WO2022038095A1 - Filtre à membrane monolithique - Google Patents

Filtre à membrane monolithique Download PDF

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Publication number
WO2022038095A1
WO2022038095A1 PCT/EP2021/072744 EP2021072744W WO2022038095A1 WO 2022038095 A1 WO2022038095 A1 WO 2022038095A1 EP 2021072744 W EP2021072744 W EP 2021072744W WO 2022038095 A1 WO2022038095 A1 WO 2022038095A1
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WIPO (PCT)
Prior art keywords
porous
fluid
starting material
point
monolithic component
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PCT/EP2021/072744
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German (de)
English (en)
Inventor
Ulrich Meyer-Blumenroth
Gisela Jung
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InnoSpire Technologies GmbH
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Publication date
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Publication of WO2022038095A1 publication Critical patent/WO2022038095A1/fr

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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
    • B01D63/06—Tubular membrane modules
    • B01D63/069—Tubular membrane modules comprising a bundle of tubular membranes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B01D46/24—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies
    • B01D46/2403—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies characterised by the physical shape or structure of the filtering element
    • B01D46/2418—Honeycomb filters
    • B01D46/2451—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure
    • B01D46/2486—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure characterised by the shapes or configurations
    • B01D46/2496—Circular
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B01D46/24—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies
    • B01D46/2403—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies characterised by the physical shape or structure of the filtering element
    • B01D46/2418—Honeycomb filters
    • B01D46/2425—Honeycomb filters characterized by parameters related to the physical properties of the honeycomb structure material
    • B01D46/2429—Honeycomb filters characterized by parameters related to the physical properties of the honeycomb structure material of the honeycomb walls or cells
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B01D46/24—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies
    • B01D46/2403—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies characterised by the physical shape or structure of the filtering element
    • B01D46/2418—Honeycomb filters
    • B01D46/2425—Honeycomb filters characterized by parameters related to the physical properties of the honeycomb structure material
    • B01D46/24491—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
    • B01D—SEPARATION
    • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B01D46/24—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies
    • B01D46/2403—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies characterised by the physical shape or structure of the filtering element
    • B01D46/2418—Honeycomb filters
    • B01D46/2451—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure
    • B01D46/247—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure of the cells
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B01D46/24—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies
    • B01D46/2403—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies characterised by the physical shape or structure of the filtering element
    • B01D46/2418—Honeycomb filters
    • B01D46/2451—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure
    • B01D46/2476—Monolithic structures
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B01D46/24—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies
    • B01D46/2403—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies characterised by the physical shape or structure of the filtering element
    • B01D46/2418—Honeycomb filters
    • B01D46/2451—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure
    • B01D46/2484—Cell density, area or aspect ratio
    • 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
    • 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
    • B01D63/066—Tubular membrane modules with a porous block having membrane coated passages
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0002—Organic membrane manufacture
    • B01D67/0004—Organic membrane manufacture by agglomeration of particles
    • B01D67/00045—Organic membrane manufacture by agglomeration of particles 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
    • B01D67/0041—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
    • 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
    • B28B1/001—Rapid manufacturing of 3D objects by additive depositing, agglomerating or laminating of 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
    • C04B38/02—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding chemical blowing agents
    • 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
    • C04B2111/00034—Physico-chemical characteristics of the mixtures
    • C04B2111/00181—Mixtures specially adapted for three-dimensional printing (3DP), stereo-lithography or prototyping
    • 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
    • C04B2111/00241—Physical properties of the materials not provided for elsewhere in C04B2111/00
    • C04B2111/00284—Materials permeable to liquids
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00793—Uses not provided for elsewhere in C04B2111/00 as filters or diaphragms

Definitions

  • the present invention relates to a method for producing monolithic components and monolithic components produced using this method, in particular as membrane filters.
  • Membrane filters for filtering or separating substances from mostly liquid mixtures are known as such.
  • a mixture can be a disperse medium or, for example, a solution in which further components are dissolved in a base material.
  • Membrane filters are used in various areas of application, e.g. E.g. in the treatment of water and food, in the manufacture of pharmaceutical products, in biotechnological or chemical processes.
  • An example of such an application can be the separation of alcohol from beer to produce non-alcoholic beer. A particularly gentle process enables preferential alcohol removal with minimal impairment of taste.
  • Another application can be the separation of cells and cell fragments from active substance solutions in the biotechnological production of pharmaceuticals.
  • There is still an intensive search for further developments here for example to increase the throughput of the medium to be filtered or to further reduce costs. In contrast to medical apparatus, much larger membrane surfaces are required for technical systems.
  • membrane filters are nowadays manufactured as standardized products with a given geometry, whereby adaptations to special requirements from the process control, such as for high viscosities and/or low pressure losses during flow or for difficult installation environments, are practically impossible or not planned. since the resulting lower quantities would drive unit costs into regions that cannot be sold.
  • filter modules typically consist of different, in particular different, components that are produced using different methods and are then reversibly or irreversibly connected to one another.
  • the separate components include membranes as flatware or tubes, components for fluid supply and removal (e.g. pressure pipes, connectors, permeate pipes, aeration pipes, ...) and components for fluid distribution and mixing (e.g. spacers, ATD's,).
  • filter modules have been used which are provided in particular with sealing rings or other sealing means and are installed in a separate housing with separate connections.
  • the seal to avoid cross-flows between the envelope side and the lumen side is included complex and limits the possible areas of application for membrane filters to a decisive extent.
  • the membranes are bonded or welded to the other components to form a filter element.
  • Mechanical seals that can be clamped between the membranes and the housing can also be provided, e.g. B. common with ceramic membranes.
  • Connectors are often detachably connected to the filter unit, e.g. E.g. supply and discharge caps via clamps, flanges or threads. Seals prevent a "short circuit" between feed and filtrate.
  • Capillary membranes are usually glued into the housing. During the curing of the casting compound, the material can shrink as a result of the crosslinking reaction. The transition from the casting block to the housing of such a filter is therefore typically under tension, which in practical use under changing temperatures and/or pressures can lead to at least partial detachment of the casting compound from the housing wall. A reliable separation between the flow on the lumen side and the flow on the envelope side is therefore no longer guaranteed.
  • the present invention has therefore set itself the task of solving the aforementioned problems or at least introducing improvements thereto.
  • the invention has set itself the task of providing filter modules or membrane filters or components that are considerably more robust with regard to their handling, alternatively or cumulatively also with regard to the applicable process and operating parameters.
  • the invention solves the problem that the described aging processes of known filters are avoided or improved and that the number of failures of entire filter modules is reduced both in production and in operation.
  • the present invention also fulfills the partial aspect of providing filter modules or components that achieve further improved mixing of the fluids used and/or further increase the filtrate throughput.
  • the yield can be increased and/or the throughput quantity can be increased.
  • the present invention also provides a filter that can be adapted with simple means and that can be optimized in the manufacturing process for the specific later application with regard to, for example, the parameters of filtration capacity, delivery capacity, with regard to the volume or mass flow of fluid and/or the mechanical resilience or resistance to mechanical influences.
  • the invention has also set itself the task of simplifying the manufacturing process of filter modules and/or making it available more cost-effectively, or even individually adaptable to the specific requirement.
  • the present description is limited to the production of monolithic components and monolithic components produced using the method, which are produced using a novel method set up within the scope of the invention, also referred to below as the TiPS method. This is done in contrast to inorganic components that can be produced using other methods and also additively, and also to those polymeric components that can be produced using other methods but are not the subject of the present application or can be the subject of claims arising therefrom. These aspects are pursued further in further applications by the same applicant in order to be able to obtain additional and parallel protection thereon and are therefore not the subject of the present application for this reason as well.
  • the improvements and new designs proposed in this description concentrate on providing a component which is suitable for separating components from a fluid.
  • a separation is, for example, the filtration of a fluid, i.e. the extraction of substances from a solution, for example, or the stripping or separation of suspended matter from a disperse medium such as a suspension.
