US20180147534A1 - Single-piece column structure for the separation of a fluid medium - Google Patents

Single-piece column structure for the separation of a fluid medium Download PDF

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Publication number
US20180147534A1
US20180147534A1 US15/575,916 US201615575916A US2018147534A1 US 20180147534 A1 US20180147534 A1 US 20180147534A1 US 201615575916 A US201615575916 A US 201615575916A US 2018147534 A1 US2018147534 A1 US 2018147534A1
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porous
columns
element according
plates
separator
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Philippe Lescoche
Jérôme Anquetil
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Technologies Avancees et Membranes Industrielles SA
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Technologies Avancees et Membranes Industrielles SA
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    • 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
    • B01D63/02—Hollow fibre modules
    • B01D63/027—Twinned or braided type modules
    • 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
    • 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
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0039—Inorganic membrane manufacture
    • B01D67/0041—Inorganic membrane manufacture by agglomeration of particles in the dry state
    • B01D67/00411—Inorganic membrane manufacture by agglomeration of particles in the dry state by sintering
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0039—Inorganic membrane manufacture
    • B01D67/0041—Inorganic membrane manufacture by agglomeration of particles in the dry state
    • B01D67/00415—Inorganic membrane manufacture by agglomeration of particles in the dry state by additive layer techniques, e.g. selective laser sintering [SLS], selective laser melting [SLM] or 3D printing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0039—Inorganic membrane manufacture
    • B01D67/0067—Inorganic membrane manufacture by carbonisation or pyrolysis
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/04—Tubular membranes
    • B01D69/043—Tubular membranes characterised by the tube diameter
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/02—Inorganic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/02—Inorganic material
    • B01D71/0215—Silicon carbide; Silicon nitride; Silicon oxycarbide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B1/00—Producing shaped prefabricated articles from the material
    • 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
    • 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
    • C04B38/0003—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof containing continuous channels, e.g. of the "dead-end" type or obtained by pushing bars in the green ceramic product
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2313/00—Details relating to membrane modules or apparatus
    • B01D2313/02—Specific tightening or locking mechanisms
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2313/00—Details relating to membrane modules or apparatus
    • B01D2313/21—Specific headers, end caps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2027—Metallic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2027—Metallic material
    • B01D39/2031—Metallic material the material being particulate
    • B01D39/2034—Metallic material the material being particulate sintered or bonded by inorganic agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2027—Metallic material
    • B01D39/2031—Metallic material the material being particulate
    • B01D39/2037—Metallic material the material being particulate otherwise bonded
    • 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
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/08—Hollow fibre membranes
    • B01D69/082—Hollow fibre membranes characterised by the cross-sectional shape of the fibre
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y80/00—Products made by additive manufacturing
    • 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
    • C04B2111/00801—Membranes; Diaphragms

Definitions

  • the present invention relates to the technical field of tangential flow separator elements for separating a fluid medium for treatment into a filtrate and a retentate, which elements are commonly referred to as filter membranes.
  • Separation methods using membranes are used in numerous sectors, in particular in the environment for producing potable water and treating industrial effluents, in the chemical, petrochemical, pharmaceutical, and agrifood industries, and in the field of biotechnology.
  • a membrane constitutes a selective barrier and, under the action of a transfer force, it enables certain components of the medium for treatment to pass through or to be stopped. Whether components pass through or are stopped is the result of their size compared with the size of the pores in the membrane, which then behaves as a filter. Depending on the size of the pores, these techniques are referred to as microfiltration, ultrafiltration, or nanofiltration.
  • membranes of various natures, structures, and textures.
  • ceramic membranes In general, they are constituted by a porous substrate that provides the membrane with mechanical strength and that also gives it a shape, and thus determines the filter surface of the membrane.
  • One or more layers having a thickness of a few micrometers for performing separation are deposited on the substrate, which layers can be referred to as separator layers, filter layers, separation layers, or active layers.
  • separator layers filter layers
  • separation layers or active layers.
  • the filtered fluid is transferred through the separator layer and the fluid then spreads out in the porous texture of the substrate in order to go towards the outside wall of the porous substrate.
