WO2004091756A1 - Filtre alveole en ceramique et procede de production correspondant - Google Patents

Filtre alveole en ceramique et procede de production correspondant Download PDF

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Publication number
WO2004091756A1
WO2004091756A1 PCT/JP2004/001763 JP2004001763W WO2004091756A1 WO 2004091756 A1 WO2004091756 A1 WO 2004091756A1 JP 2004001763 W JP2004001763 W JP 2004001763W WO 2004091756 A1 WO2004091756 A1 WO 2004091756A1
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WO
WIPO (PCT)
Prior art keywords
water collecting
ceramic honeycomb
honeycomb filter
fluid
cell
Prior art date
Application number
PCT/JP2004/001763
Other languages
English (en)
Japanese (ja)
Inventor
Tomonori Ito
Tatsuo Baba
Original Assignee
Ngk Insulators, Ltd.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ngk Insulators, Ltd. filed Critical Ngk Insulators, Ltd.
Publication of WO2004091756A1 publication Critical patent/WO2004091756A1/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
    • B01D46/0027—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions
    • B01D46/003—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions including coalescing means for the separation of liquid
    • B01D46/0031—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions including coalescing means for the separation of liquid with collecting, draining means
    • 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
    • B01D46/2425—Honeycomb filters characterized by parameters related to the physical properties of the honeycomb structure material
    • B01D46/24491—Porosity
    • 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
    • B01D46/2425—Honeycomb filters characterized by parameters related to the physical properties of the honeycomb structure material
    • B01D46/2429—Honeycomb filters characterized by parameters related to the physical properties of the honeycomb structure material of the honeycomb walls or cells
    • 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
    • B01D46/2425—Honeycomb filters characterized by parameters related to the physical properties of the honeycomb structure material
    • B01D46/24492—Pore diameter
    • 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
    • B01D46/2425—Honeycomb filters characterized by parameters related to the physical properties of the honeycomb structure material
    • B01D46/24494—Thermal expansion coefficient, heat capacity or thermal conductivity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B01D46/24—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies
    • B01D46/2403—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies characterised by the physical shape or structure of the filtering element
    • B01D46/2418—Honeycomb filters
    • B01D46/2451—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure
    • B01D46/247—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure of the cells
    • 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
    • B01D46/2486—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure characterised by the shapes or configurations
    • 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
    • B01D46/2486—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure characterised by the shapes or configurations
    • B01D46/2488—Triangular
    • 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
    • B01D46/2486—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure characterised by the shapes or configurations
    • B01D46/249—Quadrangular e.g. square or diamond
    • 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
    • B01D46/2486—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure characterised by the shapes or configurations
    • B01D46/2492—Hexagonal
    • 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
    • B01D46/2486—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure characterised by the shapes or configurations
    • B01D46/2496—Circular
    • 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
    • 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
    • C04B38/0009—Honeycomb structures characterised by features relating to the cell walls, e.g. wall thickness or distribution of pores in the walls
    • 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
    • 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
    • C04B2111/00793—Uses not provided for elsewhere in C04B2111/00 as filters or diaphragms

Definitions

  • the present invention relates to a ceramic honeycomb filter and a method for manufacturing the same. More specifically, the present invention relates to a ceramic honeycomb filter capable of effectively preventing a fluid to be filtered and a filtration fluid from staying inside and supplying a high-purity filtration fluid, and a method for manufacturing the same.
  • a ceramic honeycomb filter having cells partitioned by porous partition walls has been used as a filter for solid-liquid separation or gas-solid separation.
  • This ceramic honeycomb filter has better physical strength, durability, corrosion resistance, etc. than organic polymer films used for similar applications. In a wide range of fields such as the field, it is suitably used for removing suspended substances, bacteria, dust and the like in liquids and gases.
  • a large number of parallel-shaped porous bodies formed in the longitudinal direction of the cylindrical porous body were used.
  • a filter membrane 22 having a smaller diameter than the porous body is formed on the inner peripheral surface of the flow path (cell) 21.
  • a slit-like void (water collecting slit) 23 is provided in the longitudinal direction of the porous body, and a flow path (water collecting cell) 21 communicating with the void (water collecting slit) 23 is formed at one end of a 2 a.
  • a flow passage (water collecting cell) whose end is sealed with a clogging member 24 Ritsuto) 2 3 ceramic honeycomb fill evening 2 0 capable of flowing out to the outside via has been proposed (e.g., JP-2 0 0 0 1 5 3 1 1 7 JP).
  • the filtration membrane 22 is formed. This improves filtration performance, and the provision of voids (water collection slits) 23 increases the flow rate.