  • the invention is not limited to this.
  • the present invention also focuses on providing monolithic components which are produced using the method according to the invention, for the production of filter modules.
  • monolithic components such as membrane filters in particular, can be formed additively in the light of the present invention and/or have an intrinsic porosity.
  • all components can be provided from a uniform starting material.
  • monolithic components are typically manufactured in one piece and without interruption. Due to the lack of joined component-to-component transitions, they can be characterized by extreme robustness in the application and can also be optimized in terms of flow technology as well as their size and thus the filtration capacity for their intended use.
  • Additive manufacturing also allows, for example, the production of geometries that are not possible with previously known processes for membrane or membrane module production.
  • three-dimensional geometries should be emphasized that are prepared in such a way that a damping or force-absorbing shape can be kept ready.
  • the membrane module or modules are therefore preferably designed to be stress-tolerant, in particular longitudinal stress-tolerant.
  • the stress-tolerant design of the membrane tubes or membrane modules can also include a transverse stress-tolerant provision.
  • Membrane modules are also occasionally exposed to transverse stresses, for example if they are not inserted precisely into the respective holder and the membrane module compensates for the imprecise installation by twisting. This twisting can be transferred to the membrane tubes inside the membrane module.
  • porous material systems for additive manufacturing described in the present invention also allows, for example, the reproducible production of porous components with an average pore size of down to less than 1 m, which represents a challenge that has not been solved so far.
  • Previous attempts in this regard required an immense amount of time for a single filter due to the required high resolution, which is unacceptably long for series production.
  • the relationship between the achievable component size and the resolution of the component structure was an obstacle to the effect that such filters could not be produced in technically relevant sizes. Precisely this problem is solved particularly elegantly by the approach shown in the present description.
  • the geometric resolution that can be provided by an application device particularly preferably no longer represents an obstacle with regard to the achievable pore size.
  • the geometric resolution of the application device is then only for the general shape of the component or the membrane filter relevant, but not for the specific pore size of the membrane filter.
  • the method according to the invention for producing a component with an at least partially or at least regionally porous material structure, in particular as a filter element or filter device comprises a number of steps.
  • the step of providing a porous or porous starting material the starting material for the application is provided.
  • the starting material is provided using an extruder.
  • the starting material is already porous or it is provided in a porous form. This means that the starting material is not initially porous when it is provided, but is influenced, changed or composed differently in connection with the application of the starting material in such a way that the starting material can be interspersed with pores at the same time as the application of the starting material.
  • the provision of the porous or porous starting material means the transfer of a primary material to the component being produced.
  • the provision can also include conveying the porous or porous starting material to the site where the material is applied.
  • the provision can also include the thermal adaptation to desired application conditions, as well as the setting of an advantageous physical pressure at the moment of application of the starting material for the production of the component.
  • providing comprises conveying and pressing in the extruder screw, with the porous or porous starting material finally being provided at the outlet of the extruder.
  • the method according to the invention also includes the application of the porous or porous starting material for the construction of the component.
  • the method also includes adjusting the porosity of the porous or porous starting material.
  • the porosity is adjusted at the location of the material application. For example, this setting takes place immediately before, during or immediately after the specific application of material.
  • machine parameters of an application machine can be changed, such as an extruder, or a mixing ratio of the starting material can be changed, or process parameters can be adjusted during the solidification of the starting material in order to adjust the porosity at the site of material application.
  • the decisive factor here is that the material permeability is set intrinsically in the material in order to provide a corresponding filter performance. This means that a similar or better filter performance can be achieved than with conventional filter modules, and at the same time the production can be significantly more flexible and/or cheaper or materials can be used that were previously difficult to use for the production of filter modules because they could not be processed or were difficult to process Without the new manufacturing process, it would not have been possible to recognize that the corresponding filter performance could be achieved with it.
  • a little or no porous material can be provided in this way in order to build up parts of the housing of the component therefrom.
  • a porous material structure can be created elsewhere on the component.
  • the various component areas such as the housing and porous material structure in the aforementioned example, are constructed monolithically, ie in one piece with one another. It is therefore characteristic that there are no conventional component-to-component transitions, but rather areas of the component with different porosity can be built up, with all areas being produced together in one piece and typically bonded to one another, i.e. fused, baked, sintered or glued, for example are. The process is continued until the component is manufactured as a whole.
  • the additive manufacturing method for producing a component can comprise the application of the porous or porous starting material pointwise, linearly or in layers of the porous or porous starting material.
  • the starting material is preferably applied point by point, i.e. in particular point by point in a point target matrix, with the material being applied successively.
  • the material application can nevertheless be continuous or quasi-continuous, e.g. "caterpillar-shaped", and a point-target matrix can still be approached point by point, which can be described as a quasi-continuous material application.
  • the bottom layer can be applied in dots, lines or layers. Even the bottom layer is not necessarily a continuous layer, but rather it can include areas with and without material application.
  • the layer target matrix typically comprises target points in each application layer, into which the component to be produced and, if appropriate, intermediate spaces or cavities of the component to be produced are subdivided.
  • Such an application tool can be the extruder already mentioned, in which case the application tool can be moved in a three-dimensional manner to the point of the point-target matrix to be applied, or a component carrier is designed to be adjustable in such a way that a movable system of the point-target matrix is created, whereby the point-target matrix is shifted in front of the application tool and the point of the point-target matrix to be applied comes to rest on the application tool.
  • An application tool is preferably used when the starting material is in a liquid, pasty or solid form.
  • targeting a target point of the point target matrix means changing, preparing or positioning the target point of the point target matrix so that the starting material at the target point can be integrally bonded to the monolithic component.
  • the porous or porous starting material is preferably set, specifically at the point of the point-target matrix to be approached.
  • the setting of the porous and/or porous starting material can also take different forms. Adjusting the porous or porous starting material means, for example, adjusting a mixing ratio in the starting material if, for example, a filler is provided in a variable mixing ratio, the mixing ratio of the filler defining the porosity of the starting material.
  • the porosity of the starting material at the point to be specified in the point-target matrix is influenced, changed, composed or generally adjusted.
  • the porous or porous starting material adjusted in this way is preferably applied at the point.
  • the additive manufacturing method for producing a component can also include the step of approaching at least one first point of the point-target matrix and setting the porous or porous starting material at the at least one first point in such a way that a porous material structure is formed at the at least one first point .
  • the starting material is adjusted at the at least one first point, for example at a plurality of points that form a common area in the component, such that a porosity in the component can be adjusted in an additive manner.
  • a porous material structure is built up successively by approaching the point or points of the point-target matrix.
  • the method can also include the step of approaching at least one second point of the point-target matrix and adjusting the porous or porous starting material at the at least one second point in such a way that an impermeable material structure is formed at the second point.
  • the starting material is adjusted at this second point or at these second points, which form a region in the component, for example, such that the resulting structure has an impermeable structure.
  • a structure is impermeable, for example, which has comparatively few pores or no pores at all, or which is constructed with closed pores, so that no fluid exchange and/or mass exchange between fluids is ensured.
  • An impermeable structure within the meaning of the invention therefore preferably prevents a fluid from flowing through the impermeable material structure, but on the other hand also prevents in particular the exchange of substances from a first fluid on a first side of the impermeable material structure to a second fluid on a second side of the impermeable material structure.
  • An exemplary structure that can be advantageously constructed with an impermeable material structure is a casing around the component for protection of the same, as well as for the purpose of keeping an enveloping fluid in the component in particular and at the same time providing an enveloping side for the enveloping fluid.
  • the points of the point target matrix can be arranged in storage layers.
  • the point-target matrix can be approached in layers, so that first the points of a first storage layer are approached, it not having to be possible to approach all points of the first storage layer.
  • points of a second layer of deposits are then visited, again not requiring that all points of the second layer of deposits be visited; Rather, it is intended to provide cavities in a continuous form in the component.
  • Starting material include such that at least one storage layer areas with impermeable material structure.
  • the application can also be designed in such a way that at least one storage layer has areas with a porous material structure.