  • This portion of the fluid for treatment that has passed through the separator layer and the porous substrate is referred to as the permeate or the filtrate and it is recovered by a collector chamber or peripheral space surrounding the membrane and defined by a casing and plates for supporting the membranes.
  • the other portion is referred to as the retentate and it is usually reinjected into the fluid for treatment upstream from the membrane via a recirculation loop.
  • the substrate is initially fabricated with the desired shape by extrusion, and then sintered at a temperature and for a length of time that are sufficient to achieve the required strength, while nevertheless conserving in the resulting ceramic the desired open and interconnected texture of pores. That method makes it necessary to obtain one or more rectilinear channels within which the separator layers are subsequently deposited and sintered.
  • the substrates are conventionally tubular in shape and have one or more rectilinear channels arranged in parallel with the central axis of the substrate.
  • such membranes are used in a casing to form a filter module, which is thus constituted by a metal shell, usually of cylindrical shape, that is fitted at its ends with support plates having holes formed herein to receive the ends of the filter elements.
  • a filter module which is thus constituted by a metal shell, usually of cylindrical shape, that is fitted at its ends with support plates having holes formed herein to receive the ends of the filter elements.
  • the filter elements are positioned inside the casing, extending parallel to one another.
  • the filter elements are mounted in leaktight manner at each of their ends to the corresponding support plate via sealing gaskets.
  • casing means more precisely the assembly formed by a jacket, which is a generally cylindrical metal shell, fitted at each of its ends with a plate, more precisely referred to as a “head” plate, with holes formed therein to receive and position the ends of the filter elements in parallel inside the jacket.
  • Sealing between the filter elements and the head plate is obtained by a single gasket or by a plurality of individual gaskets.
  • prior art industrial modules come with gaskets of two types: namely single gaskets or individual gaskets.
  • a single gasket involves sealing all of the separator elements present in a casing by using a single part perforated by as many passages as there are separator elements.
  • the separator elements are arranged in parallel inside the casing and they are positioned by the head plate, which has a number of passages equal to the number of filter elements.
  • the filter elements project a little from the head plate, by a distance of the same order of magnitude as the thickness of the gasket.
  • a backing plate is placed for the purpose of compressing the gasket by means of clamping nuts.
  • the backing plate possesses passages of axes that coincide with the axes of the head plate. These passages are of diameter that is slightly smaller than the outside diameter of the filter elements.
  • the main parameters that contribute to designing this gasket are its thickness, defined by the portion of a filter element that penetrates inside the gasket, and also its hardness, as defined on the Shore hardness scale, that contributes to the flattening of the gasket while the backing plate is being clamped.
  • the combination of hardness and thickness serves to define an amount of flattening, on which sealing depends.
  • An individual gasket comprises a skirt that surrounds an end portion of a filter element.
  • the end portion of the skirt may be cylindrical or conical.
  • the skirt is extended by a top portion that covers a portion of the end of the filter element. This portion is arranged at the periphery of the end of the filter element and its inside diameter is determined so as to avoid obstructing the flow channels.
  • the casing includes a head plate with as many passages as there are filter elements. The shape and the dimensions of the passages are determined so as to receive the (cylindrical or conical) skirt of the gasket, thus avoiding any contact between the filter element and the metal of the head plate.
  • the top portion of the gasket is received in spot facing formed in the backing plate, with the depth of the spot facing being less than the top portion of the gasket.
  • Three main parameters contribute to making such individual gaskets: the shape of the skirt, the height of the top portion, and the Shore hardness of the gasket. Together these three parameters serve firstly to define an amount of flattening, on which sealing depends, and secondly to define the protection for the portion of the filter elements that passes through the head plate.
  • gaskets are made by plastics fabrication operations that require the fabrication of injection molds that are expensive and for which amortization contributes significantly to the cost price of a gasket.
  • one of the advantages of multichannel separator elements lies in obtaining channels of small hydraulic diameter without any risk of fragility for the separator elements, however the initial multichannel separator elements had channels that were exclusively of circular right section.
