EP3288669A1 - Montierte filter zum filtrieren von flüssigkeiten - Google Patents

Montierte filter zum filtrieren von flüssigkeiten

Info

Publication number
EP3288669A1
EP3288669A1 EP16725187.5A EP16725187A EP3288669A1 EP 3288669 A1 EP3288669 A1 EP 3288669A1 EP 16725187 A EP16725187 A EP 16725187A EP 3288669 A1 EP3288669 A1 EP 3288669A1
Authority
EP
European Patent Office
Prior art keywords
filter
elements
membrane
filter according
membrane filter
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP16725187.5A
Other languages
English (en)
French (fr)
Inventor
Daniel Eckardt
Michael Faber
Malte Moeller
Ronald Neufert
Stephan REMPEL
Fabiano Rodrigues
Adrien Vincent
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Saint Gobain Centre de Recherche et dEtudes Europeen SAS
Original Assignee
Saint Gobain Centre de Recherche et dEtudes Europeen SAS
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 Saint Gobain Centre de Recherche et dEtudes Europeen SAS filed Critical Saint Gobain Centre de Recherche et dEtudes Europeen SAS
Publication of EP3288669A1 publication Critical patent/EP3288669A1/de
Withdrawn legal-status Critical Current

Links

Classifications

    • 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
    • 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
    • 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
    • B01D46/2422—Mounting of the body within a housing
    • 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
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    • 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
    • B01D46/24492—Pore diameter
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D46/2451—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure
    • B01D46/2455—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure of the whole honeycomb or segments
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • 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
    • B01D46/2474—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure of the walls along the length of the honeycomb
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B01D46/2451—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure
    • B01D46/2478—Structures comprising honeycomb segments
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B01D46/2451—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure
    • B01D46/2482—Thickness, height, width, length or diameter
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    • 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
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    • 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
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
    • B01D61/027—Nanofiltration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/14—Ultrafiltration; Microfiltration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/14—Ultrafiltration; Microfiltration
    • B01D61/145—Ultrafiltration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/14—Ultrafiltration; Microfiltration
    • B01D61/147—Microfiltration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D61/14—Ultrafiltration; Microfiltration
    • B01D61/18—Apparatus therefor
    • 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
    • B01D63/061—Manufacturing thereof
    • 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
    • B01D63/062—Tubular membrane modules with membranes on a surface of a support tube
    • B01D63/063—Tubular membrane modules with membranes on a surface of a support tube on the inner surface thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D65/003—Membrane bonding or sealing
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B01D67/0081—After-treatment of organic or inorganic membranes
    • B01D67/0088—Physical treatment with compounds, e.g. swelling, coating or impregnation
    • C—CHEMISTRY; METALLURGY
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    • 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
    • C04B38/0012—Honeycomb structures characterised by the material used for sealing or plugging (some of) the channels of the honeycombs
    • 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
    • C04B38/0016—Honeycomb structures assembled from subunits
    • 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
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    • C04B38/0016—Honeycomb structures assembled from subunits
    • C04B38/0019—Honeycomb structures assembled from subunits characterised by the material used for joining separate subunits
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D2313/00—Details relating to membrane modules or apparatus
    • B01D2313/04—Specific sealing means
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B01D2315/00—Details relating to the membrane module operation
    • B01D2315/10—Cross-flow filtration
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B01D2315/00—Details relating to the membrane module operation
    • B01D2315/12—Feed-and-bleed systems
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D2319/00—Membrane assemblies within one housing
    • B01D2319/04—Elements in parallel
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • 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
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    • B01D46/2418—Honeycomb filters
    • B01D46/2498—The honeycomb filter being defined by mathematical relationships
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B01D63/022—Encapsulating hollow fibres
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    • B01D67/0039—Inorganic membrane manufacture
    • B01D67/0051—Inorganic membrane manufacture by controlled crystallisation, e,.g. hydrothermal growth
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    • C04B38/0054—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore size, pore shape or kind of porosity the pores being microsized or nanosized
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    • C04B38/0058—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore size, pore shape or kind of porosity open porosity