  • the application can also be designed in such a way that at least one storage layer has both an impermeable material structure and a porous material structure, which is applied with the same porous or porous starting material.
  • both an impermeable material structure and a porous material structure can be built up in a storage layer using the present method.
  • the basic idea of the present invention remains that all areas are monolithic, d. H. are integrally connected. Within the scope of this invention, it was possible to realize that areas with an impermeable material structure are constructed in one piece together with areas with a porous material structure. This can be achieved by adjusting the starting material at the point to be approached.
  • the application of the porous or porous starting material can be carried out in such a way that the partly or regionally porous material structure of the component is arranged or built up chaotically.
  • the porous material structure has a chaotic arrangement or a chaotic structure.
  • chaotic means that the specific microporous structure that is achieved with the application of the porous or porous starting material is not so exactly reproducible in its specific microporous design, that a component meets a second component at a specific point of the point target Matrix equals. Rather, the idea of the present invention is, at least in one aspect, that the specific pore structure is not defined exactly in the micrometer range, but is only adjusted with regard to the effect.
  • an achievable pore size can be set when the material is applied, but not the exact arrangement and structure of the pores achieved. In terms of technical effect, this is neither a difference nor a disadvantage.
  • the aspect has the advantage that an exact modeling of each individual pore can be dispensed with and only a desired porosity is set.
  • the specific arrangement of the pores in relation to one another is not important here.
  • the porosity created and provided in this way can therefore be described as intrinsic porosity.
  • the inventors have recognized that it is sufficient and particularly advantageous to provide such an intrinsic porosity, since this allows components to be produced considerably more quickly and at the same time more cost-effectively than with conceivable comparable methods.
  • the idea of adjusting the porosity of the starting material - in contrast to modeling each individual pore - can also be used with wet-precipitated flat membranes or capillary membranes made of polymers (NIPS). This can also be used in such a method, for example for polymer membranes that are produced by means of thermally induced phase inversion or phase separation (TiPS).
  • the partially or regionally porous material structure of the component can result from the application of the starting material in or on the component and can have a non-repetitive structure, i.e. a “chaotic” or “non-deterministic” structure or arrangement.
  • a non-repetitive structure i.e. a “chaotic” or “non-deterministic” structure or arrangement.
  • the structure or construction of the porous material structure cannot be repeated in such a way that an exactly identical pore arrangement could be achieved by repeating the component production. Rather, a second component will have a comparable porosity with regard to a comparison to the first component at a specific point of the point target matrix, the porosity being set or adjustable in the method according to the invention, but not the exact pore distribution and arrangement in the component.
  • the starting material can therefore preferably be made or prepared to be intrinsically porous. In other words, it is particularly advantageous not to precisely adjust the position of each pore with the method according to the invention or with the application machine according to the invention, but rather the
  • the porous material structure preferably has an open porosity.
  • the impermeable material structure can have closed porosity or no porosity at all, in any case no open porosity.
  • the porous material structure can have an open microporous or mesoporous structure.
  • the average pore size can be less than 40 ⁇ m, preferably less than 5 ⁇ m and more preferably even less than 1 ⁇ m. Such mean pore sizes have not been achieved with comparable processes to date.
  • the porous material structure preferably has an average volume porosity of 20% or greater, preferably 35% or greater. Depending on the manufacturing process, the average volume porosity can even reach 50% or more.
  • the impermeable material structure can have a higher density than the porous material structure.
  • the ratio of the density of the impermeable material structure to that of the porous material structure is in particular 1.2: 1, preferably 1.5: 1 and even more preferably 2: 1.
  • the material structure is denser in impermeable areas than in Areas of porous material structure.
  • the ratio of the density of the impermeable material structure to the porous material structure can also be specified in intervals, for example in an interval between 1.2:1 to 1.5:1 and preferably in the interval from 1.5:1 to 2:1 .
  • the step of adjusting the porosity of the porous or porous starting material can include, for example, adding additives or fillers to the starting material to adjust the porosity at the moment the material is applied. In particular, this is carried out at the point of the point-target matrix to be approached in each case.
  • the adjusting step can also include the selection of a starting material to be used from a plurality of at least two starting materials, wherein the at least two starting materials can be supplied alternately or simultaneously.
  • this can be designed in such a way that the at least two starting materials are provided at the point of the point target matrix to be approached in each case in order to produce the monolithic component.
  • the pores can also be provided to have a rounded or potato-shaped single structure.
  • the porous material structure of the component can be constructed and/or arranged in such a way that it is suitable for separating an envelope side from a carrier side in a permeable manner.
  • the component is prepared in such a way that the porous material structure forms an envelope side on its first side and a carrier side on its second side.
  • the porous material structure can be referred to as a membrane, with the membrane having two flat sides and the first flat side being swept by an enveloping fluid, with the second flat side being swept by a carrier fluid.
  • a monolithic component is also described within the scope of the invention, in particular as a device for separating components from a fluid, further in particular produced by the method as described above.
  • the monolithic component comprises a first and a second end face opposite the first end face.
  • a porous structure is arranged between the first and the second end face, which is built up and connected in one piece with the end faces.
  • the porous structure is designed to be permeable in some areas or at least in part.
  • the porous structure is also prepared and arranged in such a way that an envelope side can be separated from a carrier side at least partially and/or at least in regions in a permeable manner.
  • a carrier fluid can be provided on the carrier side.
  • the porous structure is designed to ensure mass transfer of the carrier fluid with the shell side.
  • a mass transfer means in particular a transfer from the carrier fluid into an enveloping fluid and/or from an enveloping fluid into the carrier fluid.
  • the monolithic component can be designed as a membrane element for a filter device or as a filter device as a whole.
  • the filter device is then constructed monolithically with the porous structure as a membrane element.
  • the monolithic component can further comprise a housing monolithically formed with the porous structure and the first and second faces.
  • the porous structure is preferably surrounded by the housing together with the first and second end faces.
  • An enveloping fluid can preferably be provided on the enveloping side of the monolithic component, so that both the carrier fluid and the enveloping fluid can flow in or through the monolithic component.
  • the carrier fluid is then separated from the sheath fluid by means of the porous structure.
  • the monolithic component can also be provided in such a way that the porous structure is designed to be semipermeable or selectively permeable.
  • the monolithic component can be prepared in such a way that it is set up for substances and/or particles with a size smaller than 10 ⁇ m, preferably smaller than 2 ⁇ m and more preferably smaller than 0.5 ⁇ m, for which the porous structure permeable, semi-permeable or selectively permeable.
  • the monolithic component can be prepared for receiving and discharging the carrier fluid on the carrier side and a sheath fluid on the sheath side.
  • the carrier fluid as well as the sheath fluid can then flow through the monolithic component to provide a carrier flow and a sheath flow in the monolithic component.
  • the porous structure of the monolithic component can include filter capillaries, in particular membrane capillaries.
  • the first end face of the monolithic component can be designed in the form of a plate.
  • the porous structure is formed in one piece on the first end face, ie in particular formed integrally together with the first end face.
  • the porous structure is then monolithic, i. H. formed integrally with the first end face.
  • the first end face and the porous structure consist of the same material.
  • the second end face can also be designed in the form of a plate.
  • the porous structure can be formed in one piece on the second end face, in particular formed integrally with the second end face.
  • the porous structure may comprise a plurality of elongate membrane tubes or filter capillaries.
  • the membrane tubes or filter capillaries connect the first end face of the monolithic component to the second end face in one piece and preferably integrally.
  • the membrane tubes or filter capillaries preferably have an inside.
  • the inside of the membrane tubes or filter capillaries form the carrier side.
  • the carrier fluid can therefore flow along the inside.
  • Membrane tubes or filter capillaries are particularly preferably tubular, so that the carrier side is formed in the tubular structure and the carrier fluid flows there.
  • the membrane tubes or filter capillaries preferably form the shell side on their outsides. The sheath fluid can therefore flow along the outside.
  • the membrane tubes or filter capillaries typically have a tubular or tubular design.