  • the skirt covering the outside portion of the filter element and providing sealing between the metal and the filter element is extended by a common plate for a single gasket or by an individual plate for an individual gasket.
  • the thickness of this skirt and of the web between two passages define this distance D on which the number of filter elements inside the casing depends directly.
  • This web is defined so as to provide the casing with mechanical strength, such as for example the ability to withstand an inside pressure of 10 bars.
  • the table below gives the number of separator elements and the number of individual gaskets for three industrial casings.
  • a separator module having a series of porous columns supported at one of their ends by an inlet plate and at their other end by an outlet plate.
  • the porous columns are fastened to the inlet and outlet plates, e.g. by sintering.
  • One of the drawbacks of such a module lies with the difficulty of making such an assembly when the values for the outside diameter and for the thickness of the porous columns are very small. Specifically, the brittleness of ceramics together with the small dimensions of the columns mean that they are very fragile, which industrially speaking puts considerable limits on making a separator module having a large number of such columns.
  • One solution consists in making assemblies in which the number is limited to a few tens, but it is then necessary to assemble together the resulting mini-modules in order to obtain a separator module having an equivalent filter surface area. Unfortunately, assembling such mini-modules together leads to a major loss of volume because of the space between the mini-modules, thereby reducing the compactness of the assembly.
  • the present invention seeks to remedy the drawbacks of the prior art by proposing a novel single-piece separator element for obtaining molecular and/or particulate separation by tangentially filtering a fluid medium, and designed to improve compactness, i.e. the ratio of the filter surface area divided by the total inside volume of the casing (which ratio is expressed in m 2 /m 3 ), the novel element also serving to simplify the modules by reducing the number of gaskets needed and by eliminating the need to have head plates.
  • the compactness in the casings is increased, for given hydraulic diameter, by a factor of at least 1.2, and preferably greater than 1.5, compared with the prior art and using conventional single-channel and multichannel separator elements.
  • the invention provides a separator element for obtaining molecular and/or particulate separation of a fluid medium for treatment into a filtrate and a retentate, the element comprising a structure of at least two porous rigid columns made of the same material, positioned side by side to define outside their outside walls a volume for recovering the filtrate, each column presenting internally at least one open structure for passing a flow of the fluid medium, opening out in one of the ends of the porous column for inlet of the fluid medium for treatment and in the other end for outlet of the retentate, the element being characterized in that said porous columns are secured to one another at their ends by means of an inlet plate and an outlet plate, said plates not being separate parts fitted on the porous columns in order to form together said single-piece structure.
  • the subject matter of the invention is to propose a separator module using a single-piece separator element in accordance with the invention by optimizing the distance between the porous columns and the thickness of the material of the porous columns, it is possible to obtain increased compactness expressed in m 2 /m 3 , for given hydraulic diameter, compared with prior art single-channel and multichannel separator elements.
  • the single-piece separator element of the invention also includes in combination one and/or more of the following additional characteristics:
  • the invention also proposes a separator module for obtaining molecular and/or particulate separation of a fluid medium for treatment into a filtrate and a retentate, the device comprising a casing containing at least one single-piece element in accordance with the invention in which each plate is mounted in a sealing gasket.
  • FIG. 1 is a perspective view of a first embodiment of a separator element in accordance with the invention.
  • FIGS. 1A and 1B are cross-section views taken respectively on lines A-A and B-B of the separator element shown in FIG. 1 .
  • FIG. 2 is a perspective view of another embodiment of a separator element in accordance with the invention in which the porous columns are intertwined.
  • FIG. 3 is a section view in elevation showing the principle of mounting a separator element in accordance with the invention of the kind shown in FIG. 1 inside a casing.
  • FIG. 3A is a cross-section view on line A-A of FIG. 3 .
  • FIG. 4 is a perspective view of another embodiment of a separator element in accordance with the invention in which each porous column has seven channels.
  • FIGS. 4A and 4B are cross-section views taken respectively on lines A-A and B-B of the separator element shown in FIG. 4 .
