DE102020121547A1 - Monolithic ceramic membrane filters - Google Patents

Abstract

An additive manufacturing method for producing a ceramic component with an at least partially or at least regionally porous material structure is presented, in particular as a filter element or filter device, comprising the steps of providing a porous or porous starting material, applying the porous or porous starting material to build up the ceramic component, and the application adjusting the porosity of the porous or porous starting material.

Description

field of invention

The present invention relates to a method for producing monolithic ceramic components and monolithic ceramic components, in particular as ceramic membrane filters.

Background and general description of the invention

Ceramic membrane filters for filtering or separating substances from mostly liquid mixtures are known as such. Such a mixture can be a disperse medium or, for example, a solution in which further components are dissolved in a base substance.

Ceramic membrane filters are used in various fields 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 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.

Since each different area of application has different requirements, especially in terms of the material, design or size of the filter, and process requirements such as temperature, pressure, volume and aggressiveness of the media in contact, or special hygiene requirements have to be taken into account, the membrane filter market is currently still in its infancy Development. A universal approach that is able to cover at least a number of different areas of application has not yet been achieved.

In addition, it is not uncommon for filtration systems to fail due to the only limited mechanical and/or chemical stability of known modules. Even cleaning processes at elevated temperatures, high and/or low pH values or with oxidizing cleaning agents can significantly limit the service life of the modules. Ceramic filters can react sensitively to temperature shocks or mechanical influences.

Due to the partly automated manufacturing processes, ceramic membrane filters are nowadays manufactured as standardized products with a given geometry, with 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, being practically impossible or not planned , since the resulting lower unit numbers would drive the unit costs into unsaleable regions.

It is the basis of knowledge of the present invention that the described limitations of ceramic filters that are currently available and are described in the literature result very significantly from their structure, because they are assembled from ready-made components.

In the context of the present invention, looking back at these known filters, it was recognized that there is a problem when 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,...). So far, 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 sealing to avoid cross-flows between the envelope side and the lumen side is expensive and limits the possible areas of use for membrane filters to a decisive extent.

An example of known welded tubular membranes is given in European Offenlegungsschrift EP 88 108 462 A described. It is typical that various joining methods, such as in particular welding or the filling in of potting compound, are necessary in order to achieve a seal and/or targeted liquid routing in the filter module. With such a "modular structure" it is basically interesting that different materials can be used precisely and therefore possibly more cost-effectively and can therefore be selected in a targeted manner according to the requirements.

However, it was recognized within the scope of the present invention that it can be disadvantageous that the different components, for example wise behave differently under stress, such as temperature changes, pressure changes or even swelling of the material, and as a result deteriorate the performance of the filter or fail.

Typically, the membranes are bonded or welded to the other components to form a filter element.

Mechanical seals that are clamped between the membranes and the housing are also quite common with ceramic membranes.

Connectors (filter element to piping system) 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.

For capillary modules z. For example, there are always capillary breaks in the embedding, detachment of adhesive (potting) from the housing wall or even encapsulation. In the case of flat membranes glued over the entire surface, e.g. For example, in submerged modules, delamination between the laminate layers is observed. In the case of ceramic tubular membranes or multi-channel elements, the elastomer seal used often represents the limiting weak point of the entire filter unit. Both the ceramic of the constructed membrane and the typically used stainless steel of the housing can show a significantly higher temperature and/or chemical resistance than the material used sealing material.

Another disadvantage of known multi-part filter modules is that the joining processes used have repeatedly proven to be error-prone. It is typical that various joining methods, such as in particular welding or the filling in of casting compound, are necessary in order to achieve a seal and/or liquid flow in a filter module.

Capillary membranes, including ceramic ones, are usually glued into housings. 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.

Other disadvantages of known filters arise from the limited design options. When casting capillary or tubular membranes, the transitions in or between the components, such as between the membrane and an end plate connected to it, cannot be freely selected. Rather, they are determined by the flow and wetting behavior of the potting compound used. Advantageous configurations that would improve the mechanical stability and/or could improve the flow guidance of the fluid cannot be produced in a targeted manner. This leads to mechanical fractures at this transition point and unfavorable flows, which lead to pressure peaks and wear. Typically, the membranes with the casting compound are also cut off flush with the end of the housing on the inflow side. The cut edges of the membranes are sharp and depending on the membrane and the application, these cut edges must be sealed. This significantly affects the flow of the incoming fluid.

