and 131 to end caps 118.
  • connecting tubes could also be inserted into holes 28 and 32 of structure 10 and processed or converted in the same manner. The conversion is preferably carried out in such a fashion that extrusions 12 and 113, plugs 22 and 23 in extrusion 12, and their respective end caps retain the same theoretical density or porosity as they possessed in their green state.
  • the conversion preferably occurs in a two step process in which AI2O3 and Si ⁇ 2 in a molar ratio of about 2 to 1 are heated in a closed system at 500° to 950°C in the presence of S ⁇ F4.
  • the AI2O3, Si0 2 and SiF 4 are heated for a time sufficientto react and form fluorotopaz.
  • the resulting fluorotopaz is then heated to a temperature within a range of 800°C to 1500°C, preferably 975° to 1150°C, more preferably 1 100°to 1 150°C.
  • the actual temperature depends upon SiF 4 vapor pressure. A high vapor pressure favors lowertemperatures and a low vapor pressure requires higher temperatures within said range.
  • the fluorotopaz transforms to non- stoichiometric mullite whiskers, with the evolution of all of the SiF 4 previously absorbed.
  • the reaction is preferably conducted in a closed system so the SiF 4 is recaptured and used for subsequent reactions.
  • the temperature can be cycled between these two ranges until SiF ⁇ is no longer absorbed by the material upon cooling down to the lower temperature range.
  • the lack of absorption indicates that no unreacted AI2O3 and Si ⁇ 2 remain inthe mixture.
  • the whiskers forming them fuse and become interlocked in a three dimensional fashion, so as to fixthe plugs end caps steadfastly to their respective honeycomb extrusion.
  • the resulting support 1 1 or body 11 1 is thus composed of a plurality of pieces that are extremely resistant to separation, since they are structurally uniform with and interlocked with each other, even through the locations at which the pieces abut.
  • the source of fluorine can be different from SiF 4 .
  • Materials such as AIF3, HF, a2SiF6, NaF, and NH4F are also expected to be useful for this purpose.
  • the 113 and their respective end caps are preferably coated with any conventional, compatible glaze, and fired.
  • the glaze forms a nonreact ⁇ ve, fluid-impermeable surface, designated as 34 in Figures 1 and 3 and as 134 in Figures 4-6 and 8, over the extrusions 12 and 113 and their respective end caps.
  • the preferred glaze is a mixture of glass frit and clay.
  • One particularly preferred high temperature, commercial glaze for this purpose is sold under the trademark "PEMCO" glaze by Mobay Chemical Company.
  • conventional techniques that render the exterior of honeycombs 12 and 113 and their respective end caps impermeable without a glaze may be used.
  • ⁇ -Al2 ⁇ 3 membrane or other discriminating layer 38 or 128 is then applied, respectively, to the surfaces defining the plurality of inlet chambers 36 of the filter 10 or to the surfaces of porous walls 1 12 that define the plurality of open channels 1 14 of filter 100.
  • Layers 38 and 128 can be applied in any fashion conventional for the application of discriminating layers. Layers 38 and 128 may be formed from any conventional coating so long as the resultant layer possesses a pore size less than the pore size, respectively, of honeycomb extrusions 12 and 113. The layers should also meet the respective service requirements of filters 10 and 100. Although many hydrocarbon polymers, fluorocarbon polymers and ceramics may form satisfactory layers 38 and 128, ⁇ -Al 2 03 is preferred.
  • One advantage of an ⁇ -AI 2 0 3 membrane is that it can be regenerated in filtering operations such as separating insoluble organics from an aqueous slurry. Regeneration occurs by igniting and burning organics trapped on the membrane.
  • Discriminating layers 38 and 128 may include a sintered ceramic layer, such as an C1-AI2O3 membrane having a pore size between 0.15 and 50 ⁇ m, useful for a microfilter. If an ultrafilter is desired, smaller pore sizes may be made as described hereinbelow.
  • An ⁇ -AI 2 03 discriminating membrane may be applied from an aqueous slurry of -1-AI2O3. The slurry typically contains 50 % or more water. The slurry can also include conventional dispersants in order to prevent agglomeration of the ⁇ -Al 2 0 3 powder in the slurry.
  • the slurry can further include an acid or a base in order to adjust the pH of the slurry and improve dispersion of the (1-AI2O3 in the slurry.
  • the slurry can include an agent for controlling the viscosity of the slurry, such as "METHOCEL” (a registered trademark of The Dow Chemical Company, Midland, Michigan, for its brand of methylcellulose).
  • the powdered C1-AI2O3 used to prepare of the membrane is preferably of a high grade of purity. Impurities in the powder affect the range and uniformity of membrane pore sizes.