  • FIGS. 6A to 6C show compactness (plotted up the ordinate axis in m 2 /m 3 ) obtained with separator elements in accordance with the invention mounted in a DN 200 casing as a function of the distance d (plotted along the abscissa axis in mm) between the porous columns that are provided with a single channel or with a plurality of channels in comparison with a prior art industrial configuration of equivalent hydraulic diameter taken as a reference (horizontal line), the hydraulic diameters being equal respectively to 3.47 mm, 2.3 mm, and 1.6 mm.
  • FIGS. 7A to 7E show compactness (plotted up the ordinate axis in m 2 /m 3 ) obtained for separator elements in accordance with the invention mounted in DN 100 and DN 350 casings, as a function of the distance d (plotted up the abscissa axis in mm) between porous columns provided respectively with one channel, seven, 23, 29, and 93 channels, and respectively for hydraulic diameters equal to 6 mm, 6 mm, 3.5 mm, 2.5 mm, and 1.6 mm.
  • mean pore diameter is used to mean the d50 value of a volume distribution at which 50% of the total volume of the pores corresponds to the volume of pores having a diameter less than this d50.
  • the volume distribution is the curve (analytic function) representing the frequencies of pore volumes as a function of their diameters.
  • d50 corresponds to the median separating into two equal portions the area situated under the curve of frequencies as obtained by mercury penetration for mean pore diameters greater than or equal to 4 nanometers (nm), or as obtained by adsorbing gas, in particular N 2 , when the mean pore diameters are less than 4 nm, these two techniques being retained as references in the context of the invention for measuring mean pore diameters.
  • the invention provides separator elements for obtaining molecular and/or particulate separation of a fluid medium by tangential filtering, which elements are commonly referred to as filter membranes.
  • a separator element 1 comprises a monolithic or single-piece rigid structure 2 .
  • a single-piece structure is defined as being made of a single piece that is uniform and continuous throughout, having no bonds nor any exogenous additions.
  • no component portion of the single-piece structure is a separate fitting, i.e. the single-piece structure is fabricated in a single operation such that the single-piece structure can be used directly for depositing separator layers or requires no more than single heat treatment.
  • the single-piece structure 2 comprises at least two porous rigid columns 3 made of the same porous material (there being three columns in the example shown in FIG. 1 ) which columns are placed beside one another in order to define a peripheral space 4 for recovering filtrate located outside their outer walls.
  • Each porous column 3 forms a rigid porous substrate presenting a generally elongate shape extending from a first end 3 1 to a second end 3 2 opposite from the first end.
  • Each porous column 3 includes internally at least one open structure 5 for passing a flow of the fluid medium for treatment, opening out at the first end 3 1 of the porous column for inlet of the fluid medium for treatment and at the second end 3 2 of the porous column for outlet of the retentate.
  • the open structure 5 which in the example shown is in the form of a channel, corresponds to an empty space for passing the flow of the fluid medium, i.e. a zone of the porous column 3 that does not contain porous material.
  • each porous column 3 defining the open structure or channel 5 presents a surface that is covered by at least one separator layer C that is to come into contact with the fluid medium for treatment that flows inside the open structure 5 .
  • a portion of the fluid medium passes through the separator layer C and the porous material of the porous column 3 such that this treated portion of the fluid, referred to as filtrate or permeate, flows through out through the outer wall 3 a of each porous column.
  • the filtrate is recovered in the peripheral space 4 of the porous structure by any appropriate means.
  • Each porous column 3 thus possesses a peripheral wall of thickness e between the open structure 5 and its outer wall 3 a.
  • the porous columns 3 are secured to one another at least at their neighboring first ends by means of an inlet plate 7 , and at their neighboring second ends by means of an outlet plate 8 .
  • Each plate 7 , 8 provides a mechanical assembly connection between the porous columns 3 , with the inlet plate 7 providing the connection between the porous rigid columns 3 at their first ends 3 1 and with the outlet plate 8 providing the connection between the porous rigid columns at their second ends 3 2 .
  • the plates 7 , 8 are not separate parts fitted onto the porous columns, i.e. together they form said single-piece structure.