Definitions

  • the invention relates to the field of filtering structures made of an inorganic material intended for the filtration of liquids, in particular membrane-coated structures in order to separate particles or molecules from a liquid, more particularly water, for example production water from oil extraction or shale gas.
  • Filters have long been known using ceramic or non-ceramic membranes to filter various fluids, especially polluted water. These filters can operate according to the principle of frontal filtration, this technique involving the passage of the fluid to be treated through a filter medium, perpendicular to its surface. This technique is limited by the accumulation of particles and the formation of a cake on the surface of the filter medium, and gives rise to a rapid drop in performance and a drop in the level of filtration.
  • tangential filtration is used, which, on the contrary, makes it possible to limit the accumulation of particles, thanks to the longitudinal circulation of the fluid on the surface of the membrane.
  • the particles remain in the flow of circulation whereas the liquid can cross the membrane under the effect of the pressure.
  • This technique provides stability of performance and filtration level. It is more particularly recommended for the filtration of fluids heavily loaded with particles and / or molecules.
  • the strengths of the tangential filtration are its ease of implementation, its reliability through the use of organic membranes and / or inorganic porosity adapted to perform said filtration, and its continuous operation.
  • Tangential filtration uses little or no adjuvant and provides two separate fluids that can be both valuable: the concentrate (also called retentate) and the filtrate (also called permeate): it is a clean process that respects the environment.
  • the pollutants can remain trapped in the structure. In such a case, no concentrate is collected at the outlet of the structure, but only a filtrate.
  • Tangential filtration techniques are particularly used for microfiltration
  • filter structures operating according to the principles of tangential filtration are known from the present technique. They comprise or consist of tubular supports made of a porous inorganic material formed of walls defining longitudinal conduits or channels parallel to the axis of said supports. The liquid to be filtered passes through the walls and then the filtrate is evacuated most often at the peripheral outer surface of the porous support.
  • the filters comprise at least one filter element consisting of a plurality of ducts separated by porous walls. Such a structure is commonly called in the honeycomb field.
  • the surface of said ducts is also usually covered with a membrane, most often in a porous inorganic material, referred to herein as membrane or membrane-separating layer, whose nature and morphology are adapted to stop molecules or particles whose size is close to or greater than the median pore diameter of said membrane when the fluid filtered is spread in the porosity of the porous support.
  • membrane or membrane-separating layer whose nature and morphology are adapted to stop molecules or particles whose size is close to or greater than the median pore diameter of said membrane when the fluid filtered is spread in the porosity of the porous support.
  • the median pore diameter of the material constituting the filter membrane is normally much smaller than that of the material constituting the walls of the conduits, the ratio generally ranging from 1/1000 to 1/10.
  • the thickness of the membranes is much thinner than that of the walls, the ratio ranging from 1/200 to 1/5.
  • the membrane is conventionally deposited on the inner surface of the channels by a process for coating a porous inorganic material with a slip followed by a consolidation heat treatment, in particular drying and optionally sintering of the ceramic membranes.
  • the patent application US2013 / 0153485 discloses a membrane filter comprising an assembly of filter elements whose ends are connected by a material forming a mounting ring ("mounting ring").
  • mounting ring a material forming a mounting ring
  • the object of the present invention is to solve the problems previously described, and proposes in particular to provide a mechanically resistant filter, assembled from a set of honeycomb ceramic filter elements, each comprising a plurality of ducts, and whose filtration efficiency is optimal, in particular by preventing the presence of bypass zones in the assembled filter, by which a part of the liquid is not filtered, while preserving as much as possible the filtration surface accessible to the liquid within said filter.
  • the present invention thus relates to a membrane filter for liquid filtration comprising:
  • each element comprising a plurality of parallel ducts separated by walls made of a porous ceramic material, in particular of which the open porosity is comprised between 15 and 60%, said ducts being open on a face of introduction of the liquid to be filtered,
  • a filtration membrane made of a ceramic material disposed on the internal surface of the walls of the ducts, optionally means for recovering the filtrate, arranged at the outlet of the ducts and / or at the periphery of the filter,
  • said filtering elements are linked together, at least on the end of the filter open on said introduction face, by means of a hardenable material, in particular a hardenable resin optionally incorporating a mineral filler, forming after hardening a sleeve in the form of a single piece sealingly securing all of said filter elements, said sleeve now between said interstitial volume,
  • a hardenable material in particular a hardenable resin optionally incorporating a mineral filler
  • said sleeve has a thickness e, measured along the longitudinal axis of the filter, of between 1 and 10%, preferably between 1.5 and 7% and very preferably between 2 and 5%, of the length of the filter, and
  • the curable material is present in the open porosity and through the entire thickness of each porous wall constituting the elements, over a minimum height h which is not zero, said height being measured parallel to the longitudinal axis of the element under consideration and from its open end to the insertion face.
  • Said minimum height h is less than 2.5> ⁇ e, preferably less than 2> ⁇ e, more preferably less than 1.5> e, and most preferably less than or equal to 1 ⁇ e.
  • the maximum height at which the curable material is present in the open porosity and through the entire thickness of the porous walls constituting the elements is less than 3> ⁇ e, preferably less than 2.5> ⁇ e and very preferably less than 2> ⁇ e.
  • the filter further comprises at least one second sleeve, preferably identical to the first sleeve.
  • Said second sleeve is disposed at the opposite end of the filter.
  • the average thickness e of the sleeve is between 2 and 5% of the average length of said elements.
  • the median pore diameter in the porous walls is between 5 and 50 microns, preferably between 10 and 40 microns.
  • the median pore diameter of the membrane is between 50 nanometers and 10 microns and is at least five times smaller than the median pore diameter of the porous walls.
  • the length of the filter is between 200 and 1500 mm.
  • the thickness of the porous walls of the ducts is between 0.3 and 1.5 mm.
  • the average thickness of the membrane is between 20 nanometers and 50 micrometers, especially between 20 nanometers and 10 micrometers, preferably between 100 nanometers and 2 micrometers.