  • Alcoa Aluminum Corporation and Vista Corporation each sell C1-AI2O3 powders of near 100 % purity that are useful in the present invention.
  • Typical useful grades of Alcoa ⁇ -AI 2 0 3 are grades A-13, A- 16, and A-99.
  • Alcoa grade A-99 powders range in size from 0.15 to 1.0 ⁇ m in diameter, with an average diameter of 0.2 ⁇ m.
  • Grade A-16 ranges from 0.2 to 10 ⁇ m in size, with an average diameter of about 0.4 ⁇ m.
  • Grade A-13 ranges in size from 1 to 50 ⁇ m, with a mean diameter between 5 and 10 ⁇ m. Mixtures of various particle sizes can also be employed in the present invention, to yield any desired pore size in the ceramic membrane.
  • the slurry of powdered ⁇ -Al 2 03 is prepared, it is introduced into the inlet chamber 36 of filter through the inlet hole 28 in the inlet end cap 26, and allowed to coat the surfaces of inlet channels 18, downstream plugs 22, and the interior surface of inlet end cap 26.
  • the slurry is introduced into the cross-flow filter 100 through a first connecting tube 124 and allowed to coat the surfaces of open channels 1 14 and any exposed surfaces of end caps 1 18 within filter 100. Excess slurry is then removed from filter 10 or cross-flow filter 100.
  • the filter, either 10 or 100 is then sintered in order to form a thin, continuous layer of microporous 1-AI2O3.
  • the discriminating layer may also be graded from the highly porous support through an intermediate discriminating layer of microporous material and topped with a layer of ultra- fine porous material, in order to effect more efficient ultrafiltration.
  • membrane 126 is impermeable to the fluids being treated rather than porous. Any of a variety of materials can be used to form impermeable membrane 126.
  • One material is the glaze used for external impermeable coating 136 on body 111.
  • the impermeable membrane is preferably as thin as possible, subject to the strength required of itduring use. Some of the criteria to be considered in assessing the necessary thickness and character of an impermeable membrane include, but are not limited to: high thermal conductivity; low difference in thermal expansivity from that of porous body 1 1 1 ; resistance to deformation under the pressure ofthe fluids to which it is exposed; and resistance to corrosion atthe intended temperature of use. Selection of a particular material and a material thickness for impermeable membrane 126 may be made without undue experimentation.
  • the firing schedules and optimal temperatures for conversion ofthe non- stoichrometric mixture of AI2O3 and Si ⁇ 2 or clay to acicular mullite are subjectto ready determination without undue experimentation.
  • the following heating schedule is convenient:
  • a bisque composed of either assembled green honeycomb extrusion 12, plugs 22 and 23, and end caps 26 and 30 or assembled green honeycomb extrusion 113 and end caps 118 is heated at3"C per minute from room temperature up to 350°C, then at 5°C per minute up to 650°C, and held at that temperature for 60 minutes. The assembly is then heated to 1100 c Cat 5°C per minute, and finally allowed to cool to room temperature at 20°C per minute.
  • the present invention possesses numerous advantages.
  • the interlocked whiskers are bound to each other where they cross, so that a very strong three-dimensional network of o very high porosity is achieved over a wide range of support pore sizes.
  • Relatively large whiskers that are formed in accordance with the present invention yield larger pore sizes than small whiskers.
  • the larger pore sizes allow devices incorporating the present invention to achieve very high flow rates through filters 10 and 100. This advantage is especially important in heat exchangers.
  • the strong network tends to resist flattening under pressure during use, a 5 problem sometimes experienced with conventional Al 2 0 3 or cordierite supports.
  • Perhaps the most significant advantage enjoyed by the present invention, however, is the very economical manner in which ceramic filter supports of a variety of complex shapes can be assembled.
  • the support 1 1 need not be a honeycomb extrusion, but can be any conventional or useful shape, depending upon the environment of filtration or material treatment.
  • Body 1 1 1 disclosed herein is only one example of the variety of shapes a device within the scope of the present invention can take.
  • the present invention therefore provides a filter, a single or dual fluid cross-flow filter or a heat exchanger and a method for maki ng the same that offer numerous advantages.
  • the advantages stem from the high permeability, high mechanical and impact strength, and high thermal resistivity enjoyed by non- stoichiometric acicular mullite and other fused single crystal acicular ceramics that are used as substrates. These characteristics make the present invention useful in a wide variety of environments over an improved range of service temperatures.