In ceramic membrane filters, the currently common design leads to a lack of robustness against mechanical influences, such as shocks when falling or improper handling. The membranes are usually only anchored at their ends in the housing and/or in a casting compound. The brittleness of the material therefore regularly leads to membrane ruptures between the end plates, which can occur as a result of the action of mechanical loads, such as shock loads or shear loads. A very similar situation also arises with rapid temperature changes. For example, if a hot fluid suddenly flows through the membranes, they expand. The housing, which is still cold, may not allow this expansion under certain circumstances and considerable stresses build up in the membranes, which also regularly lead to membrane rupture.

Against the general background of the invention described above and the recognition process also described there in the context of the disclosure of the present application and the disadvantages found there, the present invention has therefore set itself the task of solving the aforementioned problems or at least introducing improvements thereto. Specifically, the invention has set itself the task of providing ceramic 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 failure rates of entire filter modules are reduced both in production and in operation.

The present invention thus also fulfills the further partial aspect of increasing the service life of ceramic filter modules or components in tough technical use and thus improving economic efficiency.

The present invention also fulfills the partial aspect of providing ceramic filter modules or components that achieve further improved mixing of the fluids used and/or further increase the filtrate throughput. In this way, on the one hand, the yield can be increased and/or the throughput quantity can be increased.

In addition to the aforementioned and numerous other aspects that the present invention solves, the present invention also provides a ceramic filter that can be adapted with simple means and that can be optimized in the manufacturing process for the specific subsequent application with regard to, for example, the parameters of filtration performance, flow rate, and volume - Or mass flow of fluid and/or the mechanical resilience or resistance to mechanical influences.

Alternatively or cumulatively, the invention has also set itself the task of simplifying the manufacturing process of ceramic filter modules and/or making it available more cost-effectively, or even individually adaptable to the specific requirement.

The object is solved by the subject matter of the independent claims. Advantageous developments of the invention are the subject matter of the dependent claims.

The present description is limited to ceramic components and their production in contrast to polymeric components, which can also be produced additively, but cannot be the subject of the present application or the claims arising therefrom. Furthermore, the present description does not include such components which are manufactured using a method known as TiPS. These aspects are pursued in further applications by the same applicant in order to be able to obtain additional and parallel protection and are therefore not the subject of the present application.

In addition to numerous other aspects, the improvements and new designs proposed in this description concentrate on providing a ceramic component which is suitable for separating components from a fluid. Such 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. However, the invention is not limited to this.

In an underlying idea and in a further aspect of the invention, the present invention focuses on providing monolithic ceramic components for the production of ceramic filter modules. Such monolithic components, such as in particular ceramic membrane filters, can be formed additively in the light of the present invention and/or have an intrinsic porosity. For example, in the case of a monolithic component, all components can be provided from a uniform starting material.

Also, monolithic components are typically manufactured in one piece and without interruption. Due to the lack of joined component-to-component transitions - or their limitation to a few transitions that are technically possible or reasonable in terms of manufacturing costs - they can be characterized by extreme robustness in the application and can also be used in terms of flow technology as well as in their Size and thus the filtration capacity can be optimized for their intended use.

There are various already known methods of additive manufacturing, which offer great freedom of design. Typically, the elements to be manufactured are built up in layers. However, the methods of additive manufacturing known hitherto are inadequate in various respects, particularly for use in the construction of ceramic membrane modules, and are only ready for use with the present invention.

Additive manufacturing also allows, for example, the production of geometries that are not possible with previously known processes for membrane or membrane module production.

The use of 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 μm, 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 file due to the required high resolution ter, which is unacceptably long for series production. From a technological point of view, 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, such as a 3D printer, particularly preferably no longer represents an obstacle with regard to the achievable pore size. In a particularly advantageous embodiment, 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 ceramic 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. In the step of providing a porous or porous starting material, the ceramic starting material is provided for the application. In one example, 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 initially not 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 in the temporal connection with the application of the starting material.

In other words, the provision of the porous or porous starting material means the transfer of a primary material to the component being produced. Thus, 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. In the example of the extruder, 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. During application, the method also includes adjusting the porosity of the porous or porous starting material. In other words, in connection with the material application of the starting material to or on the component, 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.

For example, 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 using the same starting material but different physical parameters or different composition or different additives. The various component areas, such as the housing and porous material structure in the example above, are monolithic, i. H. integral with each other, built. It is therefore characteristic that there are no conventional component-to-component transitions, but rather areas of the ceramic 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 are glued. The process is continued until the ceramic component is produced as a whole. In particular, the method is continued without interruption or without a break, so that the additive manufacturing method is carried out in one piece. In this way, for example, an advantageous application temperature can be kept constant or maintained in a material application zone, so that there is a continuous application of material for the production of the component.