  • the clogging member 24 that seals the end of the flow passage (water collecting cell) 21a simply has a structure in which the fluid to be filtered is merely a flow passage (water collecting cell) 21a. It was only recognized that it would be enough to prevent intrusion into the interior, and when the clogging member 24 was filled too deeply, the flow passage (collection cell) 21 a was filled Since the clogging member 24 protrudes from the gap (water collection slit) 23 and causes troubles and repairs, it is necessary to reach only the minimum necessary position where the inflow of the fluid to be filtered can be prevented. Was not filled. Therefore, in the flow passage (water collecting cell) 2 la, between the end of the clogging member 24 and the gap (water collecting slit) 23, the portion where the filtered fluid to be discharged stays (the liquid reservoir) 2) 25 were formed.
  • the ceramic honeycomb filter 20 may be periodically cleaned using a chemical solution.
  • the chemical solution used for this cleaning stays in the above-described liquid pool 25 and the ceramic honeycomb film 20 starts cleaning. It was not possible to completely remove the solution, and the accumulated drug solution gradually diffused and contaminated the filtered fluid.
  • the filtration membrane slurry containing a solid component to become the filtration membrane 22 is reduced to a predetermined pressure under reduced pressure.
  • the present invention has been made in view of the above problems, and has a ceramic honeycomb filter capable of effectively preventing a fluid to be filtered and a filtration fluid from staying inside and supplying a high-purity filtration fluid. A method for manufacturing the same is provided.
  • the present invention provides the following ceramic honeycomb filter and a method for manufacturing the same.
  • a plurality of membrane filtration cells serving as flow paths for a fluid to be filtered which are partitioned by a porous partition wall made of ceramics, and a filtration membrane is disposed inside the partition wall;
  • the membrane filtration cell and the water collection cell An outer wall surrounding the outer wall, and a portion separated by a predetermined length from both ends of each of the water collecting cells on the outer wall for allowing the filtered fluid that has passed through the water collecting cell to flow outside.
  • each of the plurality of communication holes formed in the clogging member has a portion having a hole diameter of 20 zm or less.
  • Each of the plurality of membrane filtration cells having a cross section perpendicular to the flow direction of the fluid to be filtered has a circular, elliptical, oval, triangular, quadrangular, pentagonal, hexagonal,
  • each of the plurality of water collection cells having a cross section perpendicular to the flow direction of the filtration fluid is from a circle, an ellipse, an oval, a triangle, a square, a pentagon, a hexagon, and a heptagon.
  • the raw material is extruded to obtain an unsintered filter molded body having a predetermined shape having cells serving as flow paths for the fluid to be filtered and the filtered fluid.
  • An unsintered filter molded body with a water collecting slit is obtained by forming a water collecting slit that penetrates the predetermined cell from one part and communicates with the other part to obtain an unsintered filter molded body with the water collecting slit.
  • a body is filled with a clogging material from each end face of the predetermined cell to the water collecting slit penetrating the predetermined cell to obtain a plugged material-filled unfired filled rubber molded body.
  • the ceramic honeycomb filter of the present invention can effectively prevent the fluid to be filtered and the filtration fluid from staying inside, and can supply the filtration fluid with high cleanliness.
  • FIGS. 1 (a) and 1 (b) are explanatory views schematically showing one embodiment of the ceramic honeycomb filter of the present invention, and FIG. 1 (a) shows a part of the ceramic honeycomb filter.
  • FIG. 1 (b) is a cross-sectional view cut along a plane including the central axis.
  • 2 (a) and 2 (b) are cross-sectional views showing a step of filling a predetermined cell with a plugging material in one embodiment of the method for manufacturing a ceramic honeycomb filter according to the present invention. .
  • FIG. 3 is a cross-sectional view schematically showing a conventional ceramic honeycomb filter.
  • FIG. 4 is a cross-sectional view showing a step of filling a predetermined cell with a plugging material in a conventional method for manufacturing a ceramic honeycomb filter.
  • FIGS. 1 (a) and 1 (b) are explanatory views schematically showing one embodiment of the ceramic honeycomb filter of the present invention, and FIG. 1 (a) is a part of the ceramic honeycomb filter.
  • FIG. 1 (b) is a cross-sectional view taken along a plane including the central axis.
  • the ceramic honeycomb filter 1 of the present embodiment is divided by a porous partition wall 2 made of ceramics, and a filtration membrane 3 is provided therein.
  • a plurality of membrane filtration cells 4 serving as flow paths for the fluid to be filtered, and a plurality of membrane filtration cells 4 which are partitioned by the partition walls 2 and are adjacent to the predetermined membrane filtration cells 4 with the partition walls 2 interposed therebetween.