  • the average thickness of the membrane is at least 5 times or at least 10 times its median pore diameter.
  • the ducts are of square section, round or oblong, preferably round, and preferably further whose hydraulic diameter is between 1 and 5mm.
  • the elements are of round section, the diameter of said round section being between 20 and 80 mm.
  • the elements are of hexagonal section, the distance between two opposite sides of the hexagonal section being between 20 and 80 mm.
  • the ducts of the filter elements are open at both ends.
  • the conduits of the filter elements are alternately plugged on the introduction face of the liquid to be filtered and on the opposite face.
  • the ducts of the filter elements are open on the liquid introduction face and closed on the recovery face.
  • the filtrate recovery means are arranged at the periphery of the filter.
  • the filter elements and preferably the membrane comprise and preferably consist essentially of particles of silicon nitride and / or silicon carbide.
  • the curable material is selected from epoxy resins and acrylate resins.
  • the curable material comprises a filler consisting of mineral particles whose median diameter D 5 o is between 1 and 100 microns.
  • Said filter is surrounded by a compartment in which is made an opening for said recovery of the filtrate.
  • the filter according to the invention is normally disposed in a compartment (also called housing or "housing" in the present description).
  • a compartment also called housing or "housing” in the present description.
  • said compartment thus surrounds the filter elements and the sleeve or sleeves.
  • Such a compartment allows in particular the confinement of liquids (filtrate and / or retentate) within a filtration unit.
  • said filtrate recovery means may therefore include the compartment (housing) in which said filter is inserted.
  • said means comprise in particular an opening in said compartment, as described for example in the publication US 2013/0153485) or in FIGS. 8 attached.
  • said recovery means may comprise or be constituted by an opening made in the housing surrounding the filter.
  • the invention also relates to a filtration unit comprising a filter as described previously inserted into its compartment, including the filtrate recovery means.
  • the invention also relates to a method of manufacturing a membrane filter according to one of the preceding claims, comprising the following successive steps: a. manufacturing a set of honeycomb filter elements comprising a plurality of parallel ducts separated by walls made of a porous ceramic material whose open porosity is between 15 and 60%,
  • a hardenable material preferably a resin optionally comprising a charge of mineral particles, and adjusting its viscosity such that said hardenable material penetrates the entire thickness of each porous wall of all the elements at a non-zero height h said height being measured along the longitudinal axis of the filter,
  • the ends of each of the filter elements are pre-impregnated with a resin, for example curable, which blocks the porosity of the porous ceramic material on the introduction face of the liquid to be filtered.
  • a resin for example curable
  • channels or internal ducts are understood to mean ducts that do not share a wall that is common to the external or peripheral surface of the filter element.
  • a conduit which has at least one wall common with the outer surface of the filter element is said peripheral. This wall is called outer wall.
  • the other walls are called internal walls.
  • the open porosity and the median diameter of the pores of the porous walls described in the present description are determined in known manner by mercury porosimetry.
  • the pore volume is measured by mercury intrusion at 2000 bar using an Autopore IV 9500 Micromeritics mercury porosimeter, on a sample of 1 cm 3 taken from a block of the product, the sampling region excluding the skin. typically extending up to 500 microns from the block surface.
  • the applicable standard is ISO 15901-1.2005 part 1.
  • the increase in pressure up to high pressure leads to "push" the mercury into pores of smaller and smaller size.
  • the intrusion of mercury is conventionally done in two stages. Initially, a mercury intrusion is made at low pressure up to 44 psia (about 3 bar), using air pressure to introduce mercury into the larger pores (> 4ym). In a second step, a high-pressure intrusion is carried out with oil up to the maximum pressure of 30000 psia (about 2000 bar).
  • a mercury porosimeter thus makes it possible to establish a pore size distribution by volume.
  • the median pore diameter of the walls porous corresponds to a threshold of 50% of the population in volume.
  • the porosity of the membrane, corresponding to the total pore volume in the membrane, and the median pore diameter of the membrane are advantageously determined according to the invention using a scanning electron microscope.
  • sections of a wall of the support are made in cross section so as to visualize the entire thickness of the coating over a cumulative length of at least 1.5 cm.
  • the acquisition of the images is performed on a sample of at least 50 grains, preferably at least 100 grains.
  • the area and the equivalent diameter of each of the pores are obtained from the images by conventional image analysis techniques, possibly after a binarization of the image to increase the contrast. A distribution of equivalent diameters is thus deduced, from which the median diameter of pores is extracted.
  • the porosity of the membrane is obtained by integrating the distribution curve of equivalent pore diameters.
  • this method can be used to determine a median size of the particles constituting the membrane layer.
  • the median size of the particles constituting the membrane layer is generally between 20 nanometers and 10 micrometers, preferably between 100 nanometers and 2 micrometers.
  • An example of determination of the median pore diameter or the median size of the particles constituting the membrane layer comprises the succession of the following steps, conventional in the field:
  • a series of SEM images is taken of the support with its observed membrane layer in a cross-section (that is to say throughout the thickness of a wall). For more clarity, the pictures are taken on a polished section of the material. The acquisition of the image is performed over a cumulative length of the membrane layer at least equal to 1.5 cm, in order to obtain values representative of the entire sample.
  • the images are preferably subjected to binarization techniques, well known in image processing techniques, to increase the contrast of the particle or pore contour.
  • a measurement of its area is carried out.
  • An equivalent diameter of pores or grain is determined, corresponding to the diameter of a perfect disk of the same area as that measured for said particle or for said pore (this operation may possibly be carried out using software especially dedicated Visilog® marketed by Noesis).
  • a size distribution of particles or grains or pore diameter is thus obtained according to a conventional distribution curve and a median particle size and / or a median pore diameter constituting the membrane layer are thus determined, this median size or median diameter respectively corresponding to the equivalent diameter dividing said distribution into a first population comprising only particles or pores of equivalent diameter greater than or equal to this median size and a second population comprising particles of equivalent diameter less than this median size or this median diameter.