In an advantageous embodiment, the additive manufacturing method for producing a component can comprise the application of the porous or porous starting material, pointwise, line-like or layered application of the porous or porous starting material. In other words, 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 still 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.

In this case, it is not necessary and typically also not provided for material to be applied at every point of the point-target matrix. Thus, in the point-target matrix, points are provided which are not approached and those points which are approached and starting material is applied there. The material is typically applied from the bottom up, following gravity, with a bottom layer first being deposited on a component carrier, with the bottom layer being able to be applied pointwise, linearly or in layers. Even the bottom layer is not necessarily a continuous layer, but rather it can include areas with and without material application.

The application of material can also advantageously take place in a layer target matrix. In this way, a number of points to be approached can be combined in such a layer. Layers of the layer target matrix are arranged one above the other, for example, at a further, for example, equidistant distance from one another. The application of material can also be prepared in layers and an entire layer can be connected or crosslinked as a unit, for example if the starting material is in powder form, layer by layer can first be laid down and a layer can be prepared as a whole, i.e. for example heated with a radiation source and connected to one another in one piece will.

Layers as well as points can also be provided in other coordinate systems, such as cylindrical coordinates, for example if a tubular structure is to be produced as a component. In this description, the point-target matrix is understood as the best possible resolution or subdivision of the component to be produced in spatial coordinates, since this describes the smallest possible subdivision of the component to be produced. The point distance from one point to the next neighboring point does not have to be identical; Rather, it can be advantageous to vary the point spacing, to vary it within one direction depending on the application and/or to express it differently in different directions of the coordinate system. For example, an area of particularly complex geometry can be provided with a narrower grid of points, whereas simple structures can be described with fewer points. This is easy to understand, for example, in the case of pasty starting material, when the starting material is applied in a "bead-like" manner and a long straight layer is applied, where only the start and end point of the straight layer would have to be defined. However, equidistant point-target matrices can also be advantageous. In turn, 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.

Point-by-point application can include moving to a point in the point-target matrix to be approached, to which point the porous or porous starting material is to be applied. From a technical point of view, various configurations can be implemented here for approaching a point to be approached. In principle, approaching a point to be approached means that the starting material is provided in such a form and manner that it is available at the corresponding point in the point-target matrix. The approach can thus take place by means of an application tool. 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. If the starting material is in powder form, the point of the point-target matrix to be approached can also include, for example, directing a heat generator, such as in particular a laser or a radiation source, to the point of the point-target matrix to be approached be understood in order to bring the powdery starting material deposited there at least into a kind of pre-melt at the point of the point-target matrix, so that it connects to the surrounding component or the surrounding starting material, possibly as a preparation for a later sintering of the component as a whole. For example, the starting material in powder form can be a ceramic-filled polymer powder.

In general, 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.

When applying at the point to be approached, the porous or porous starting material is preferably set, specifically at the point of the point-target matrix to be approached. The porous and/or porous starting material can also be set in different ways take on 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. Setting the starting material at the point to be approached in the point-target matrix can also implement the setting of the radiation source or the source for thermal treatment of the starting material at the point to be approached. For example, the intensity of a laser to be used can be adjusted in such a way that a higher intensity produces a different porosity than a lower intensity.

What the examples mentioned have in common is that 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 . In other words, 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. Thus, 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. In other words, 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 has a closed-pore structure, 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. In this case, 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. Afterwards, i. H. after moving to the first layer of deposits, 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.

The application step can include the application of the porous or porous starting material in such a way that at least one storage layer has areas with an 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.

Furthermore, 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. In other words, 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. In other words the porous material structure has a chaotic arrangement or a chaotic structure. In this context, 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. In principle, 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. On the contrary, the aspect has the advantage that an exact modeling of each individual pore can be dispensed with and only a desired porosity is adjusted. 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. In the present case, 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 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. As described above, 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 porosity in a material structure.

The porous material structure preferably has an open porosity. The impermeable material structure, on the other hand, can have closed porosity or no porosity at all, in any case no open porosity.

The porous material structure can be characterized in that it is at least partially permeable to the fluid or at least to components of the fluid. The porous material structure can be characterized in that there is less resistance to the flow or penetration of a fluid through the porous material structure than in the impermeable material structure.

The porous material structure can have an open microporous or mesoporous structure. The average pore size can be less than 40 μm, preferably less than 5 μm and more preferably even less than 1 μm. 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. In other words, 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 adjustment can also include the adjustment of hardening parameters for the respective point of the point-target matrix to be approached.

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. In particular, can 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 for the production of the monolithic component.

Polymeric or inorganic nanoparticles can be used as an additive. An inorganic or organic filler can be used as the filler.