  • a columnar ceramic honeycomb filter 1 is shown, but the shape of the ceramic honeycomb filter 1 of the present embodiment is not limited to a columnar shape, and is not limited to a central axis.
  • the shape of the cross section in the vertical plane may be a columnar shape such as a quadrangle.
  • the fluid to be filtered flows into the inside of the membrane filtration cell 4 from the end face, and passes through the filtration membrane 3 disposed inside the membrane filtration cell 4.
  • the fluid to be filtered is filtered, and the filtered fluid that has been filtered by the filtration membrane 3 flows into the water collecting cell 5 via the porous partition wall 2 and is collected from the water collecting cell 5 through the water collecting cell 5.
  • the water flows into the water slit 7 and flows out of the water collecting slit 7 formed in the outer wall 6 to the outside.
  • a configuration may be adopted in which a part of the filtration fluid filtered by the filtration membrane 3 does not flow into the water collecting cell 5 from the partition 2 but flows out through the outer wall 6 to the outside.
  • the ceramic honeycomb filter 1 of the present embodiment has a configuration including the water collecting slits 7 so that the water flow resistance is reduced and the ceramic honeycomb filter 1 has excellent water permeability. Also, in a conventional ceramic honeycomb filter provided with a water collecting cell, a portion of the water collecting cell in which the filtered fluid to flow out stagnates between the end of the clogging member and the water collecting slit (liquid reservoir). When some of the filtration fluid stays in the liquid pool, various bacteria and the like propagate and contaminate the entire filtration fluid, and the chemical used for cleaning the ceramic honeycomb filter becomes in the liquid pool.
  • the ceramic honeycomb filter 1 of the present embodiment has a problem that the clogging member 8 Since the space from each end face to the water collecting slit 7 is filled, a portion where the filtration fluid or the chemical solution stays is not formed, and the filtration fluid is not contaminated. No.
  • the fluid to be filtered flows directly from the partition 2 at the end face of the ceramic honeycomb filter 1 and is filtered by the filtration membrane 3 on the inner surface of the membrane filtration cell 4.
  • a seal portion 9 is formed so as to cover the partition 2 at the end face of the ceramic honeycomb fill 1.
  • the seal portion 9 is formed by applying a glaze such as silica glass to the end face of the ceramic honeycomb filter 1 and firing the same.
  • the shape of the ceramic honeycomb filter 1 Is cylindrical, its end face diameter is 180 mm and its axial length is 100 mm, the shape of the opening of the water collecting slit 7 formed in the outer wall 6 is one side
  • the length is 20 to 80 mm, which is oval, square or rectangular.
  • the clogging member 8 is filled in the space from each end face of the water collecting cell 5 to the water collecting slit 7, but in this embodiment,
  • the phrase "filled in the space from each end face of the water collecting cell 5 to the water collecting slit 7" means that the water collecting cell 5 is filled from the viewpoint of accuracy when filling the clogging member 8.
  • the partition wall 2 of the ceramic honeycomb fill 1 is made of, for example, a kneaded clay obtained by mixing an aggregate binder and an inorganic binder with an organic binder such as methylcellulose, a dispersant, and water. It can be formed by extrusion molding with a honeycomb molding machine.
  • a kneaded clay obtained by mixing an aggregate binder and an inorganic binder with an organic binder such as methylcellulose, a dispersant, and water. It can be formed by extrusion molding with a honeycomb molding machine.
  • the aggregate particles at least one compound selected from the group consisting of alumina, mullite, selven, and cordierite can be suitably used.
  • the inorganic binder at least one compound selected from the group consisting of alumina, silica, zirconia, titania, glass frit, feldspar, and cordierite can be suitably used.
  • the same material as that of the partition wall 2 described above can be suitably used, and for example, at least one selected from the group consisting of alumina, mullite, uß, and coalite It is preferably formed from a porous material containing one material.
  • the plugging material (plugging material slurry) used in the manufacturing process includes the plugging member 8 in the ceramics 82 cam filter 1 obtained from each end face of the water collecting cell 5 to the water collecting slit 7. It is preferable to use a material to which a binder, a thickener and a water retention agent are further added so that is filled.
  • the configuration of the plugging material (plugging material slurry) will be specifically described when a method for manufacturing a ceramic honeycomb filter is described.
  • the clogging member 8 is preferably coarse enough to discharge moisture contained in the filtration membrane slurry used when forming the filtration membrane 3, and more specifically, a plurality of communication holes are formed. It is preferable to be constituted by the formed porous body. Further, when the clogging member 8 is formed of a porous body having a plurality of communication holes formed therein, it is preferable that each of the plurality of communication holes has a portion having a hole diameter of 20 zm or less. In the present embodiment, it is preferable that the porosity of the clogging member 8 is 25 to 50%.