  • the diameter of the tubular or tubular configuration can vary along the length.
  • the membrane tubes or filter capillaries are preferably essentially straight and tubular.
  • the membrane tubes or filter capillaries are designed to be stress-tolerant, in particular longitudinal stress-tolerant, but also transverse stress-tolerant. If the first end and the second end are arranged parallel to one another, a longitudinal tension may imply a force application to the membrane tubes or filter capillaries, in which the end faces remain arranged parallel to one another, but possibly are shifted parallel; A longitudinal stress that increases beyond a certain point can therefore result in a evasive movement of the end faces towards one another. In this case, the membrane tubes or filter capillaries are subjected to a force along their main extension direction, that is to say they are typically compressed, but also lengthened. The membrane tubes or filter capillaries can break.
  • a transverse stress can imply that a force is applied to the membrane tubes or filter capillaries, in which case the end faces are tilted relative to one another, ie a force is applied perpendicularly to the main direction of extension of the membrane tubes or filter capillaries.
  • the membrane tubes or filter capillaries are designed to be stress-tolerant, they can be subjected to a higher degree of longitudinal stress and/or transverse stress than a comparable straight membrane tube or filter capillary.
  • the geometry of the membrane tubes or filter capillaries is constructed in such a way that a higher longitudinal stress or transverse stress can be absorbed without the membrane tubes or filter capillaries breaking.
  • a membrane tube or a filter capillary that is designed to be stress-tolerant is a spring-like compressible membrane tube or filter capillary.
  • the membrane tube or the filter capillary can be compressed by 1 mm or more without being damaged or destroyed, preferably by 2 mm or more, more preferably by 5 mm or more, even more preferably by 10 mm or more, finally preferred by 20 mm or more.
  • the length change tolerance - i.e.
  • the length change that results when voltage is applied due to the voltage tolerance of the membrane tube or filter capillary - 0.1% of the original length or more, preferably 0.2% or more, more preferably 0.5% or more, even more preferably 1% or more, and finally 2% or more of the original length of the membrane tube or the filter capillary.
  • Stress-tolerant can also be understood as elastic, stress-distributing or stress-reducing, because stress peaks in inelastic areas are distributed over a larger component area, but may even be reduced overall if the component allows deformation as a result. It is particularly preferred that the membrane tubes or filter capillaries are designed to dissipate stress, because if the membrane tubes or filter capillaries can yield under the application of force, e.g. compress like a spring, and at the same time the component housing is designed to be sufficiently rigid, then the applied stress, e.g. the compressive stress, can be derived from the component housing and be accommodated by it.
  • force e.g. compress like a spring
  • the membrane tubes or filter capillaries can extend helically or helically, in particular as a double helix or triple helix, in which two or three membrane tubes or filter capillaries run around one another.
  • a helical or helical extension of the membrane tubes or filter capillaries has several advantages. This intensifies the mass transfer on the inside of the membrane tube or the filter capillary; the resistance to external mechanical influences, such as a shock or torsion of the component, is also improved. This represents a suitable design for equipping the membrane tubes or filter capillaries to be stress-tolerant, as described above.
  • the membrane tubes or filter capillaries preferably each have a first or second opening through which a fluid can flow.
  • the mouth is preferably designed integrally with the first or second end face. In other words, the first or second end face merges in one piece from a flat extension into the mouth.
  • the orifice can have a flow-guiding surface configuration.
  • the flow-guiding surface design reduces flow resistances for a fluid flowing through, for example by avoiding or reducing turbulence and/or pressure fluctuations in the course of the flow.
  • Such a flow-guiding surface design of the orifice can have, for example, a conical, cone-shaped, parabolic or torus-shaped inner surface design.
  • the flow-guiding surface configuration is concentric around the orifice arranged around and integrally embedded in the first or second face. In other words, the mouth merges into the first or second end face in one piece.
  • the monolithic component can further include a first carrier fluid collection port formed monolithically with the first end face and the porous structure.
  • the first carrier fluid collection port is in particular an inlet for the carrier fluid.
  • the monolithic component can also comprise a second carrier fluid collection connection which is constructed monolithically with the second end face and the porous structure, ie in particular an outlet.
  • the monolithic component can comprise a sheath fluid connection formed monolithically with the porous structure.
  • the enveloping fluid connection can also be formed monolithically together with the porous structure via the first or second end face.
  • the porous structure can have at least one connection, cross-connection or stiffening made monolithically with the porous structure in order to increase the mechanical stability of the porous structure.
  • connection, cross-connection or stiffener may directly integrally connect the porous structure to the housing.
  • connection, cross-connection or reinforcement can be arranged in such a way that it directly and immediately connects the porous structure to the housing, ie the latter is arranged between the porous structure and the housing.
  • the connection, cross-connection or stiffener can also connect porous structures to one another, for example when a plurality of porous structures together define a filter element.
  • the porous structure can have at least one turbulator for mixing the carrier fluid and/or for mixing the enveloping fluid.
  • a turbulator can provide turbulence in the corresponding fluid, so that there is improved mixing and thus an improved mass transfer between the enveloping fluid and the carrier fluid.
  • the porous structure can provide a flow cross section that is variable over the length for the carrier fluid and/or the sheath fluid.
  • the porous structure has a higher or lower porosity and/or pore size distribution in some areas or in parts.
  • the porous structure can have impermeable areas, permeable areas and other areas that have a different porosity compared to both the impermeable areas and the permeable areas.
  • Such a further different range of porosity can be materialized in such a way that, for example, a type of coating is carried out on the inner surface inside the membrane capillaries.
  • the coating can be applied monolithically from the same starting material.
  • the first and/or the second end face has an integral fluid barrier or is designed as an integral fluid barrier, with the fluid barrier separating the flow of the carrier fluid from the enveloping flow.
  • the use of potting compound is completely avoided here, so that the associated disadvantages are eliminated.
  • the monolithic component is preferably made up entirely of the porous or porous starting material.
  • the porous or porous starting material has inorganic components, ie in particular metallic and/or ceramic components, in particular provided as a ceramic paste or metallic paste.
  • the starting material also has polymers, in particular provided as polymer particles or polymer paste, including, for example, polypropylene or polyvinylidene fluoride (PVDF) or polyether sulfone (PES), polysulfone (PSU), polyamide (PA), polyacrylonitrile (PAN), peloyether ether ketone (PEEK), polyethylene terephthalate ( PET) or the like.
  • the starting material can also comprise a polymer-solvent mixture, for example in molten form.
  • the porous or porous starting material can also be provided as a polymer solution with inorganic fillers, e.g. metallic and/or ceramic fillers.
  • the invention also includes a monolithic component which is produced using a method as described above.
  • the invention also describes a monolithic filter module for a device for separating components from a fluid.
  • the filter module of monolithic construction comprises a first end face and a second end face lying opposite the first.
  • the filter module also includes a filter housing, in particular an elongate or tubular one, formed in one piece with the first and second end faces.
  • the filter module also has a porous structure which is arranged in the filter housing and is constructed and connected in one piece to the end faces and the filter housing. In any case, the porous structure is designed to be permeable in part or in certain areas.
  • the filter module also has at least one carrier fluid collection port and at least one sheath fluid port. The first end face and the second end face of the filter module are each designed as an integral fluid barrier to prevent a cross flow between the carrier fluid collection port and the sheath fluid collection port.
  • the porous structure is prepared and arranged in such a way that an envelope side is separated from a carrier side in an at least partially and/or at least regionally permeable manner.
  • a carrier fluid can be provided on the carrier side.
  • the porous structure is prepared in such a way that mass transfer of the carrier fluid with the shell side is ensured.
  • FIG. 8 shows a perspective representation of a monolithic component with membrane tubes arranged to form triple helixes
  • Fig. 12a - 12e monolithic component with internals or internal structures (static mixer)
  • Fig. 15 example scheme for various process sequences for the production of a monolithic polymeric filter module
  • Fig. 18 system with two selectable application devices
  • Fig. 22 washing bath for washing out production aids.