  • the porous columns 3 and the plates 7 , 8 are fabricated in a single operation such that the resulting single-piece structure 2 is directly usable for depositing separator layers C for the fluid medium for treatment or requires no more than single heat treatment.
  • Each plate 7 , 8 possesses a respective inside face 7 1 , 8 1 facing towards and in contact with the peripheral space 4 of the porous structure, and a respective outside face 7 2 facing towards and in contact with the fluid medium for treatment, or 8 2 facing towards and in contact with the retentate.
  • the inlet and outlet plates 7 , 8 which possess respective perimeters 7 3 , 8 3 of thickness that varies as a function of the desired mechanical strength, present a right section appropriate for enabling them to be mounted in a casing, as can be better understood from the description below.
  • the plates 7 , 8 possesses a right section that is circular, however it is clear that the right section of these plates could be different, i.e. non-circular.
  • the porous columns 3 are also secured to one another by means of at least one connection bridge 9 serving to stiffen the porous columns 3 together, while ensuring that a constant spacing is conserved between the porous columns 3 .
  • connection bridges 9 are made locally with any appropriate shape, being distributed preferably regularly between the plates.
  • connection bridges 9 are made of the same material as the porous columns.
  • the porous columns 3 , the inlet and outlet plates 7 and 8 , and the connection bridges 9 together form a single-piece structure.
  • Such single-piece structures 2 that cannot be made by conventional extrusion techniques can be made preferably by additive techniques such as that described by way of example in patent application FR 3 006 606.
  • additive method of fabrication it is considered that the plates and columns are said not to be separate parts fitted to one another if fabrication enables the plates 7 , 8 and the porous columns 3 to be shaped in such a manner that the resulting single-piece structure 2 can be used directly for depositing layers or requires no more than single heat treatment.
  • the entire single-piece structure is constructed by superposing mutually connected elementary layers by projecting a liquid in fine droplets or by supplying energy, with first consolidation heat treatment being essential when using the first method; while with the second method the interaction between energy and material is normally sufficient to lead either to sintering or else to melting and/or solidification of the material.
  • Heat treatment is essential particularly when the localized delivery of liquid is performed using microdroplets created with a piezoelectric element, which droplets are possibly charged and directed in an electrostatic field; the liquid is a binder or an agent for activating binder that has previously been added to the ceramic powder.
  • Such single-piece structures 2 may also be made for example by the casting technique, which requires operations of making a mold, of preparing a suspension for casting, of casting proper, of drying, of unmolding, and of heat treatment to obtain the porosity and the strength of the single-piece structure.
  • the porous columns 3 present a porous texture that is continuous throughout the volume of the porous columns.
  • This porous texture is characterized by the mean diameter of the pores as deduced from their distribution as measured by mercury penetration porometry.
  • the porous texture of the porous columns 3 is open and forms a network of interconnected pores, thus enabling the fluid that has filtered through the filter separator layer to pass through the porous structure and be recovered by the peripheral space 4 of the porous structure. It is common practice to measure the permeability to water of the porous structure in order to qualify the hydraulic resistance of the porous structure, which simultaneously makes it possible to confirm that the porous texture is interconnected. Specifically, in a porous medium, the steady flow of an incompressible viscous fluid is governed by Darcy's law.
  • the speed of the fluid is proportional to the pressure gradient and inversely proportional to the dynamic viscosity of the fluid, via a characteristic parameter known as “permeability” that may be measured, for example, in compliance with French standard NF X 45-101, of December 1996.
  • the porous columns 3 are made of a non-metallic inorganic material.
  • the porous columns 3 are made of a ceramic, selected from among oxides, nitrides, carbides, and other ceramic materials, and mixtures thereof, and in particular from titanium oxide, alumina, zirconia, and mixtures thereof, titanium nitride, aluminum nitride, boron nitride, and silicon carbide, possibly mixed with some other ceramic material.
  • the porous structure may also be made out of an organic material or out of an inorganic material that is purely metallic.
  • the porous columns 3 may be made of a pure metal such as aluminum, zinc, copper, or titanium or in the form of an alloy of a plurality of these metals, or of stainless steels.