  • the filtration membrane 3 is formed.
  • the solid component contained in the filtration membrane slurry used for It may pass through and enter the water collection cell 5. If the porosity is less than 25%, it may be difficult to discharge water contained in the filtration membrane slurry used for forming the filtration membrane 3.
  • the communication hole in the present embodiment is a pore communicating from one part of the surface of the clogging member 8 to another part. Further, it is preferable that the clogging member 8 is uniformly filled so that there is no void whose volume exceeds 0.065 mm 3 . The volume 0.
  • the coefficient of thermal expansion of the clogging member 8 is lower than or equal to the coefficient of thermal expansion of the partition 2. If the coefficient of thermal expansion of the clogging member 8 is larger than the coefficient of thermal expansion of the partition 2, the clogging member 8 may expand during firing, and the partition 2 may be damaged.
  • each of the cross-sections of the plurality of membrane filtration cells 4 perpendicular to the flow direction of the fluid to be filtered is a circle
  • the shape of the membrane filtration cell 4 is The shape is not limited to this, and for example, is preferably at least one shape selected from the group consisting of a circle, an ellipse, an oval, a rectangle, a rectangle, a pentagon, a hexagon, and a heptagon.
  • the shape of the water collection cells 5 is not limited to this.
  • the shape is preferably at least one selected from the group consisting of a circle, an ellipse, an oval, a triangle, a rectangle, a pentagon, a hexagon, and a heptagon.
  • the filtration membrane 3 disposed inside the membrane filtration cell 4 preferably contains titania, alumina, or both.
  • the filtration membrane 3 has an average pore diameter smaller than the average pore diameter of the partition walls 2, and for example, preferably has an average pore diameter of 0.1 to 1.0 / zm.
  • the filtration membrane is an intermediate membrane having an average pore diameter in the middle between the partition wall and the upper filtration membrane, wherein the filtration membrane is an upper filtration membrane. Configuration further equipped with It may be.
  • the raw material is extruded using, for example, a vacuum extruder to obtain an unsintered filter molded body having a predetermined shape and having cells serving as flow paths of the fluid to be filtered and the filtered fluid.
  • the raw materials are described as a preferred material for the partition wall 2 of the ceramic honeycomb filter 1 shown in FIG. 1 (a), by adding an organic binder such as methyl cellulose, a dispersant, and water to the aggregate particles and the inorganic binder.
  • an organic binder such as methyl cellulose, a dispersant, and water
  • a kneaded clay that is mixed using a kneader or a kneader can be suitably used.
  • a water collecting slit is formed in the obtained green body from one part of the side surface of the green body through a predetermined cell to communicate with the other part, and the green body with the water collecting slit is formed.
  • the water collecting slit is formed by grooving the outer wall of the part where the water collecting slit is formed at the time of molding, breaking the water collecting cell wall at the outer periphery with a grindstone, and then collecting the water with a jig having a sharp tip. It can be formed by piercing a water cell.
  • the water collecting slit is used as a part for installing a sealing member that separates the fluid to be filtered from the filtered fluid at the end of the ceramic honeycomb filter, which is the final product, when it is installed in water purification equipment. If a defect occurs in the gripping part that grips the end face in the filtration film forming process described later, it is necessary to remove the defective part by a maximum of about 30 mm. In consideration of the occurrence of cracks, it is preferable to form the unsintered filter formed body with the water collecting slit on a side surface about 55 mm away from the end face. The steps so far can be performed according to a conventional method for manufacturing a ceramic honeycomb filter.
  • a predetermined cell 1 Fill the space up to the water collecting slit 7 penetrating 2 with the plugging material (plugging material slurry) 13 to obtain a plugged material-filled unfired filter molded body.
  • films 11 (masking) of polyester or the like are attached to both end surfaces of the unsintered filter molded body 10 with the water collecting slit, and holes are formed in portions corresponding to predetermined cells 12.
  • the end face of the unsintered filter molded body 10 with the water collecting slit, to which the film 11 is attached is pressed into a container 14 filled with the clogging material 13 and an air cylinder is further provided.
  • pressurization is performed at 200 kgf / cm 2 to fill a predetermined cell 12 with the clogging material.
  • the plugging material 13 used in the present embodiment includes an aggregate particle, an inorganic binder, and the like, so that the plugging material 13 can be filled in a predetermined cell 12 until it reaches the water collecting slit. It is preferable that the composition contains a binder, a thickener and a water retention agent.
  • the aggregate particles and the inorganic binder those similar to the aggregate particles and the inorganic binder used when producing the unfired filter molded body can be suitably used.