  • the median diameter D50 of the powders of the particles, in particular silicon carbide powders, used to produce the support or the membrane is evaluated classically by a particle size distribution characterization performed with a particle size analyzer.
  • laser according to ISO 13320-1.
  • the laser granulometer may be, for example, a Partica LA-950 from the company HORIBA.
  • the median diameter of the particles respectively denotes the diameter of the particles below which 50% by mass of the population is found.
  • all the ducts have a section and a substantially constant and identical distribution over the entire length of the filter, regardless of the cross sectional plane considered.
  • thickness e of the sleeve it is understood the average thickness of said sleeve measured parallel to the longitudinal central axis of the filter.
  • the thickness of the sleeve may, however, vary locally substantially in the longitudinal direction of the filter, in particular depending on the technique of developing the sleeve, for example depending on the profile of the mold used to cast the curable material binding the filter elements together.
  • the filter element is obtained by extrusion of a paste through a die configured according to the geometry of the structure to be produced according to the invention.
  • the extrusion is followed by drying and baking to sinter the inorganic material constituting the support and to obtain the characteristics of porosity and mechanical strength required for the application.
  • it when it is a support in SiC, it can be obtained in particular according to the following manufacturing steps:
  • the mixture also comprises an organic binder of the cellulose derivative type. Water is added and kneaded to obtain a homogeneous paste whose plasticity allows extrusion, the die being configured to obtain the monoliths according to the invention.
  • the baking atmosphere is preferably nitrogenous.
  • the baking atmosphere is preferably neutral and more particularly argon. The temperature is typically maintained for at least 1 hour and preferably for at least 3 hours.
  • the obtained material has an open porosity of 15 to 60% by volume and a median pore diameter of the order of 5 to 50 microns, preferably between 10 and 40 microns.
  • the average thickness of the outer walls of an element according to the invention is between 0.5 and 2.0 mm. Such a thickness makes it possible in particular to ensure that the porous ceramic material constituting the outer wall and the hardenable resin entering into its porosity has a suitable cohesion and bonding. If necessary, the outer surface of the porous walls can also be roughened to further facilitate the attachment and penetration of the resin into the porosity of the walls.
  • the average thickness of the inner walls of the elements is generally lower than that of the outer walls and is preferably between 0.3 and 1.5 mm.
  • the length of the filter elements is in principle between 200 and 1500 mm.
  • the hydraulic diameter of the ducts is preferably between 1 and 5 mm, preferably between 1.5 and 4 mm.
  • certain conduits may or may not be plugged at the ends, in particular at the opposite end of the conduits with reference to the introduction of the liquid into the filter.
  • no duct is clogged.
  • the filter element is then coated according to the invention with a membrane (or membrane separator layer).
  • a membrane or membrane separator layer.
  • One or more so-called primary layers can be deposited before forming the filter membrane according to various techniques known to those skilled in the art: deposition techniques from suspensions or slips, chemical vapor deposition techniques (CVD) or thermal projection, for example plasma projection (plasma spraying).
  • the primer layers and the membrane are deposited by coating from slips or suspensions comprising ceramic particles.
  • a first layer is preferably deposited in contact with the substrate (primary layer), acting as a bonding layer.
  • the formulation of the primer comprises 50% by weight of grains of SiC (median diameter between 2 and 20 microns) and 50% of deionized water.
  • a second layer of finer porosity is deposited on the primer layer, and constitutes the membrane itself. The porosity of this last layer is adapted to give the filter element its final properties.
  • the formulation of the membrane preferably comprises 50% by weight of SiC grains (in particular of median diameter between 0.1 and 2 micrometers) and 50% of deionized water.
  • thickening agents in proportions typically between 0.02 and 2% of the water mass
  • binding agents typically between 0.5 and 20% of the mass of water
  • SiC powder can be added.
  • the thickening agents are preferably cellulosic derivatives
  • the binding agents preferably PVA or acrylic derivatives
  • the dispersing agents are preferably of the ammonium polymethacrylate type.
  • the thus coated member is then dried at room temperature typically for at least 30 minutes and then at 60 ° C for at least 24 hours.
  • the supports thus dried are sintered at a firing temperature typically between 1700 and 2200 ° C under a non-oxidizing atmosphere, preferably under argon, so as to obtain a membrane porosity (measured by image analysis as described above) included preferably between 10 and 40% by volume and a median equivalent diameter of pores (measured by image analysis) preferably between 50 nm and 10 micrometers, or even between 100 nm and 5 micrometers.
  • the lower end of the elements is then leveled to remove excess coating materials, much more concentrated in this part of the ceramic part, over a length of about 5 to 20 mm.
  • the filtration membranes according to the invention preferably have the following characteristics: They consist essentially of a ceramic material, preferably based on non-oxide ceramics, preferably chosen from silicon carbide, in particular sintered SiC. in liquid phase or in solid phase or recrystallized SiC, silicon nitride, in particular S1 3 N 4 , oxynitride,
  • the membrane is based on silicon carbide typically recrystallized. - They are deposited on one or more layers of a primary whose pore diameter is intermediate between that (the largest) of the walls and that of the membrane, to facilitate its deposition and homogeneity.
  • the ratio between the size the particles constituting the intermediate layer and the particles constituting the membrane layer are between 5 and 50.
  • the ratio between the mean size of the grains constituting the porous wall and that of the particles constituting the intermediate membrane layer is between 2 and 20.
  • the porosity of the membrane-separating layer is less than 70% and very preferably is between 10 and 70%.
  • the median equivalent pore diameter measured by image analysis of the membrane forming layer is between 1 nm and 5 micrometers.
  • a plurality of filter elements thus obtained are then assembled to form the filter according to the invention, so as to leave between them an interstitial void through which the filtrate introduced on an introduction face of the filter thus obtained can flow.
  • Figure 3 shows in more detail such a configuration.
  • all the elements obtained previously are deposited in a container so as to rest on one of their ends. They are also kept spaced apart by calibrated spacers.