  • the material constituting the porous columns 3 may present a mean pore diameter lying in the range 1 micrometer ( ⁇ m) to 100 ⁇ m.
  • the porous columns 3 and the plates 7 , 8 are made out of the same material with identity and continuity of material and porous texture between the plates and the porous columns 3 .
  • the porosity of the material constituting the porous columns 3 and the plates 7 , 8 is identical.
  • each plate 7 , 8 is made in the form of a solid element so as to form a solid plate of section covering all of the sections of the porous columns 3 .
  • the plates 7 , 8 thus close the peripheral space 4 of the porous structure, thereby confining the filtrate.
  • Each plate 7 , 8 has an outside face 7 2 , 8 2 in contact respectively with the fluid medium for treatment and with the retentate, these outside faces 7 2 , 8 2 being sealed so as to avoid the fluid medium for treatment and the retentate penetrating into the plates.
  • the outside faces 7 2 , 8 2 of the plates 7 , 8 may be sealed in any appropriate manner.
  • the outside faces 7 2 , 8 2 of the plates 7 , 8 may be sealed by densification up to a value equal or very close to the intrinsic density of the material or by impregnation or by depositing an additional material other than the material of the plate.
  • the separator element 1 in accordance with the invention is for use in a separator module 11 of any known type.
  • the separator module 11 comprises a casing 12 of tubular shape in which one or more separator elements 1 are mounted.
  • the separator module 11 is mounted so that the inlet and outlet plates 7 and 8 are located at the ends of the casing 12 .
  • These inlet and outlet plates 7 and 8 are mounted in sealed manner to the casing 12 via sealing gaskets 14 .
  • These sealing gaskets 14 are mounted in any appropriate manner on the casing, either directly at the ends of the casing or else in holes formed in separate support plates that are fastened to the ends of the casing.
  • the porous columns 3 are thus positioned inside the casing 12 , which is closed by the plates 7 , 8 and by the sealing gasket 14 optionally associated with the support plates.
  • the casing 12 thus co-operates with the outside walls 3 a of the porous columns 3 and the inside faces 7 1 , 8 1 of the plates to define the peripheral space 4 for recovering the filtrate.
  • the filtrate as confined in this way in the casing 12 is removed by any appropriate means, via an outlet 15 provided in the casing 12 .
  • the separator device 11 comprises a single separator element 1 having a number of porous columns 3 that is selected to obtain the desired filter surface area.
  • the separator device 11 may have a plurality of separator elements 1 in accordance with the invention. Under such circumstances, each separator element 1 is mounted in sealed manner in the casing 12 by using plates 7 , 8 provided with sealing gaskets 14 .
  • the fluid medium enters and leaves respectively via the inlet plate 7 and the outlet plate 8 of the single-piece structure 2 through separate openings forming the open structure 5 that has three channels in the example shown in FIG. 1 .
  • the separator filter layer C that covers the walls of each of the channels 5 serves to filter the fluid medium for treatment.
  • the separator filter layers C need to have a mean pore diameter that is less than the mean pore diameter of the porous columns 2 .
  • the separator layers define the surface of the tangential flow separator element that is to be in contact with the fluid for treatment and over which the fluid for treatment flows.
  • a prior art tangential flow separator element generally presents a length in the range 1 meter (m) to 1.5 m.
  • the section of a tangential flow separator element usually presents an area lying in the range 0.8 square centimeters (cm 2 ) to 14 cm 2 .
  • the single-piece columnar-structure separator elements present a length of several centimeters to several meters, preferably lying in the range 5 cm to 5 m.
  • the section of a single-piece columnar-structure separator element depends on the number of columns and on the distance between the columns, and it may lie in the range a few centimeters to a few meters.
  • the thicknesses of the separator filter layers typically lie in the range 1 ⁇ m to 100 ⁇ m.
  • a separator layer in order to perform its separator function, and act as an active layer, presents a mean pore diameter that is less than the mean diameter of the pores of the porous column.
  • the mean pore diameter of the separator filter layers is less than the mean pore diameter of the porous column by a factor of at least 3, and preferably by a factor of at least 5.