  • the binder that forms the plugging material 13 has the function of increasing the drying strength of the plugging material 13 at the time of drying and preventing the occurrence of cracks during drying, and is made of polyvinyl alcohol, polyethylene glycol, starch, and clay. It is preferably at least one compound selected from the group consisting of:
  • the filler 13 preferably contains 0.08 to 0.12 parts by mass of the binder with respect to 100 parts by mass of the aggregate particles. If the amount of the binder is less than 0.08 parts by mass, cracks may occur when the plugging material 13 is dried. When the amount of the binder exceeds 0.12 parts by mass, the strength of the plugging material 13 is increased, and cracks may be generated in the unsintered filled molded article 10 having the water collecting slit.
  • the thickening agent constituting the plugging material 13 is made of a filler 1 such that the plugging material 13 can be easily inserted into a predetermined cell 12 of the unsintered filter molded body 10 with a water collecting slit. 3 has the function of developing an appropriate viscosity, and methylcellulose, lipoxyl methylcellulose, and the like can be suitably used.
  • the filler 13 preferably contains the thickener in an amount of 0.04 to 0.1 part by mass with respect to 100 parts by mass of the aggregate particles. If the amount of the thickener is less than 0.04 parts by mass, the plugging material 13 does not enter the predetermined cell 12 smoothly, and it is difficult to fill the plugging material 13 to a predetermined depth. It can be. If the amount of the thickener exceeds 0.1 parts by mass, the depth of the plugging material 13 filled in each cell 12 differs, and the plugging material 13 is uniformly filled to a predetermined depth. Can be difficult.
  • the water retaining agent constituting the plugging material 13 absorbs the water content of the plugging material 13 into the dried green filter molded body 10 with the water collecting slit. It functions to prevent solidification and to allow the clogging material 13 to uniformly penetrate to a predetermined depth.
  • the water retention agent starch, glycerin and the like can be suitably used.
  • the plugging material 13 preferably contains 5 to 6 parts by mass of the water retention agent with respect to 100 parts by mass of the aggregate particles.
  • the water retention agent is less than 5 parts by mass, when filling the plugging material 13, the moisture of the plugging material 13 is instantaneously absorbed by the unsintered filled molded product 10 with the water collecting slit, and It may not be possible to fill the filling material 13 to the specified depth. If the water retention agent exceeds 6 parts by mass, the plugging material 13 may not be sufficiently dried by drying before firing, and cracks may be generated during firing.
  • the obtained unfired filter-filled filter molded product is fired, for example, at 900 to 140 ° C. to obtain a filter-filled filter molded product.
  • a filter membrane is formed on the inner peripheral surface of a predetermined cell constituting the obtained plugged material-filled filter molded body, and then fired.
  • a method for forming a filtration membrane for example, when forming a filtration membrane composed of an intermediate membrane and an upper filtration membrane having a smaller pore size than the intermediate membrane, first, an intermediate membrane is formed. Is formed.
  • the interlayer slurry is composed of 100 parts by mass of a ceramic raw material such as alumina, mullite, titania, cordierite, etc., having the same material as the green compact and having an average particle size of 3.2 m. It can be formed by adding 100 parts by mass of water.
  • an inorganic binder for film may be added to the intermediate film slurry in order to increase the film strength after firing.
  • the inorganic binder for the film clay, kaolin, titania sol, silica sol, glass frit, or the like can be used, and the addition amount is preferably 5 to 20 parts by mass from the viewpoint of the film strength.
  • This intermediate film slurry was formed on the surface of each cell using an apparatus disclosed in Japanese Patent Application Laid-Open No. Sho 61-238338, dried, and then dried at a predetermined firing temperature, for example, 900 It can be sintered at up to 150 ° C. and fixed to a plugging material-filled filter to form an intermediate film.
  • an upper filtration membrane slurry for forming an upper filtration membrane is formed.
  • the upper-layer filtration membrane slurry is, for example, a ceramic material such as alumina, mullite, titania, cordierite, or the like, having an average particle diameter of 0.4 m and the same material as the unfired filter molded body, or a coefficient of thermal expansion higher than these ceramic materials. It can be formed by adding 100 parts by mass of water to 100 parts by mass of a material having a small content. Also, this upper filtration membrane An inorganic binder for a film may be added to the slurry in order to increase the film strength after firing.
  • the inorganic binder for the film clay, kaolin, titania sol, silica sol, glass frit, or the like can be used.
  • the addition amount is preferably 5 to 20 parts by mass from the viewpoint of the film strength.
  • This upper-layer filtration membrane slurry was formed on the surface of the intermediate membrane using an apparatus disclosed in Japanese Patent Application Laid-Open No. Sho 61-238338, dried, and then dried at a predetermined firing temperature 90 °. It can be sintered at 0 to 150 ° C. and adhered to the intermediate film formed on the filter-filled filter molded body to form a filtration membrane.