  • a curable resin whose viscosity is adapted according to the invention is introduced into the container so as to fill the interstices between the elements and then the resin is cured, at room temperature or under the effect of heating for the case of a thermosetting resin, until a rigid sleeve in the form of a single piece surrounding and now secured to all the filter elements, as shown in Figures 1 and 5.
  • the same operation is carried out according to a second step at the other end of the filter elements, to obtain the final filter thus comprising a plurality of honeycomb ceramic filter elements arranged substantially in parallel, with a interstitial volume present between said filter elements.
  • the adaptation of the resin and in particular its viscosity during this step of forming the sleeve has appeared critical to allow the proper operation of the assembled filter thus obtained, in particular to ensure the quality of filtration of the device.
  • the viscosity of the hardenable resin injected into the container must be sufficiently low so that curable material penetrates to the core of the open porosity of the walls of the filter elements, ie through the entire thickness of all the porous walls constituting the plurality of elements, in particular through the entire thickness of the inner walls of all the filter elements used to constitute the assembled filter.
  • the presence of the resin in all the porosity of the walls ensures the best operation of the complex structure while effectively avoiding the bypass zones mentioned above (said height being measured along the longitudinal axis of the filter and from said end, see Figure 4).
  • the viscosity must not be too low, in order to avoid excessive clogging of the remaining filtration surface within ducts.
  • the experiments carried out by the applicant company have in fact shown that the use of a too fluid resin induces, by capillary action, the sealing of a sensitive portion of the porosity of the ducts and consequently a reduction of the filtration capacities. filter, or even the complete closure of the most peripheral ducts of the structure.
  • too low viscosity also induces a small thickness of the final sleeve, detrimental to the stability and overall strength of the structure.
  • the most suitable viscosity has been determined as being between 1000 and 3000 mPa.s at 25 ° C. (or more generally at the temperature at which its curing is carried out), even if its optimum value is likely to vary significantly notably. depending on the porosity of the porous walls and / or the geometry of the ducts.
  • the assembled filter thus obtained is then inserted into a housing (also called compartment or housing or casing according to the English term "housing" generally used), comprising openings for the entry of the liquid to be filtered and openings of outlet for the filtrate and optionally retentate, according to conventional configurations such as for example described in the US2013 / 0153485 application.
  • FIGS. 1 illustrate a conventional configuration of a filter comprising 19 filter unitary elements according to the invention, in a front view corresponding to the intake face of the liquid to be filtered (Figure 1A) and in longitudinal section (Figure 1B).
  • Figure 1C shows the filter of Figure 1B inserted in its housing, in operation.
  • FIG. 2 schematizes another configuration of a filter element according to the invention, before it is assembled in a filter according to the invention.
  • FIG. 3 schematizes an alternative configuration of a filter element according to the invention, before it is assembled in a filter according to the invention.
  • FIGS. 4 (4A and 4B) illustrate the phenomenon of impregnation of the resin in the porosity of the walls of a filter element during the formation of the sleeve according to the invention.
  • Figure 4B is a schematic representation, provided for clarity, illustrating the features visible in Figure 4A.
  • Figure 5 is a photograph of a filter according to the present invention.
  • FIGS. 6A and 6B schematically show a filter element extracted from the assembly with its portion of the sleeve, in an elevational view ( Figure 6A) and in a three-dimensional section ( Figure 6B).
  • FIGS. 6A and 6B are provided to illustrate the possible bypass of the membrane by the fluid to be filtered in an assembled filter according to
  • Figure 7 shows the plane of a filter according to the invention comprising 7 filter elements. In FIG. 7, the dimensions are indicated in mm.
  • FIG. 1A schematizes a front view of a filter according to the invention, from the inlet face 3 of the liquid to be filtered.
  • Figure 1B shows a schematic view of the filter along the longitudinal sectional plane AA 'shown in Figure 1A.
  • the filter 1 has a longitudinal central axis 13, perpendicular to the front face 3, and passing through its center.
  • the filter comprises a filter element assembly 2 made of a porous inorganic material, preferably non-oxide, such as recrystallized SiC.
  • Each element has, for example, a tubular shape, which may be of hexagonal section as illustrated in FIG. 1A or preferably of circular section as illustrated in FIG. 2.
  • Each element has a longitudinal central axis 12.
  • the filter is inserted into a housing or compartment (housing) a portion of the walls 5 is shown in Figure 1B.
  • Each element 2 comprises in its inner portion a set of ducts (or channels) 7 adjacent axes parallel to each other and separated from each other by walls 8 formed in the porous material.
  • the walls 8 are therefore made of a porous inorganic material passing the filtrate from the inner part of the elements to their outer surface.
  • the ducts 7 are covered on their inner surface with a membrane separating layer (also called filtration membrane or membrane), lining the inside of the ducts (not shown in Figures 1).
  • This filtration membrane comes into contact with said fluid to be filtered flowing in said channels after its introduction into the assembled structure according to the inlet face 3.
  • the filtering structure comprises internal ducts and peripheral ducts occupying the crown of the outermost channels of the filter. In a most conventional configuration illustrated in Figure 1, all the ducts have a circular section.
  • the filter elements have a hexagonal cross section.
  • the filter elements may have other forms than that shown in Figure 1.
  • the filter elements may have a circular section, in a sectional plane perpendicular to their length.
  • Figure 2 illustrates such a configuration of the filter elements.
  • half of the channels of the peripheral ring have a truncated shape, in order to maintain a sufficient thickness of the outer wall.
  • FIG. 3 illustrates another filter configuration comprising elements whose ducts are arranged in a manner similar to those of FIG. 2, the section of the ducts being this time square. According to this configuration, all the ducts have the same section.
  • the filter according to the invention comprises a plurality of conduits distributed along a plurality of rings around a central axis.
  • Conduit ring means a set of ducts whose barycentre is located on the same concentric circle of the central axis of the filter element.
  • the filter elements 2 according to FIGS. 1A and 2 and 3 are grouped in the form of an assembled filter, as illustrated by FIGS. 1B, 5 and 7.
  • Each of the elements 2 is separated from the following by a volume interstitial 6 through which flows the filtrate from the elements 2, after passing through the membrane.