The pores of the porous or porous starting material can during material application, i. H. ie in particular at the specific point in time and the specific location of the point of the point target matrix to be approached, are designed or prepared in such a way that they form a coherent porous material structure in the 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. In other words, 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. Specifically, in one example, 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 ceramic component includes a first face and a second face opposite the first 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. In any case, 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.

With regard to the porous structure, the monolithic component can be prepared in such a way that it is set up for substances and/or particles with a size of less than 10 μm, preferably less than 2 μm and more preferably less than 0.5 μm, for which the porous structure permeable, semi-permeable or selectively permeable.

The monolithic ceramic component can be adapted to contain and drain the carrier fluid on the carrier side and a cladding fluid on the cladding 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. Particularly preferably, 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 - as for first face described - be integrally formed on the second face, in particular formed integrally with the second 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 can also 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. Such 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.

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 in particular arranged or constructed concentrically around the mouth and embedded in one piece in the first or second end face. In other words, the mouth merges into the first or second end face in one piece.

The monolithic ceramic 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.

Furthermore, 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.

The connection, cross-connection or stiffener may directly integrally connect the porous structure to the housing. In other words, the 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 a turbulence in the corresponding fluid, so that there is improved mixing and thus a improved mass transfer between sheath fluid and 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.

In particular, 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 applied to 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. Advantageously, 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 preferably has ceramic components. Such ceramic components can be provided in particular as a ceramic paste.

The invention also includes a monolithic ceramic component which is produced using a method as described above.

The invention also describes a monolithic ceramic 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 ceramic 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 ceramic 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.

The invention is explained in more detail below using exemplary embodiments and with reference to the figures, in which identical and similar elements are partially provided with the same reference symbols and the features of the various exemplary embodiments can be combined with one another.

character list

• 1, 1a, 1b perspektivische Ansicht auf ein monolithisches Rohrbündel als Bauteil mit Detailausschnitten,
• 2, 2a, 2b ein monolithisches Bauteil in Schnittdarstellung,
• 3, 3a, 3b ein monolithisches Bauteil mit Gehäuse,
• 4, 4a, 4b ein monolithisches Bauteil als Einsatzmodul,
• 5, 5a, 5b ein monolithisches Bauteil als Filtermodul,
• 6, 6a perspektivische Ansicht eines monolithischen Bauteils mit Stegen,
• 7, 7a, 7b monolithisches Bauteil als Kartusche mit Stegen und Detailansicht,
• 8 ein monolithisches Bauteil mit zu Triplehelixen angeordneten Membranrohren in perspektivischer Darstellung,
• 9 Segment eines in Tripelhelix angeordneten Membranrohrbündels,
• 10 bis 10e monolithisches Bauteil mit variablem Membranrohrdurchmesser,
• 11 -11e weiteres Beispiel eines monolithischen Bauteils mit variabler Rohrgeometrie
• 12a - 12e monolithisches Bauteil mit Einbauten bzw. inneren Strukturen (statische Mischer)
• 13 - 13b monolithisches Bauteil mit aufgetragener Beschichtung
• 14 Darstellung eines Haufwerks, das mit dem erfindungsgemäßen Verfahren erzielbar ist,
• 15 Beispielschema für verschiedene Verfahrensabläufe zur Herstellung eines monolithisch aufgebauten keramischen Filtermoduls,
• 16 Auftragsvorrichtung zum Auftragen von pulverförmigem Ausgangsmaterial,
• 17. Heizofen zur Vorbehandlung von festem Ausgangsmaterial,
• 18 Mischvorrichtung,
• 19 weitere Auftragsvorrichtung mit Zuführung,
• 20 Anlage mit zwei wählbaren Auftragsvorrichtungen,
• 21 weitere Auftragsvorrichtung,
• 22 noch ein Beispiel für eine Auftragsvorrichtung,
• 23 Brennkammer mit Grünkörper,
• 24 Waschbad für die Auswaschung von Produktionshilfsstoffen,
• 25 Spülvorrichtung.