  • the filtration membrane slurry (the intermediate membrane slurry and the upper filtration membrane slurry)
  • the water and the like contained in the water remain in the liquid pool and do not lift and separate the filtration membrane, and the filtration membrane can be formed normally over the entire area of the predetermined cell.
  • a defect may occur in the gripping portion that grips the end face, so that the end face of the formed clogging material-filled molded product is set to 30%. Cut about mm.
  • a glaze such as glass frit is applied to the cut and newly formed end face of the filler-filled molded product, dried once, and then fired at 900 to 140 ° C.
  • the conditions for applying and firing the glaze can be determined according to the conventional method of manufacturing ceramic honeycomb fillers.
  • the ceramic honeycomb filter thus obtained effectively prevents the fluid to be filtered and the filtered fluid from staying inside, and can supply a highly clean filtered fluid.
  • alumina having a predetermined average particle size as an aggregate particle and glass frit as an inorganic binder were mixed at a mass ratio of 9: 1.
  • Parts by mass, water and 4.5 parts by mass of methylcellulose as an organic binder, and 1 part by mass of a dispersant were added and kneaded to obtain a kneaded material.
  • electrofused alumina having a raw material particle size of 0.2 to 0.5 mm and an alumina purity of 99.8% was pulverized by a dry method for a predetermined time, and the average particle sizes were 30 rn and 50, respectively.
  • m, 100 m were designated as alumina A, alumina B, and alumina C.
  • a clogging material is placed in each of the obtained unsintered filter molded bodies with water collecting slits in a space from each end face of a predetermined cell to a water collecting slit penetrating the predetermined cell. Filling was performed to obtain a plugged material-filled green compact.
  • a material obtained by mixing aggregate particles, an inorganic binder, a binder, a thickener, and a water retention agent in the proportions shown in Tables 1 and 2 was used as a plugging material.
  • Example 1 Alumina A 30 95 5 0.1 0. 05 5.6 22
  • Example 2 Alumina A 30 90 10 0.1 0.15 5.6 22
  • Example 3 Alumina A 30 85 15 0. 1 0.05 5.6 22
  • Example 4 Alumina B 50 90 10 0.1 0.15 5.6 22
  • Example 5 Alumina C 100 90 10 0.1.05 5.6 22
  • Example 6 Alumina B 50 90 10 0.06 0.05 5.6 22
  • Example 7 Alumina B 50 90 10 0.08 0.05 5.6 22
  • Example 8 Alumina B 50 90 10 0.12 0.05 5.6 22
  • Example 9 Alumina B 50 90 10 0.14 14.05 5.6.22
  • Example 10 Alumina B 50 90 10 0.10.02 5.6.22 Example 11 Alumina B 50 90 10 0.1.08.6.22 Example 12 Alumina B 50 90 10 0. 1 0.10 5.6 22 Example 13 Alumina B 50 90 10 0.1 0.1 0.25 5.622 Example 14 Alumina B 50 90 10 0.1.05 4.8.22 Example 15 Alumina B 50 90 10 0.10.05 5.4 22 Example 16 Alumina B 50 90 10 0.1.05 6.022 Example 17 Alumina B 50 90 10 0.1.05 6.22 22
  • the ratio (%) of the shrinkage defect of the plugging material in the dried state of the plugging material-filled unsintered fill molding was measured.
  • the shrinkage defect of the plugging material is a defect in the center of the plugging material filling portion when moisture is supplied to the filling portion after the portion filled with the plugging material is dried.
  • the ratio of clogging defect of clogging material (%) is a value calculated by calculating the ratio (%) of the number of clogging defect of clogging material to the number of cells filled with clogging material. The results are shown in Tables 3 and 4.
  • Example 10 2 ⁇ 0.8 10.23 37 13 13 ⁇ Example 11 2 ⁇ 0 10.1 36 ⁇ 16 ⁇ Example 12 1 ⁇ 0.3.2 35 ⁇ 15 ⁇ Example 13 2 ⁇ 0. 5 9.93 6 ⁇ 17 ⁇ Example 14 3 ⁇ 2. 5 9.93 6 ⁇ 15 ⁇ Example 15 2 ⁇ 1.9 10.1 36 ⁇ 15 ⁇ Example 16 2 ⁇ 2. 1 10. 2 35 ⁇ 16 ⁇ Example 17 1 ⁇ 2. 5 10. 0 36 ⁇ 18 ⁇
  • the obtained plugged material-filled unfired filter molded body is fired to obtain a plugged material-filled filter molded product, and the inner peripheral surface of a predetermined cell constituting the obtained plugged material-filled filter molded product.