  • a first embodiment of a monolithic component 50 which has a first end face 2 and a second end face 2a and a bundle of membrane tubes 1.
  • FIG. The two end faces 2, 2a are constructed in one piece with the membrane tubes 1 and are directly connected.
  • the membrane tubes 1 and end plates 2 are successively manufactured in one process step. A subsequent connection by joining, welding, gluing, clamping or the like is in particular not required or not produced.
  • the end plates 2 and membrane tubes 1 are made of the same, similar, but at least compatible material, so that the end plates 2 and membrane tubes 1 can be built in one piece.
  • the membrane tubes 1 have membrane inlets 3, which merge into the respective end face 2, 2a.
  • the membrane inlets 3 are therefore at the same time part of the respective membrane tube 1 as well as part of the respective end face 2, 2a.
  • the membrane inlets 3 therefore also represent the respective connection point between the membrane tube 1 and the end plate 2, 2a, so that mechanical forces can possibly also act on the membrane inlet.
  • the membrane inlet 3 can therefore also be optimized in terms of mechanical resistance in order to reduce the tendency to fracture in the area of the transition from the end face 2, 2a to the respective membrane tube 1.
  • the membrane tubes 1 together form the membrane or the membrane filter 60a.
  • FIG. 1a shows a detail of the end face 2a, as shown in FIG.
  • the diaphragm inlets 3 are designed in a hydraulically favorable rounded manner with a rounded Funnel area 4a.
  • the rounded transitions 4a from the membrane tubes 1 to the end faces 2, 2a also ensure a mechanically favorable coupling of the membrane tubes 1 to the respective end plate 2, 2a.
  • FIG. 2 shows a cross-sectional view of a longitudinal section through the monolithic component 50 along the line marked A-A in FIG. 2b.
  • FIG 2b shows a top view of the end face 2 of the monolithic component 50.
  • three cut membrane tubes 1 are shown in FIG , for example in order to couple the monolithic component 50 to a further connection piece (not shown).
  • FIG. 2a shows the detail "B" from FIG. 2, the membrane inlets 3 of the end face 2 being shown more clearly.
  • the shell side 10 is located between each membrane tube 1 and the next membrane tube 1.
  • the membrane inlets 3 are rounded in order to improve the mechanical load-bearing capacity as well as the flow profile at this point.
  • a monolithic component 50 is shown with an inlet 7 and an outlet 7a on the respective end face 2, 2a of the monolithic component 50.
  • the membrane tubes 1 extend from the end face 2 to the end face 2a and connect the two end faces 2 , 2a integral with each other.
  • the monolithic component also has an outer side 5 in the form of a housing 5, which also closes the shell side 10 off from the environment, in particular in a fluid-tight manner, apart from the connections provided for the shell fluid inlet and shell fluid outlet 8, 8a.
  • FIG. 3b represents a plan view of the filter 50 shown with FIG. 3, the line AA illustrating the sectional plane in which FIG. 3 is represented as a sectional view.
  • a sheath fluid collection port 56 is arranged on one side of the monolithic component 50 as an inlet or outlet for the sheath fluid.
  • the sheath fluid collection connection 56 can be designed as a flange, so that a connection line for the sheath fluid can be connected there, for example by means of a screw connection.
  • a carrier fluid collection connection 52 which can also be designed as a flange for the screw-type or clamped connection of a connection line for the carrier fluid, is arranged on one longitudinal side, specifically on the inlet 7 in particular.
  • FIG. 3a shows the detail "B" of FIG.
  • the inlet 7 forms a carrier fluid chamber 54 in which the carrier fluid is supplied to the individual membrane tubes 1 communicating with the carrier fluid chamber 54 or is discharged from the membrane tubes 1 .
  • the inlet 7 is formed in one piece with the end face 2 and in one piece with the housing 5 and the membrane tubes 1 .
  • the membrane tubes 1 are formed in that the side walls 9 of the membrane tubes emerge in one piece from the end face 2 and are lengthened to form a tubular structure.
  • the carrier fluid can flow inside the membrane tube 1, ie on the inside of the side surface 9 of the membrane tube, in order to get from one end face 2 to the opposite end face 2a.
  • the carrier fluid typically flows from the front side 2 to the front side 2a (or in the opposite direction), with direct fluid-dynamic communication between the carrier side and the shell side not occurring or being prevented as far as possible.
  • the side surface 9 of the membrane tube provides a porous surface in order to ensure a mass transfer between the enveloping fluid on the enveloping side 10 and the carrier fluid in the membrane tube 1 .
  • the side walls 9 of the membrane tubes 1 therefore form the porous structure 60, which is designed to be permeable, semi-permeable or selectively permeable.
  • the transitions 6, 6a between the housing 5 and the membrane end plates 2, 2a are also rounded.
  • End plates 2, 2a and housing 5 are in particular made of the same, but at least compatible material, in order to ensure the monolithic construction of component 50.
  • the fluid to be separated or the carrier fluid reaches the housing 5 via the inlet 7 , more precisely the membrane tubes 1 there. It enters the respective membrane tube 1 via the membrane inlet 3, flows through the membrane tubes 1 from their first side to their second side and at the other end of the housing the fluid exits again at the opposite end face 2a.
  • the filtrate penetrates through the walls 9 of the membrane tubes 1, i. H. through the porous structure 60, possibly collects in the filtrate chamber 10 and can leave the housing via one of the filtrate connections 8.
  • a membrane tube bundle 1a according to FIG. 1 can also be designed as a porous structure 60 as an insert for a separate housing 62, as is shown, for example, with FIGS. 4 to 5 is further specified.
  • a groove 11 for a possible seal can be provided on the end faces 2, 2a.
  • the membrane tube bundle 1a from the plurality of membrane tubes 1 is in any case formed in one piece with the end plates 2, 2a, so that the separation of the carrier fluid from the enveloping fluid is completely ensured by the monolithic component 50 and here the particularly vulnerable casting compound is already dispensed with can be. This already represents a significant further development compared to the well-known dialysis filters.
  • FIG. 4a shows detail “B” from FIG. 4, the structure with the groove 11 in the connecting collar 58 being further illustrated.
  • the connection collar 58 is shown rounded with the fillets 4, 4a, as shown in detail with reference to FIG.
  • FIG. 4b shows the top view of the second end face 2a, with the line AA clarifying the sectional plane for FIG.
  • FIG. 5 a further embodiment of the monolithic component 50 is shown, which has the two end faces 2, 2a formed in one piece with the porous structure 60.
  • FIG. An inlet piece 13 and an outlet piece 13a are flanged on by means of a clamping ring 15.
  • the housing 62 is designed as a separate component which is slipped over the porous structure 60 in a tubular manner.
  • FIG. 5b shows a top view of the end face 2a, with the section line A-A clarifying the section plane of FIG.
  • the carrier fluid collection connection 52 is arranged concentrically in order to enable a supply line to the porous structure 60 and thus to the filter element, consisting of the membrane tubes 1 .
  • FIG. 5a shows the detail "B" from FIG. 5, with an exemplary structure for connecting the monolithic component to the inlet piece 13 being shown.
  • the separate housing 62 is placed sealingly against the flat sealing element 14 via the sealing element 12 and is clamped to the inlet piece 13 by means of the clamping ring 15 .
  • An overhang 16 of the inlet piece 13 improves the axial fixation of the membrane tube bundle 1 in the separate housing 62.
  • the clamping ring 15 can be subjected to a corresponding contact pressure in order to produce a sealing connection between the separate housing 62 and the inlet piece 13.
  • an identical connection is also realized on the second end face 2a.
  • an end face 2, 2a could also be designed integrally with an inlet 7 and one side as separate components, which is advantageous proves when the housing is designed as a monolithic housing 5 with at least one end face 2, 2a and the porous structure 60.
  • FIG. 6 another embodiment is shown in perspective, wherein the monolithic component 50 is characterized as having support structures 17 to provide mechanical reinforcement of the monolithic component 50 .