  • the micro- or ultrafiltration layer is deposited directly on the porous column (a single-layer separator layer), or indeed on an intermediate layer of smaller mean pore diameter, itself deposited directly on the porous column.
  • the separator layer may be based on or constituted exclusively by one or more metallic oxides, carbides, or nitrides, or other ceramics.
  • the separator layer could be based on or constituted exclusively by TiO 2 , Al 2 O 3 , and ZrO 2 , singly or in a mixture.
  • each porous column 3 advantageously possesses a single channel.
  • the porous support has a plurality of channels, mention may be made to arrange the channels 5 so as to create within each porous column at least two flow circuits for the fluid medium that are not mutually interconnected between the inlet and outlet ends of the porous column.
  • each channel 3 extends from the inlet to the outlet of the porous column without being connected to another channel.
  • FIGS. 4, 4A, and 4B show such an embodiment in which each porous column 3 possesses seven channels 5 arranged independently of one another in the inlet plate 7 and going to the outlet plate 8 .
  • the number of channels per porous column may be different from the example shown.
  • An advantage of the subject matter of the invention is to enable the compactness of separator elements to be improved once they have been mounted in a casing.
  • Table 1 below gives compactness in m 2 /m 3 for various separator membranes mounted in a DN 200 cylindrical casing having an inside diameter of 213 mm.
  • the separator membranes are of sections that are either circular or else hexagonal, presenting a determined number of channels 5 of circular section or of non-circular section, and presenting a hydraulic diameter Dh.
  • These compactness values are given as a function of the distance d (plotted along the abscissa axis in mm, with decreasing values).
  • the 2 mm maximum distance d between columns corresponds to the distance that, in the prior art, lies between filter elements having an outside diameter of 10 mm when they are installed in such industrial casings.
  • Compactness is compared with a reference compactness (horizontal line) for a prior art industrial configuration made up of multichannel membranes having an outside diameter of 25 mm, and with an equivalent hydraulic diameter.
  • the separator elements of the invention make it possible to obtain compactnesses that are greater depending on the value of the distance d between the porous columns 3 , with this applying up to a certain limit value for the hydraulic diameter Dh, which is close to 2.3 mm.
  • FIGS. 6A to 6C show compactness (plotted up the ordinate in m 2 /m 3 ) obtained with separator elements 1 in accordance with the invention mounted in a DN 200 casing, as a function of the distance d (plotted up the abscissa axis and in mm, with increasing values), between porous columns 3 having only one channel or a plurality of channels, and in comparison with a prior art industrial configuration of equivalent hydraulic diameter taken as a reference (horizontal line).
  • the separator elements of the invention In general manner, when the porous columns possess more channels, in comparison with prior art industrial configurations using multichannel circular membranes with equivalent hydraulic diameters, the separator elements of the invention always enable compactnesses to be obtained that are greater, providing the distance d is less than 8.1 mm.
  • the maximum distance d between the porous columns of 8.1 mm corresponds to the distance that, in the prior art, lies between filter elements having an outside diameter of 25 mm when they are installed in such industrial casings.
  • the maximum distance d between the porous columns of 8.1 mm corresponds to the distance that, in the prior art, lies between filter elements having an outside diameter of 25 mm when they are installed in such industrial casings.
  • the maximum distance d between the porous columns of 8.1 mm corresponds to the distance that, in the prior art, lies between filter elements having an outside diameter of 25 mm when they are installed in such industrial casings.
  • the maximum distance d between the porous columns of 8.1 mm corresponds to the distance that, in the prior art, lies between filter elements having an outside diameter of 25 mm when they are installed in such industrial casings.
  • each porous column 3 has one or more channels 5
  • the thickness e of the porous material preferably lies in the range 0.250 mm to 2.500 mm
  • the distance d between the porous columns 3 preferably lies in the range 0.250 mm to 5.000 mm.
  • Another advantage of the invention relates to simplifying mounting such a separator element 1 in accordance with the invention in a separator module 11 made in any conventional manner.
  • the presence of inlet and outlet plates serving to assemble a plurality of porous columns together also makes it easier to achieve sealing with the casing, and in particular serves to limit the number of sealing gaskets that need to be used compared with prior art solutions.