  • a filter membrane was formed, dried and fired, and the end face was cut to a predetermined length.
  • the dry processability of the fired filter material filled with plugging material was evaluated by checking whether sparks fly from the cutting blade that cuts each filter-filled plugging material. The results are shown in Tables 3 and 4. If the amount of the inorganic binder contained in the plugging material is large, the strength of the fired plugging material filled filter molded body increases and sparks may fly from the cutting blade at the time of cutting, resulting in poor machinability. The sample that could be cut well without cutting was marked as ⁇ , and the spark was slightly blown, but the cut was satisfactorily cut as ⁇ . Those that were no longer rated are X. The results are shown in Tables 3 and 4.
  • the crack occurrence rate (%) was measured at the portion filled with the plugging material.
  • the crack occurrence rate (%) is a value calculated by calculating the ratio (%) of the number of cracked cells to the number of cells filled with clogging material. The results are shown in Tables 3 and 4.
  • each ceramic honeycomb filter was molded into a block shape, and a test piece having a width of 10 mm, a thickness of 5 mm, and a length of 50 mm was cut out. A three-point bending strength measurement with a distance between supports of 30 mm was performed. The results are shown in Tables 3 and 4.
  • Each ceramic honeycomb filter is immersed in water, the water collecting slit provided near one end face of each ceramic honeycomb filter is closed, air is sent from the other water collecting slit, and foam is generated from each ceramic 82 cam filter.
  • the foaming test was performed by measuring the pressure at that time. The results are shown in Tables 3 and 4. In the foaming test evaluation, if no foaming is seen from the clogging member and the outer wall when pressurized at 8 kPa, it is judged as ⁇ , and if foaming is not seen when pressurized at 6 kPa Is indicated by ⁇ , and X is indicated when foaming is observed when pressurized at 3 kPa. The results are shown in Tables 3 and 4.
  • the fluid to be filtered flows in from one end face of each ceramic honeycomb filter. It was measured whether filtration fluid stayed between the water collecting slit and the clogging member when the purification was performed. If there was no stay, it was marked as ⁇ , and if there was stay, it was marked as X. The results are shown in Tables 3 and 4.
  • a ceramic honeycomb filter was manufactured in the same manner as in the above-described example except that a molded body was obtained, and the same measurement was performed. Tables 5 and 6 show the composition of the clogging material and the results of each measurement.
  • Binder Thickener Water retention agent Water Average particle size
  • the ceramic honeycomb filters of Examples 1 to 17 were obtained from each end face of a given cell until reaching the water collection slit penetrating the given cell. Since the space was filled with the clogging material, there was no stagnation of the filtered fluid in the above-mentioned space, and a highly clean filtered fluid could be supplied.
  • the ceramic honeycomb fills of Examples 1 to 17 show excellent values in the percentage of shrinkage defects of the plugging material (%), dry workability, crack occurrence rate (%), and foaming inspection.
  • the pore size (m) and the porosity (%) were suitable for use as a filter.
  • the ceramic honeycomb filter of the present invention can effectively prevent the fluid to be filtered and the filtered fluid from staying inside, and can supply a highly purified filtered fluid.
  • a wide range of fields such as water treatment, exhaust gas treatment, and pharmaceutical and food fields, it can be suitably used for removing suspended substances, bacteria, dust and the like in liquids and gases.

Abstract

L'invention concerne un filtre alvéolé en céramique (1) comprenant une pluralité de cellules de filtration membranaires (4), séparées les unes des autres par une paroi de séparation en céramique poreuse (2), comportant des membranes de filtration (3) disposées dedans et formant des passages d'écoulement pour un fluide filtré. Ledit filtre comprend également une pluralité de cellules collectrices d'eau (5), séparées les unes des autres par la paroi de séparation (2), positionnées de manière adjacente aux cellules de filtration membranaires (4) spécifiques, par le biais de la paroi de séparation (2) et formant les passages d'écoulement pour le fluide filtré produit par filtration du fluide à filtrer par les membranes de filtration (3). Une paroi extérieure (6) entoure les cellules de filtration membranaires (4) et les cellules collectrices d'eau (5). Des fentes de collecte d'eau (7) allant d'une partie de la paroi extérieure (6) vers les autres parties de ladite paroi extérieure (6), en passant par les cellules collectrices d'eau (5), aux positions de la paroi extérieure (6) situées en dehors de distances spécifiées, à partir des deux parties terminales des cellules collectrices d'eau (5) pour permettre au fluide filtré ayant traversé les cellules collectrices d'eau (5) de s'écouler vers l'extérieur. Un élément d'étanchéité poreux (8) est introduit dans les espaces compris entre les faces terminales des cellules collectrices d'eau et les fentes de collecte d'eau (7). Ledit filtre alvéolé en céramique permet d'obtenir un fluide filtré de niveau de pureté élevé, le fluide à filtrer et le fluide filtré étant empêchés efficacement de s'accumuler dedans.