  • the filter elements 2 are kept at a distance from each other to provide an interstitial volume 6 between them, in a single structure and mechanically resistant by means of two sleeves 9 and 10 arranged preferably on either side of the elements 2 and at each end of these this. Both sleeves are in contact and held in compression by the walls 5 of the filtration compartment (often called housing or casing in the field).
  • the liquid to be filtered is introduced from the introduction face 3 of the filter thus obtained, passes through the membrane lining the interior of the ducts 7, a filtrate being collected in the interstitial volumes 6 to be finally collected at the filter outlet, generally through an opening in the housing surrounding the filter (see for example US 2013/0153485).
  • FIG. 1C describes the operation of a filter 1 according to the invention as described in FIG. 1B.
  • the arrows 14 indicate the path of the liquid to be filtered in the filtration unit 20.
  • the filter 1 is disposed in its compartment whose walls 5 comprise an opening 15 for the discharge of the filtrate 16.
  • a retentate 17 is also recovered through the openings of the channels disposed opposite the introduction face for possible recycling.
  • FIGS. 8A to 8C only a filtrate 15 is collected.
  • the configurations described in Figures 8A-8C attached should not, however, be considered as limiting the scope of the present invention, in any of the aspects described.
  • the liquid to be filtered 14 is introduced at the inlet face 3 of the filter. It has a structure in which the conduits of the filter elements 2 are alternately plugged on the face of introduction of the liquid to be filtered and on the opposite side by plugs 18 preferably impervious to liquids, so as to force the liquid to pass through. the porous walls of said filter elements and the membrane covering them.
  • inlet ducts 7 of the liquid to be filtered and outlet ducts 7 'of the filtrate after passing through the porous walls provided with a filtration membrane.
  • the filter 1 is confined in the compartment surrounding it in the filtration unit and a portion of the walls 5 is shown in Figure 8A.
  • the filtrate 16 is recovered at the outlet of the unit 20 through an opening 15 made in the compartment confining the liquids in the filtration unit.
  • Another part of the filtrate 16 ', recovered from the interstitial volumes 6, is collected by an opening 15' made on the peripheral part of the compartment surrounding the filter.
  • the liquid to be filtered is introduced at the inlet face 3 of the filter. This is confined in the compartment surrounding it in the filtration unit and a part of the walls 5 is shown in Figure 8B.
  • the liquid to be filtered passes through the porous walls of said filter elements and the membrane covering them.
  • the filtrate 16 is recovered in the interstitial volumes 6 present around the filter elements and then collected at the outlet of the unit 20 via an opening 15 made in the compartment confining the liquids in the filtration unit.
  • the ducts 7 are obstructed by liquid-tight plugs to force the entire filtrate to pass through the interstitial volumes 6.
  • the sleeve itself ensures the sealing of the opposite face the liquid filter.
  • the liquid to be filtered 14 is first introduced at the inlet face 3 of the filter. This is confined in the surrounding compartment in the filtration unit and a portion of the walls 5 is shown in Figure 8C. As shown in FIG. 8C, during operation, the liquid to be filtered passes through the porous walls of said filter elements and the membrane covering them. The filtrate 16 is first recovered in the interstitial volume 6 present around the filter elements. Apertures 19 are made in the rear filter sleeve to allow filtrate 16 to be exhausted which is finally collected at the outlet of the unit 20 through an opening 15 in the liquid-confining compartment in the filtration unit.
  • FIGS. 6A and 6B illustrate the difficulties encountered in implementing such an assembled filter: when the liquid to be filtered is introduced from the introduction face 3 of the filter, part of it passes directly into the filter. the greatest porosity of the porous walls 8 of the filter element, without entering the ducts 7 and through the membrane 11.
  • Such a bypass circuit is illustrated by the arrows 100 in FIG. 6B.
  • the implementation of the present invention solves such a problem.
  • Filter elements were produced according to the techniques of the art by shaping and baking structures made of porous recrystallized silicon carbide, according to the method of production described above.
  • the hydraulic diameter D h of a channel is calculated, in a plane of any cross section P of the tubular structure, from the surface of the section of the channel S of said channel and its perimeter P, according to said section plane and by applying the following standard expression:
  • the open front area (OFA) is obtained by calculating the percentage ratio of the area covered by the sum of the cross sections of the channels on the total area of the corresponding cross-section of the porous support.
  • the median diameter dso denotes the diameter of the particles below which 50% by weight of the population of said particles).
  • the green monoliths thus obtained are dried by microwave for a time sufficient to bring the water content not chemically bound to less than 1 ⁇ 6 by mass.
  • honeycomb monoliths are then fired to a temperature of at least 2100 ° C which is maintained for 5 hours.
  • the obtained material has an open porosity of 43% and a median pore distribution diameter of about 25 microns, as measured by mercury porosimetry.
  • a membrane separating layer is then deposited on the inner wall of the channels of the support structure according to the method described below:
  • a primer of attachment of the separating layer is constituted in a first step, from a slip whose mineral formulation comprises 30% by weight of a powder of black SiC grains (SIKA DPF-C) whose diameter median D50 is about 11 microns, 20% by weight of a black SiC grain powder (SIKA FCP-07) whose median diameter D50 is about 2.5 microns, and 50% deionized water.
  • a slip whose mineral formulation comprises 30% by weight of a powder of black SiC grains (SIKA DPF-C) whose diameter median D50 is about 11 microns, 20% by weight of a black SiC grain powder (SIKA FCP-07) whose median diameter D50 is about 2.5 microns, and 50% deionized water.
  • a slurry of the material constituting the membrane filtration layer is also prepared, the formulation of which comprises 40% by weight of SiC grains (dso around 0.6 micrometer) and 60% of demineralized water.
  • the rheology of the slips was adjusted by adding organic additives at 0.5-0.7 Pa.s under a shear rate of ls -1 , measured at 22 ° C. according to the DINC33-53019 standard.
  • the slip is introduced into a tank with stirring (20 rpm). After a light vacuum de-aerating phase (typically 25 millibars) while maintaining stirring, the tank is pressurized approximately 0.7 bar in order to coat the interior of the support from its lower part until at its upper end.
  • a light vacuum de-aerating phase typically 25 millibars
  • the elements are then dried at ambient temperature for 30 minutes and then at 60 ° C. for 30 hours.
  • the thus dried supports are then fired at a temperature of 1800 ° C. under argon for 2 hours and at ambient pressure.