  • the connection between the individual membrane tubes 1 and thus the sensitivity to impacts with the risk of membrane rupture can be significantly improved.
  • FIG. 6a shows the detail labeled “A” in this regard, with webs 17 being shown, which represent a suitable connection in order to bring about the above-mentioned improvement in mechanical stability.
  • Such webs 17 or a support structure 17 can also be continued up to the housing 5, see for example Figure 7a.
  • FIG. 7 shows a further illustration of a monolithic component 50 with a support structure 17 in a side view, the housing 5 being omitted for reasons of better visibility.
  • FIG. 7a shows the sectional plane B-B of FIG. 7, although the housing 5 can be shown here.
  • the support structure 17 extends between the individual membrane tubes 1, with 19 membrane tubes 1 being shown in this embodiment, which together form the porous structure 60 or the filter element.
  • the support structure 17 is also connected to the repositioning 5 with housing webs 17a in order to further improve the mechanical stability, in particular of the prosize structure 60.
  • FIG. 7b shows a further detail of an embodiment of the monolithic component 50 with support structure 17 in a sectional view.
  • the 17 membrane tubes 1 also shown in this representation, which together form the membrane filter 60a, are each connected to one another with the adjacent membrane tube 1 by means of the support structure 17 .
  • the porous structure comprises curved membrane tubes 1.
  • the membrane tubes are helically shaped, specifically divided into triple helixes 1b.
  • Helically shaped membrane tubes 1 offer the advantage of better mass transfer on the inside when carrier fluid flows through them.
  • the advantage over straight membrane tubes 1 is that helically shaped membrane tubes 1 have elastic resilience under loads in the direction of the main axis of the membrane tube bundle or the triple helix 1b. Such a load can occur during operation when the temperature of the fluid flowing through changes rapidly.
  • the membrane tube bundle 1a wants to expand according to the temperature, for example, but is prevented from doing so by the still cold housing 5 (cf., for example, FIG. 3). The same applies to rapid temperature drops.
  • the triple helix 1b or, in general, the helical shape acts like a helical spring.
  • the shape of the membrane tubes shown thus provides a stress-tolerant design that tolerates longitudinal stresses that build up, in that these are stored like a spring in the triple helix 1b and relieved again after the monolithic component 50 has cooled. It is therefore a stress-tolerant monolithic component 50, in particular longitudinal stress-tolerant, which can absorb higher stresses, in particular longitudinal stresses caused by temperature differences, before fatigue or even fracture of one or more membrane tubes 1 occurs.
  • the helical structure 1b can also be provided to be tolerant of transverse stresses, with the membrane tubes 1 having a higher capacity to absorb transverse stresses before fatigue or fracture occurs. This increases the service life and service life of the monolithic components 50 and further simplifies handling.
  • the membrane filter 60 is made up of seven triple helixes 1 b and thus of 21 membrane tubes 1 .
  • the membrane tubes open out in one piece on their first side into the first end face 2 and on their second side into the second end face 2a. They have the curves 4, 4a already described to improve the mechanical stability and the flow guidance for the carrier fluid.
  • the membrane tubes 1 are designed in such a way that they have an impermeable structure 64 at their front ends and the porous structure 60 only in the central part, which is prepared for the exchange of substances with the enveloping fluid.
  • FIGS. 9a, 9b and 9c A further embodiment of a membrane tube 28a is shown in FIGS. 9a, 9b and 9c, which is shaped like a meander or a wavy line.
  • the monolithic component 50 in this embodiment is shaped to improve various requirements.
  • the wavy membrane tube 28a can, if necessary, bring about a thorough mixing of the carrier fluids flowing inside the tube 28a, so that overall the mass transfer towards the enveloping flow is also improved.
  • a directionally variable direction of flow is generated Eddy formation can cause in the carrier fluid.
  • the meandering or wavy membrane tube 28a can be provided such that the curves of the membrane tube 28a alternate with the curves of an adjacently arranged membrane tube 28a, so that overall no increased space requirement arises despite the wavy design of the membrane tube 28a.
  • wavy membrane tubes 28a have the same advantages as the helical membrane tube bundle 1b described above, namely mechanically a damping effect or elastic flexibility in the direction of the main axis of extension of the membrane tube 28a.
  • this embodiment is also a suitable stress-tolerant design of the monolithic component 50.
  • the wavy Membrane tube 28a is shown in Fig. 9a in a perspective three-dimensional view, in Fig. 9b in a perspective side view and with Fig. 9c in a side sectional view through the corrugated membrane tube 28a.
  • FIG. 10 shows a sectional view through a membrane tube 1 with variable cross-sectional geometry.
  • the membrane tube cross section is varied in the flow direction. Due to the variable cross sections in the flow direction, the flow speeds and flow directions also change with the cross sections, which leads to better mixing of the flowing carrier fluid.
  • FIG. 10a shows a plan view of a correspondingly shaped membrane tube 1 with a variable cross section, with section line BB showing the widest cross-sectional geometry also shown in FIG. 10d, section line C-C showing the narrowest cross-sectional geometry also shown in FIG. 10c.
  • FIG. 10b shows a top view of an inlet opening 3 of the membrane tube 1, the plane AA showing the sectional plane of FIG.
  • FIG. 10e shows a perspective view of the membrane tube 1 with variable cross-sectional geometry.
  • the narrower cross section 20 alternates with the wide cross section 21 in an alternating manner.
  • Impermeable material structures 64 are shown at the two ends, and the membrane tube 1 is designed as a porous structure 60 in the middle region.
  • Fig. 11a shows a perspective view of another embodiment of a membrane tube with variable cross-sectional geometry 19.
  • the narrowest cross-section 20 alternates with the wide cross-section 21, the ends are designed as an impermeable structure 64, and the porous structure 60 is in the central region for a material exchange or mass exchange of the carrier fluid formed with the sheath fluid.
  • the membrane tube segment has a variable elliptical cross-section, the long axis of the elliptical cross-sections being alternately aligned in the starting position according to the section BB shown in FIG. 11d and rotated by 90° thereto, as shown in FIG. 11e.
  • a longitudinal section along the section line AA marked in FIG. 11c is reproduced in FIG.
  • turbulators 29 it has been shown that an even stronger mixing of the carrier fluid flowing through can also be achieved by suitable turbulators 29 .
  • Internals, such as static mixers as turbulators 29, are known as such in process engineering in order to improve the thorough mixing of a flowing fluid.
  • Static mixers cannot be fixed well in conventional membrane tubes or can they be fixed at all with third materials and therefore regularly perform movements relative to the membrane surface during operation. The membrane surface is permanently damaged by the resulting friction and it can no longer fulfill its separation task.
  • FIG. 12b shows the embodiment of FIG. 12a in a perspective representation.
  • Fig. 12c shows a membrane tube 28 with a plurality of turbulators 29 arranged one behind the other or one after the other, which are each arranged at an angle to one another, for example offset by 90° to one another, and thus a far greater mixing of the Carrier fluids and thus ensure a better mass transfer with the sheath fluid.
  • FIG. 12d shows a top view of an inlet 3 of the porous structure 60 in the form of the membrane tube 28, the line AA illustrating the sectional plane of FIG. 12c.
  • Fig. 12e shows a perspective view of the membrane tube 28.
  • the aforementioned or other turbulators 29 can also be used monolithically in the other embodiments, for example in the helical membrane tube bundles 1a, 1b, or in the wavy or meandering membrane tubes 28a Intensifying the mixing of the carrier fluid flowing through the membrane tube 1, 28, 28a.
  • the membrane tubes 1 having an additional layer 30 on the side surfaces 9, which is either applied monolithically and thus consists of a compatible or identical material to the porous structure 60, or which is applied as a coating 30 after the production of the porous structure.
  • This can involve one or more layers 30 on the inside 9, which have a different porosity and/or pore size distribution.
  • FIG. 13a This is shown enlarged in FIG. 13a, with the coating 30 being applied to the inner surfaces 9 of the membrane tubes 1.