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Abstract

Une structure (10 ou 100) utile pour la séparation d'éléments contaminants de fluide ou pour l'échange de chaleur entre deux fluides comprend un support céramique aciculaire monocristal fusionné (12 ou 112) ayant une couche distinctive (38 ou 128) disposée sur au moins une partie du support. Le support possède au moins un canal qui s'étend entièrement à travers le corps. Si la structure est utilisée comme filtre, la couche distinctive est avantageusement une membrane d'alphar-alumine frittée, poreuse ou une autre membrane poreuse. Si la structure est utilisée comme échangeur de chaleur, la couche distinctive est imperméable. Le support se compose de préférence de mullite aciculaire non stoechiométrique. Le support peut avoir une configuration en cul-de-sac ou une configuration à écoulement transversal. La structure peut comprendre des bouchons (22 et 23) pour fermer une extrémité ou l'autre des canaux du support. La structure comprend de préférence des chapeaux (118) sur les extrémités du suppport. Les chapeaux devraient être en céramique similaire à celle utilisée dans le support. Le matériau céramique utilisé dans le support, dans les bouchons et les chapeaux est interverrouillé, ce qui permet de relier les bouchons et les chapeaux au support. Le filtre est de préférence recouvert d'un émaillage sur l'extérieur du support et les chapeaux d'extrémité. Un procédé de fabrication du filtre consiste dans la conversion d'un support céramique vert in situ en des particules céramiques aciculaires, de préférence des barbes. Le procédé comprend de préférence la fixation du support, des bouchons et des chapeaux d'extrémité ensemble en les reliant entre eux par l'étape de conversion.
PCT/US1992/010203 1991-12-05 1992-11-24 Structure pour un filtre ou un echangeur de chaleur et procede de fabrication de la structure WO1993011087A1 (fr)

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EP92925418A EP0615519A1 (fr) 1991-12-05 1992-11-24 Structure pour un filtre ou un echangeur de chaleur et procede de fabrication de la structure
JP5510245A JPH07501783A (ja) 1991-12-05 1992-11-24 フィルターまたは熱交換器に用いられる構造物、並びに該構造物の製造法

Applications Claiming Priority (4)

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US07/803,292 US5198007A (en) 1991-12-05 1991-12-05 Filter including a porous discriminating layer on a fused single crystal acicular ceramic support, and method for making the same
US803,296 1991-12-05
US803,292 1991-12-05
US07/803,296 US5194154A (en) 1991-12-05 1991-12-05 Structure for filter or heat exchanger, composed of a fused single crystal acicular ceramic