  • the thicknesses of the primer layers and the membrane filtration layer after sintering are substantially equal and of the order of 45 micrometers.
  • the firing temperature is a function of the characteristics required for the final porosity of the membrane, ie a median diameter of D50 pores of about 1 micrometer and a total porosity of 40%, by volume.
  • the coated carriers of Examples 7 to 8 were fired at a firing temperature of 1600 ° C under nitrogen for 2h and at ambient pressure.
  • the median pore diameter D 50 of the membrane is measured as equal to about 250 nanometers.
  • the lower part of the elements comprising an accumulation of the materials of the different layers applied, is cut over a length of 10 mm.
  • a cross section is performed on the filters thus obtained.
  • the structure of the membrane is observed under a scanning microscope.
  • the porous wall of the element, of high porosity is observed on an electron microscopy plate, the primer layer enabling the membrane layer to be finer in porosity, which ultimately lines the interior of the conduits.
  • the filter elements thus synthesized are then immersed in a silicone container so as to rest on one of their end.
  • Epoxy-based thermosetting resins are introduced into the container to form a sleeve between the elements.
  • the viscosity of the resin used is different and modulated according to Examples 1 to 6 by the chemical nature of the epoxide used, or by the addition in the initial epoxy resin, before curing, of a mineral filler in the form of a greater or lesser amount of Sic particles of different sizes.
  • Epofix TM An epoxy resin marketed by Struers under the reference Epofix TM, with a viscosity of 390 mPa ⁇ s at 25 ° C.
  • More added SiC powder has a small average diameter plus the viscosity of the mixture with the resin increases.
  • the curable material is cured at ambient temperature, according to the recommendations and conditions recommended by the supplier, until a rigid sleeve is obtained in the form of a single piece surrounding the filter element as schematically illustrated in FIG.
  • the filter elements are cut in their middle and in the longitudinal direction, that is to say in a longitudinal sectional plane passing through the central axis 12 of the element, and a visual observation of the depth and penetration profile of the resin in each conduit is performed.
  • FIG. 4B schematically illustrating the photograph shown in FIG. 4A, the penetration heights of the hardened material 4 in the porosity of the walls 8 are measured for each of the ducts 7 constituting the filter element.
  • the sleeve thicknesses obtained after impregnation and hardening are very variable according to the nature of the hardenable material and that the resin always impregnates the peripheral walls to a maximum height greater than the thickness of the final sleeve, because capillary phenomena.
  • the filtration surface of a filter element corresponds to the internal surface summed of all the internal walls, covered by the membrane and accessible to the fluid to be filtered in said element (or said filter).
  • the portion of the walls whose internal porosity is obstructed by the hardened material during manufacture of the sleeve is not considered to be a filtration surface.
  • Example 7 shows that the curable resin mixture which was suitable according to Example 6 is no longer suitable in the case of a membrane of significantly smaller pore diameter, the most central ducts of the elements not being impregnated by the curable material, which implies the presence of bypass zones of the membrane in the filter.
  • Example 8 shows that it is possible again a device with a sleeve thickness and an impregnation of all the internal walls, provided to change the load (and therefore the viscosity) of the mixture in the resin, using particles of significantly larger size.
  • the results reported in the previous table show that the viscosity of the hardenable material injected into the porosity of the walls of the elements must be adjusted: it must be sufficiently low so that hardenable material penetrates into the open porosity and through all the thickness of all the porous walls constituting the plurality of elements, in particular through the entire thickness of the innermost walls of all the filter elements used to constitute the assembled filter.
  • the presence of the resin throughout the porosity of the walls, along a non-zero height h ensures the best operation of the complex structure by effectively avoiding the bypass zones mentioned previously.
  • the viscosity must not be too low, in order to avoid too much clogging of the remaining filtration surface within the ducts and the general weakening of the assembled filter of the duct. due to a lack of thickness of the sleeves making the constituent elements of the structure integral.
  • filtration is carried out from assembled filters whose configuration is shown in FIG.
  • a turbidity measurement is performed on the filters corresponding to assemblies of 7 filter elements according to Figure 7 attached, using the filter elements and sleeve compositions respectively described in Examples 1 and 2 above.
  • two filters are synthesized and each assembled from 7 filter elements as described in the previous examples.
  • the first filter according to the invention is obtained by bonding the 7 filter elements together on both ends by sleeves 9 and 10, via the curable material as described in Example 1. According to the invention and as shown in Figure 7, the filter is obtained after curing the sleeves in the form of a single piece making integral by sealing all 7 filter elements.
  • the second comparative filter is obtained in the same way as the first, but this time using as a hardenable material the mixture of the resin and the filler described in Example 2.
  • Synthetic dirty water comprising clay, salt, oil and surfactants are used in amounts of 100ppm, 4000ppm, 300ppm and 2ppm, respectively.
  • the dirty water supplies, at a constant temperature of 25 ° C, the two filters to be evaluated under a transmembrane pressure of 0.5 bar and a circulation speed in the channels of 3 m / s.
  • the filtrate (purified water) is recovered at the periphery of the filter, via the interstices 6.
  • the turbidity of the filtrate is continuously measured by means of a BAT-Turbidy Meter series turbidimeter LAT NI series supplied by Kobold Instrumentation, after 10 cycles of filtration.
  • a lower value after turbidity test therefore corresponds to a better filtration quality of the incoming liquid, which can itself be directly related to the absence of bypass zones 100 of the filter membrane, as described in Figure 6B.
  • This turbidity expressed is 0.8 NTU for the first filter (according to the invention) and 3.5 for the comparative filter. Such a difference proves the increased filtration efficiency of the filter obtained according to the principles of the present invention.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Geometry (AREA)
  • Engineering & Computer Science (AREA)
  • Water Supply & Treatment (AREA)
  • Ceramic Engineering (AREA)
  • Nanotechnology (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Filtering Materials (AREA)
EP16725187.5A 2015-04-29 2016-04-29 Montierte filter zum filtrieren von flüssigkeiten Withdrawn EP3288669A1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR1553899A FR3035599B1 (fr) 2015-04-29 2015-04-29 Filtres assembles pour la filtration de liquides
PCT/FR2016/051021 WO2016174373A1 (fr) 2015-04-29 2016-04-29 Filtres assembles pour la filtration de liquides