  • FIG. 13a The coating 30 is also extended to the surface of the end plate 2 in order to further improve the transition from the membrane tube 1 via the inlet 3 to the end plate 2.
  • the coating can be produced as a separate track in the layered structure of the filter body during the additive manufacturing process.
  • traces for producing the coating 30 can be laid by a separate print head, which deposits, for example, an inorganic mass, for example an unfilled or ceramically or metallically filled polymeric mass, which leads to a finer pore structure than in the base body.
  • a separate print head which deposits, for example, an inorganic mass, for example an unfilled or ceramically or metallically filled polymeric mass, which leads to a finer pore structure than in the base body.
  • One or more coatings can also be applied subsequently after the base body has been fired and, for example, sintered at a lower temperature, particularly if inorganically filled polymeric masses are used.
  • a ceramic coating can be applied to a metallic base body.
  • FIG. 13b shows a top view of the end face 2, with the line A-A representing the sectional plane of FIG.
  • FIG. 14 an exemplary heap 31 of porous structure 60 achievable with the method of the present invention is illustrated.
  • the heap 31 has a plurality of pores 32 on.
  • the resulting pore structure, as shown in FIG. 14, can be produced, for example, with additive manufacturing using the principle of thermal phase separation.
  • At least one polymer is dissolved at an elevated temperature in a solvent which is poorly soluble at room temperature.
  • the composition of the solution is chosen - if necessary by adding further additives - so that a phase separation takes place during cooling and the polymer solution separates into a polymer-rich phase (membrane matrix) and a polymer-poor phase (pores).
  • the membrane is shaped by continuous extrusion through an annular die in the case of tubular membranes or through a slit die for flat membranes. The dimensions of the membrane that can be achieved depend on the geometry of the nozzle and can only be varied within narrow limits.
  • the membranes are then freed from the auxiliary materials by extraction, then dried and, in further steps, connected to various components to form a filter.
  • the aforementioned solution is formed into a membrane using an extrusion printer.
  • the TiPS solution or the starting material is fed to the printer nozzle above the demixing temperature and deposited in the form of thin filaments in a desired shape, such as a tubular membrane 1 .
  • Phase separation occurs as the TiPS solution cools.
  • the phase separation can be additionally influenced (N-TiPs) by providing a non-solvent, such as in particular water vapor or glycerol.
  • Sandwich structures with different pore structures can also be built up by depositing TiPS solutions with different compositions.
  • a polymer melt can be extruded at the same pressure, which forms a non-permeable layer when it cools down.
  • This polymer can be printed into impermeable housing parts of the filter, such as a filtrate collection tube or filtrate discharge tube, an aeration unit or even filter heads with connections.
  • nozzles with a mixing function for two or more components can also be used. This results in the possibility of changing the composition during the printing process and thus producing areas of different porosity up to impermeable areas with just one head. This is therefore a mixing head.
  • a pore structure resulting from such a method is shown in FIG. 14, the pore structure being essentially determined by the composition of the polymer solution of the starting material 70, 72, 74.
  • a solid matrix 31 made of polymer material with inorganic particles such as ceramic particles or metal particles optionally enclosed therein is produced by a phase inversion.
  • cavities 32 are formed, which are typically connected to one another. The size and number of cavities depends on the composition of the polymer solution (polymer content, possibly with ceramic content and/or metal content, solvent content and/or additives) and the precipitation conditions or the ambient conditions (temperature, medium, etc.).
  • the resulting microporous structure 60 is fundamentally suitable as a filter medium for micro- and ultrafiltration. Defined particles cannot be recognized in the solid matrix.
  • the solvent can be removed from the finished filter in a separate step or even when the filter is put into operation and, depending on the composition of the solvent, protect the filter during transport and installation. This also reduces clogging of the filter with foreign matter, such as dust.
  • the resulting pore structure of the porous material 60 does not have to be specified as a predetermined pattern in a control program and the production head therefore does not have to produce the concrete pore structure at the micrometer level.
  • the pore structure of the porous material 60 can be produced by the composition of the recipe used, for example in the extraction process, optionally with subsequent steps for solidifying the starting material 70, 72, 74, such as the sintering of inorganic green bodies, such as metallic or ceramic green bodies.
  • the resulting microporous structure possibly with a high proportion of inorganics, eg in the form of ceramic particles and/or metal particles, represents the green body for the subsequent firing process, particularly as part of a manufacturing process based on or analogous to the TiPS process.
  • the microporous structure 60 changes only slightly as a result of the firing process and is fundamentally suitable as a filter medium for micro- and ultrafiltration. Defined particles cannot be recognized in the solid matrix or inorganic particles of the heap 31, 31a, 31b that may be recognizable are smaller than the pores that have formed. Sintering or baking of the green bodies can be carried out, for example, at 1600° C. or more. A degree of filling of the inorganic particles in the heap 31, 31a, 31b in the polymeric phase can be between 50 and 70%. With such mixing ratios, it is advantageous to use dynamic mixers.
  • the resulting microporous structure 60 can be used without inorganic fillers without further firing. It is advantageous here to remove the washable components to complete the filter.
  • the porous or porous starting material 70, 72, 74 is provided.
  • Starting material 70, 72, 74 can be provided, for example, but not exclusively, as a liquid starting material 72 or as a pasty starting material 74.
  • the starting material 70, 72, 74 is set, adjusted or prepared to be intrinsically porous.
  • the starting material 70, 72, 74 can be provided in various ways. For example, providing 100 the starting material 70, 72, 74 includes storing 102 an extruder device with starting material 70, 72, 74.
  • the providing step 100 can also include mixing 106 the starting material 70, 72, 74 or heating 108 the starting material 70, 72, 74 include.
  • the provision 100 thus includes the possible preparation of the starting material 70, 72, 74, for example at a specific point, in particular a point of a point matrix of the monolithic component 50 to be produced, for a subsequent application of material.
  • providing 100 can also include moving to the point to be approached by means of the application device if the application device has to be moved and/or adjusted accordingly for this purpose.
  • the step of providing 100 can also include the preparation of a radiation source for later activation or heating of the point to be approached.
  • the porosity of the porous or porous starting material 70, 72, 74 is adjusted 110 for the material application to be carried out.
  • the setting can also be done in different ways.
  • the admixture 112 of additive or filler to the starting material 70, 72, 74 for adjusting the porosity can be included at the moment the material is applied.
  • the adjustment of curing parameters 114 can be included in order to adjust the porosity of the porous or porous starting material 70 , 72 , 74 in step 110 .
  • the setting step 110 can also include the selection 116 of a starting material 70 , 72 , 74 to be used from a plurality of at least two starting materials 70 , 72 , 74 . The selection can also lead to a mixture if the starting material 70, 72, 74 comprises two starting materials 70, 72, 74, which can be fed in simultaneously or alternately in order to produce a material mix at the point of the point target matrix to be approached .
  • the aim of setting step 110 is that the porous or porous starting material 70, 72, 74 is designed or prepared when the material is applied in such a way that it can form a coherent porous material structure in the component, which is preferably at the respective point of the point-target matrix to be approached with regard to the porosity can be variably adjusted in order to construct a porous material structure 60 on the one hand, but also impermeable regions 64 formed monolithically therewith. Ideally, this can be carried out in a common process sequence such that the monolithic component 50 is produced in one piece continuously, preferably without interruption. Depending on the procedure used, this can also be done step by step and with appropriate breaks between the steps if this should be necessary for the procedure.
  • the monolithic component 50 that is produced is characterized in that there is a material connection between all of the components of the monolithic component 50 in such a way that the component appears to have grown from one piece, so that the areas that are prepared for a flow passage are already in place during construction or construction the fabrication of the monolithic component 50 so that these areas allow fluid flow; on the other hand, that the impermeable areas, which are intended to prevent a flow of flow, and the housing, are already set to be correspondingly impermeable during the production of the monolithic component.
  • the entire monolithic component 50 consists of mutually compatible material or of the same starting material 70, 72, 74, to which various filling materials or additives may be added.
  • the set starting material 70, 72, 74 is applied to the point to be approached in step 120.