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WO2008061847A1 (fr) * 2006-11-24 2008-05-29 Robert Bosch Gmbh Composition pour la fabrication d'un matériau céramique, contenant des nanoparticules formant des pores
EP2324921A1 (fr) * 2009-11-19 2011-05-25 Ibiden Co., Ltd. Structure en nid d'abeille
US9427687B2 (en) 2011-10-11 2016-08-30 Ngk Insulators, Ltd. Ceramic filter
US10391454B2 (en) * 2014-03-28 2019-08-27 Ngk Insulators, Ltd. Monolithic separation membrane structure and method for producing monolithic separation membrane structure
US10406486B2 (en) * 2014-04-18 2019-09-10 Mitsubishi Chemical Corporation Porous support-zeolite membrane composite
US20200346149A1 (en) * 2018-02-02 2020-11-05 Hitachi Metals, Ltd. Water-treating ceramic filter module

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WO2002085814A2 (fr) * 2001-04-23 2002-10-31 Dow Global Technologies Inc. Procede de fabrication d'un filtre monolithique a ecoulement sur paroi

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US4509966A (en) * 1983-05-18 1985-04-09 General Motors Corporation Wall-flow monolith filter with porous plugs
US4519820A (en) * 1982-08-05 1985-05-28 Nippondenso Co., Ltd. Fitter apparatus for purifying exhaust gases
EP0306350A1 (fr) * 1987-09-04 1989-03-08 Ngk Insulators, Ltd. Structure à nid d'abeilles pour la filtration de fluides
WO1990009360A1 (fr) * 1989-02-08 1990-08-23 THE GOVERNMENT OF THE UNITED STATES OF AMERICA, as represented by, THE SECRETARY OF THE DEPARTMENT OF THE NAVY PREPARATION DES TRICHITES DE MULLITE A PARTIR DE POUDRES AlF3, SiO2 et Al2O¿3?
US5098455A (en) * 1990-12-21 1992-03-24 The Dow Chemical Company Regenerable exhaust gas filter element for diesel engines

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US4519820A (en) * 1982-08-05 1985-05-28 Nippondenso Co., Ltd. Fitter apparatus for purifying exhaust gases
US4509966A (en) * 1983-05-18 1985-04-09 General Motors Corporation Wall-flow monolith filter with porous plugs
EP0306350A1 (fr) * 1987-09-04 1989-03-08 Ngk Insulators, Ltd. Structure à nid d'abeilles pour la filtration de fluides
WO1990009360A1 (fr) * 1989-02-08 1990-08-23 THE GOVERNMENT OF THE UNITED STATES OF AMERICA, as represented by, THE SECRETARY OF THE DEPARTMENT OF THE NAVY PREPARATION DES TRICHITES DE MULLITE A PARTIR DE POUDRES AlF3, SiO2 et Al2O¿3?
US5098455A (en) * 1990-12-21 1992-03-24 The Dow Chemical Company Regenerable exhaust gas filter element for diesel engines

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008061847A1 (fr) * 2006-11-24 2008-05-29 Robert Bosch Gmbh Composition pour la fabrication d'un matériau céramique, contenant des nanoparticules formant des pores
EP2324921A1 (fr) * 2009-11-19 2011-05-25 Ibiden Co., Ltd. Structure en nid d'abeille
US9427687B2 (en) 2011-10-11 2016-08-30 Ngk Insulators, Ltd. Ceramic filter
US10391454B2 (en) * 2014-03-28 2019-08-27 Ngk Insulators, Ltd. Monolithic separation membrane structure and method for producing monolithic separation membrane structure
US10406486B2 (en) * 2014-04-18 2019-09-10 Mitsubishi Chemical Corporation Porous support-zeolite membrane composite
US11065586B2 (en) 2014-04-18 2021-07-20 Mitsubishi Chemical Corporation Porous support-zeolite membrane composite and process for producing porous support-zeolite membrane composite
US20200346149A1 (en) * 2018-02-02 2020-11-05 Hitachi Metals, Ltd. Water-treating ceramic filter module
EP3718974A4 (fr) * 2018-02-02 2021-03-17 Hitachi Metals, Ltd. Module de filtration en céramique pour traitement de l'eau
US11712648B2 (en) 2018-02-02 2023-08-01 Proterial, Ltd. Water-treating ceramic filter module

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EP0615519A1 (fr) 1994-09-21

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