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EP3288669A1 true EP3288669A1 (de) 2018-03-07

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US (1) US20180304201A1 (de)
EP (1) EP3288669A1 (de)
CN (1) CN107530630A (de)
FR (1) FR3035599B1 (de)
WO (1) WO2016174373A1 (de)

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CN114307665B (zh) * 2020-09-29 2023-02-14 三达膜科技（厦门）有限公司 一种大直径侧积水流道蜂窝陶瓷过滤膜的制备方法
JP7399901B2 (ja) * 2021-02-22 2023-12-18 日本碍子株式会社 ハニカムフィルタ、及びその製造方法
CN113087083A (zh) * 2021-05-21 2021-07-09 上海城市水资源开发利用国家工程中心有限公司 一种新型轻质碳化硅陶瓷可反洗精密过滤装置和方法

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US5779897A (en) * 1996-11-08 1998-07-14 Permea, Inc. Hollow fiber membrane device with inert filaments randomly distributed in the inter-fiber voids
JP3277918B2 (ja) * 1999-06-15 2002-04-22 住友電気工業株式会社 セラミック多孔体を用いた濾過器
JP4599656B2 (ja) * 2000-04-26 2010-12-15 宇部興産株式会社 中空糸分離膜エレメント、中空糸分離膜モジュール、および、その製造方法
US6716275B1 (en) * 2001-12-11 2004-04-06 Sandia Corporation Gas impermeable glaze for sealing a porous ceramic surface
US6767455B2 (en) * 2002-08-21 2004-07-27 Ceramem Corporation Airlift membrane device and membrane bioreactor and bioreactor process containing same
US8814974B2 (en) * 2007-08-24 2014-08-26 Corning Incorporated Thin-walled porous ceramic wall-flow filter
EP2539052B1 (de) * 2010-02-22 2017-07-26 Nanostone Water GmbH Verfahren zum herstellen eines membranmoduls sowie membranmodul
WO2013020968A2 (en) * 2011-08-09 2013-02-14 Shell Internationale Research Maatschappij B.V. Large surface supported molecular sieve membrane

Also Published As

Publication number Publication date
FR3035599A1 (fr) 2016-11-04
CN107530630A (zh) 2018-01-02
US20180304201A1 (en) 2018-10-25
WO2016174373A1 (fr) 2016-11-03
FR3035599B1 (fr) 2019-03-22

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