PCT/JP2004/001763 2003-04-10 2004-02-18 Filtre alveole en ceramique et procede de production correspondant WO2004091756A1 (fr)

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US7687008B2 (en) 2006-01-27 2010-03-30 Hitachi Metals, Ltd. Method for producing ceramic honeycomb filter
CN102172477A (zh) * 2011-03-24 2011-09-07 景德镇陶瓷学院 一种组合式蜂窝陶瓷膜过滤元件
CN103285736A (zh) * 2013-06-20 2013-09-11 景德镇陶瓷学院 一种具有高膜面积/体积比的无机膜元件及其膜组件的制备方法
CN103657422A (zh) * 2012-09-14 2014-03-26 浙江瑞普环境技术有限公司 一种膜芯及由其组成的膜组件
WO2014119742A1 (fr) * 2013-02-01 2014-08-07 日本碍子株式会社 Procédé d'utilisation d'un filtre céramique et dispositif-filtre associé
WO2017103473A1 (fr) * 2015-12-18 2017-06-22 Saint-Gobain Centre De Recherches Et D'etudes Europeen Filtre monolithique

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JP5597579B2 (ja) * 2011-02-28 2014-10-01 株式会社クボタ 膜エレメント、膜モジュール、及び膜エレメントの製造方法
JP6308943B2 (ja) * 2011-09-27 2018-04-11 ダウ グローバル テクノロジーズ エルエルシー セラミックハニカム構造体用セメント及び表皮材
JP6023068B2 (ja) 2011-10-11 2016-11-09 日本碍子株式会社 セラミックフィルタ
EP2832429B1 (fr) * 2012-03-30 2019-02-20 NGK Insulators, Ltd. Corps en céramique poreux en forme de nid d'abeilles, son procédé de fabrication, et structure à membrane de séparation en céramique en forme de nid d'abeilles
JP6102114B2 (ja) * 2012-07-31 2017-03-29 株式会社明電舎 モノリス型のセラミックスフィルタ用基材とその製造方法
JP6279891B2 (ja) * 2013-11-27 2018-02-14 日本特殊陶業株式会社 フィルタ構造体及びその製造方法
JP6541644B2 (ja) * 2014-03-28 2019-07-10 日本碍子株式会社 モノリス型基材、モノリス型分離膜構造体及びモノリス型基材の製造方法
JP6687438B2 (ja) * 2016-03-25 2020-04-22 日本碍子株式会社 ハニカムフィルタ
WO2023153057A1 (fr) * 2022-02-08 2023-08-17 日本碍子株式会社 Dispositif de séparation de gaz mixte, procédé de séparation de gaz mixte et dispositif de réacteur à membrane

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7687008B2 (en) 2006-01-27 2010-03-30 Hitachi Metals, Ltd. Method for producing ceramic honeycomb filter
CN102172477A (zh) * 2011-03-24 2011-09-07 景德镇陶瓷学院 一种组合式蜂窝陶瓷膜过滤元件
CN102172477B (zh) * 2011-03-24 2013-04-17 景德镇陶瓷学院 一种组合式蜂窝陶瓷膜过滤元件
CN103657422A (zh) * 2012-09-14 2014-03-26 浙江瑞普环境技术有限公司 一种膜芯及由其组成的膜组件
WO2014119742A1 (fr) * 2013-02-01 2014-08-07 日本碍子株式会社 Procédé d'utilisation d'un filtre céramique et dispositif-filtre associé
CN104994939A (zh) * 2013-02-01 2015-10-21 日本碍子株式会社 陶瓷过滤器的使用方法及过滤器装置
JPWO2014119742A1 (ja) * 2013-02-01 2017-01-26 日本碍子株式会社 セラミックフィルタの使用方法及びフィルタ装置
CN104994939B (zh) * 2013-02-01 2017-03-08 日本碍子株式会社 陶瓷过滤器的使用方法及过滤器装置
CN103285736A (zh) * 2013-06-20 2013-09-11 景德镇陶瓷学院 一种具有高膜面积/体积比的无机膜元件及其膜组件的制备方法
WO2017103473A1 (fr) * 2015-12-18 2017-06-22 Saint-Gobain Centre De Recherches Et D'etudes Europeen Filtre monolithique
FR3045398A1 (fr) * 2015-12-18 2017-06-23 Saint-Gobain Centre De Rech Et D'Etudes Europeen Filtre monolithique

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