  • such a separator element 1 is mounted at the ends of the casing 12 using plates 7 , 8 .
  • respective sealing gaskets 14 are mounted on the periphery 7 3 , 8 3 of the plates 7 , 8 .
  • These two sealing gaskets 14 are mounted by any appropriate means relative to the ends of the casing so as to close the peripheral space 4 for recovering the filtrate that is removed from the casing via an outlet 15 or via any appropriate known means.
  • the separator device 11 has a single separator element 1 with a number of porous columns 3 that is selected so as to obtain the desired filter surface area.
  • the separator device 11 may have a plurality of separator elements 1 in accordance with the invention. Under such circumstances, each separator element 1 is mounted in sealed manner in the casing 12 using plates 7 , 8 provided with sealing gaskets 14 .
  • the porous columns 3 are all identical in shape.
  • all of the porous columns 3 are in the form of cylinders of circular section.
  • porous columns 3 are cylindrical in shape.
  • the section of the porous columns 3 may be circular or other.
  • the porous columns 3 possess identical transverse dimensions.
  • the thickness e of the porous columns 3 is identical for all of the porous columns 3 .
  • the rigid columns 3 possess outside shapes that are constant or that vary along their length, i.e. between the plates 7 , 8 .
  • These rigid columns 3 possess, optionally in combination with the above shape characteristic, transverse dimensions that are constant or that vary along their length.
  • each porous column is constructed by turning a circular or other section about its central axis, the generator section remaining either perpendicular to the central helix (coil), or horizontal (twisted column), or else vertical, i.e. parallel to the central axis (spiral staircase).
  • porous columns 3 are intertwined, as shown in FIG. 2 .

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Filtering Materials (AREA)
  • Cyclones (AREA)
US15/575,916 2015-05-29 2016-05-25 Single-piece column structure for the separation of a fluid medium Abandoned US20180147534A1 (en)

Applications Claiming Priority (3)

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FR1554913A FR3036628B1 (fr) 2015-05-29 2015-05-29 Structure colonnaire monobloc de separation d'un milieu fluide
FR1554913 2015-05-29
PCT/FR2016/051234 WO2016193574A1 (fr) 2015-05-29 2016-05-25 Structure colonnaire monobloc de séparation d'un milieu fluide

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US20230120148A1 (en) * 2021-10-20 2023-04-20 Irpi Llc Multiplex inertial filter, collector and separator
US11697095B2 (en) * 2016-12-21 2023-07-11 Technologies Avancees Et Membranes Industrielles Tangential flow separation element incorporating flexuous channels
EP4012394A4 (en) * 2019-08-05 2023-08-09 Hitachi High-Tech Corporation DEGASTER AND ELECTROLYTE MEASUREMENT SYSTEM

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DE102020121549A1 (de) * 2020-08-17 2022-02-17 InnoSpire Technologies GmbH Monolithisch aufgebaute Membranfilter
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US11779869B2 (en) * 2021-10-20 2023-10-10 Irpi Llc Multiplex inertial filter, collector and separator

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HUE044492T2 (hu) 2019-10-28
WO2016193574A1 (fr) 2016-12-08
FR3036628A1 (fr) 2016-12-02
BR112017024712B1 (pt) 2022-04-19
RU2710568C2 (ru) 2019-12-27
CN107810046B (zh) 2021-10-22
HK1250499A1 (zh) 2018-12-21
JP2018516168A (ja) 2018-06-21
EP3302767A1 (fr) 2018-04-11
CN107810046A (zh) 2018-03-16
EP3302767B1 (fr) 2019-05-08
ES2739879T3 (es) 2020-02-04
FR3036628B1 (fr) 2019-12-20
TR201910999T4 (tr) 2019-08-21
DK3302767T3 (da) 2019-08-12
JP6754776B2 (ja) 2020-09-16
PT3302767T (pt) 2019-08-21
RU2017146226A3 (hu) 2019-08-02
BR112017024712A2 (hu) 2018-08-21
RU2017146226A (ru) 2019-07-01

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