  • the application can have different characteristics. Depending on the monolithic component 50 to be produced, this can be understood to mean the dispensing of set starting material 70, 72, 74 by means of an application machine according to step 122. Such an application machine is, for example, an extruder. It can also be a include additional depositing of powdered starting material 71 according to step 124 at the point to be approached if this cannot be carried out completely with step 104.
  • the application 126 for example the manual application of a paste, can also be included in the application 120 step.
  • the application 120 results in the starting material 70, 72, 74 being applied to the monolithic component 50 in a form that creates areas with an impermeable material structure on the one hand and areas with a porous material structure on the other hand, with the areas with a porous material structure also being able to be further subdivided into Areas with different porosity.
  • step 130 the application 120, the setting 110 and any sub-steps thereof are continued until the monolithic component 50 is finally completed.
  • steps 110, 120 are carried out repetitively, i.e., for example, again for each point of the point-target matrix, or again for each layer of the layer-target matrix, or the starting material 70, 72 , 74 are initially set in step 110, for example for contiguous areas of the monolithic component, and then approached or applied throughout step 120.
  • FIGS. 16 to 22 show, by way of example, how some of the method steps described above can be carried out.
  • FIG. 16 shows an example of the mixing 112 of starting material 70 with additive 75 and/or filler 76 in a mixing device 82.
  • Starting material 70 is supplied to the mixing container 82c in a feed quantity which can be adjusted by means of the quantity regulator 82a;
  • Additive 75 and/or filler 76 is also supplied to the mixing container 82c in a supply quantity that can be set separately by means of the quantity controller 82b.
  • the quantity controller 82b Depending on the process conditions, at least one of the quantity regulators 82a, 82b may also be dispensable.
  • the mixing device 82 can also have three filling containers if additive 75 or filler 76 is to be provided separately.
  • the illustration in FIG. 16 does not differ in the basic form shown if either additive 75 or filler 76 or both are to be mixed together with the starting material 70, so that these variants are summarized in one figure 16 to keep things short.
  • the quantity controller(s) 82a, 82b allows/allow the adjustment 110 of the subsequent porosity of the starting material 70 and thus of areas of the monolithic component 50 to be created.
  • the mixed starting material 70a is circulated in the mixing container 82c, for example when using liquid starting material 72.
  • the mixing container 82c has an outlet quantity regulator 82e, by means of which the quantity to be applied for the application 120 can be adjusted.
  • FIG. 16 shows a punctiform application 120 of the starting material 70a to the outlined monolithic component 50, the punctiform application 120 being achievable, for example, by opening and closing the output quantity regulator 82e.
  • FIG. 17 shows a further embodiment of a storage device or application machine 80 for applying starting material 70 to a component carrier 80b or, if the monolithic component 50 has already been partially applied to the component carrier 80b, to the partially finished monolithic component 50.
  • a feed 80a for example, a coolant or also a precipitant or a hardener can be supplied during application 110 and thus hardening parameters 114 can be set.
  • FIG. 18 Yet another alternative for setting the porous or porous starting material 70 is shown in FIG. 18 with the provision of two storage devices 80, 80'.
  • an already preset starting material 70, 72, 74 can be selected in that the material application 110 onto the component carrier 80b or the partially applied monolithic component 50 is carried out with the corresponding depositing device 80, 80'.
  • FIG. 19 shows the application 122 of starting material 70, 72, 74 by means of a depositing device 80 on a component 50 that has already been partially deposited.
  • the storage device 80 is designed to be movable horizontally, that is to say at least in two axial directions, so that each point on the component carrier 80b can be approached. Vertical movement, i.e. moving up and down, is also possible.
  • the storage device 80 can be designed to be movable in order to allow movement in all three spatial directions in total, in order to make it possible to approach each point of the point matrix with the storage device 80 .
  • a "strand-by-strand" or "bead-shaped" application 122 of starting material 70, 72, 74 is shown.
  • annular or snail-shaped application 126 of pasty starting material 74 by means of a depositing device 80 is shown.
  • Firing 132 of a green body is shown in FIG.
  • the green body is inserted into the heating device 81, for example into a combustion chamber, and heated by means of a heat source 81a.
  • a washing step 134 is shown, with auxiliary materials that may be required for the application of the starting material 70, 72, 74 or for the production of the component 50 being washed out of the component 50 so that they can be removed .
  • the component 50 is placed in a bath 85 with rinsing solution 85a and rinsed.
  • the present application describes a partial aspect of the production of monolithic components and monolithic components, namely the production and construction of monolithic components by means of the method referred to as TiPS, and monolithic components produced therefrom.
  • the present application therefore does not extend to inorganic or polymeric monolithic components, insofar as these are produced using other production processes, or production processes other than TiPS.
  • These other inorganic or polymeric monolithic components as well as alternative manufacturing processes to TiPS are hereby explicitly excluded from this description and the potential patent protection that may arise.

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  • Ceramic Engineering (AREA)
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Abstract

Est divulgué un procédé de fabrication additive pour la fabrication d'une pièce comprenant une structure de matériau au moins partiellement ou au moins localement poreuse, en particulier sous la forme d'un élément filtrant ou d'un dispositif filtrant. Le procédé comprenant les étapes suivantes de : la fourniture d'un matériau de départ qui est ou peut être rendu poreux, l'application dudit matériau qui est ou peut être rendu poreux, pour former la pièce, et pendant l'étape d'application, l'ajustement de la porosité du matériau de départ qui est ou peut être rendu poreux.
PCT/EP2021/072744 2020-08-17 2021-08-16 Filtre à membrane monolithique WO2022038095A1 (fr)

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DE102022105243A1 (de) * 2022-03-07 2023-09-07 InnoSpire Technologies GmbH Monolithisch aufgebauter Membranfilter
CN115779661B (zh) * 2022-11-14 2024-06-18 华南农业大学 一种可调孔隙率的畜禽养殖末端空气净化填料装置

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WO2016024056A1 (fr) * 2014-08-11 2016-02-18 Technologies Avancees Et Membranes Industrielles Nouvelles geometries d'elements tubulaires multicanaux de separation par flux tangentiel integrant des promoteurs de turbulences et procede de fabrication
WO2016024058A1 (fr) * 2014-08-11 2016-02-18 Technologies Avancees Et Membranes Industrielles Element de separation par flux tangentiel integrant des obstacles a la circulation et procede de fabrication
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US20170203406A1 (en) * 2016-01-19 2017-07-20 Applied Materials, Inc. Porous chemical mechanical polishing pads
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FR3024663B1 (fr) 2014-08-11 2020-05-08 Technologies Avancees Et Membranes Industrielles Nouvelles geometries d'elements tubulaires monocanaux de separation par flux tangentiel integrant des promoteurs de turbulences et procede de fabrication
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FR3006606A1 (fr) * 2013-06-11 2014-12-12 Technologies Avancees Et Membranes Ind Procede de fabrication de membranes de filtration par technique additive et membranes obtenues
WO2016024056A1 (fr) * 2014-08-11 2016-02-18 Technologies Avancees Et Membranes Industrielles Nouvelles geometries d'elements tubulaires multicanaux de separation par flux tangentiel integrant des promoteurs de turbulences et procede de fabrication
WO2016024058A1 (fr) * 2014-08-11 2016-02-18 Technologies Avancees Et Membranes Industrielles Element de separation par flux tangentiel integrant des obstacles a la circulation et procede de fabrication
WO2016193574A1 (fr) * 2015-05-29 2016-12-08 Technologies Avancees Et Membranes Industrielles Structure colonnaire monobloc de séparation d'un milieu fluide
US20170203406A1 (en) * 2016-01-19 2017-07-20 Applied Materials, Inc. Porous chemical mechanical polishing pads
WO2020109716A1 (fr) * 2018-11-27 2020-06-04 Technologies Avancees Et Membranes Industrielles Procede de fabrication par addition de matiere d'un support inorganique de filtration a partir d'une composition thermofusible et membrane obtenue

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