Show it:

• 1 , 1a , 1b Perspective view of a monolithic tube bundle as a component with details,
• 2 , 2a , 2 B a monolithic component in section,
• 3 , 3a , 3b a monolithic component with housing,
• 4 , 4a , 4b a monolithic component as an insert module,
• 5 , 5a , 5b a monolithic component as a filter module,
• 6 , 6a perspective view of a monolithic component with webs,
• 7 , 7a , 7b monolithic component as cartridge with bars and detailed view,
• 8th a perspective view of a monolithic component with membrane tubes arranged in triple helixes,
• 9 Segment of a membrane tube bundle arranged in a triple helix,
• 10 until 10e monolithic component with variable membrane tube diameter,
• 11 - 11e another example of a monolithic component with variable tube geometry
• 12a - 12e monolithic component with internals or internal structures (static mixers)
• 13 - 13b monolithic component with applied coating
• 14 Representation of a heap that can be achieved with the method according to the invention,
• 15 Example scheme for various process sequences for the production of a monolithic ceramic filter module,
• 16 Application device for applying powdered starting material,
• 17 . heating furnace for the pretreatment of solid starting material,
• 18 mixing device,
• 19 further application device with feeder,
• 20 System with two selectable application devices,
• 21 further application device,
• 22 another example of an application device,
• 23 combustion chamber with green body,
• 24 washing bath for washing out production aids,
• 25 flushing device.

Detailed description of the invention

Referring to 1 a first embodiment of a monolithic component 50 is shown, which has a first end face 2 and a second end face 2a as well as a bundle of membrane tubes 1 . 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. In this example, 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.

1a shows a detail of the end face 2a, as in 1 shown. The diaphragm inlets 3 are rounded in a hydraulically favorable 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.

1b shows a detail of the end plate 2, the rounded transitions 4 being visible from its outside in the perspective view.

2 shows a sectional view in a longitudinal section through the monolithic ceramic component 50 along the in 2 B line marked AA.

2 B represents a plan view of the end face 2 of the monolithic ceramic component 50 2 three cut membrane tubes 1 are shown as well as the spaces between the membrane tubes of the shell side 10. The end faces 2, 2a have a connecting collar 58, for example in order to couple the monolithic component 50 to a further connecting piece (not shown).

2a shows the detail "B". 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.

Referring to 3 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 to one another in one piece. Furthermore, the monolithic component also has an outer side 5, in the form of a housing 5, which also closes off the envelope side 10 from the environment, and in particular in a fluid-tight manner, if one of the ones provided for this purpose Connections for the sheath fluid inlet or sheath fluid outlet 8, 8a apart.

3b puts an oversight on the with 3 filter 50 shown, the line AA depicting the sectional plane in which the 3 shown 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.

3a shows the detail "B" of the 3 , the structure of the inlet 7 being further illustrated. 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. Inside the membrane tube 1, ie on the inside of the side surface 9 of the membrane tube, the carrier fluid can flow through in order to get from one end face 2 to the opposite end face 2a. In other words, 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. Rather, 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. Subsequent or non-material connection by joining, welding, gluing, clamping or the like is not required in a particularly advantageous manner. 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 enters 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 and 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.

In the synopsis of 1 with the 3 it becomes clear that a membrane tube bundle 1a after 1 can also be designed as a porous structure 60 as an insert for a separate housing 62, as with, for example 4 until 5 is further specified.

As in 4 to see, a groove 11 for a possible seal can be provided on the end faces 2, 2a. In this example, 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 dispensed with can. This already represents a significant further development compared to the well-known dialysis filters.

4a shows the detail "B" from the 4 , the structure with the groove 11 in the connecting collar 58 being further illustrated. The terminal collar 58 is shown rounded with fillets 4, 4a, as with reference to FIG 1 is shown in detail.

4b this shows the plan on the second end face 2a, the line AA being the sectional plane for the 4 clarified.

Referring to 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. 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.

5b shows this a plan view of the end face 2a, with the section line AA the section plane of the 5 clarified. The carrier fluid collection port 52 is arranged concentrically to a supply line with the porous structure 60 and thus with the filter element consisting of the membrane tubes 1 to allow.

the 5a shows the detail "B" from the 5 , wherein an exemplary structure for connecting the monolithic component to the inlet piece 13 is 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 . A projection 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 create a sealing connection between the separate housing 62 and the inlet piece 13. In this example, an identical connection is also realized on the second end face 2a. Of course, one end face 2, 2a could also be designed integrally with an inlet 7 and one side as separate components .

Referring to 6 Another embodiment is shown in a perspective view, wherein the monolithic component 50 is characterized in that it has support structures 17 in order to achieve mechanical reinforcement of the monolithic component 50 . Especially in the case of brittle membrane materials such as ceramics, the connection between the individual membrane tubes 1 and thus the sensitivity to impacts with the risk of membrane rupture can be significantly improved.

6a FIG. 12 shows the detail marked “A”, wherein webs 17 are 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 7a .

7 shows a further illustration of a monolithic component 50 with support structure 17 in a side view, the housing 5 being omitted for reasons of better visibility.

7a shows the section plane BB 7 , In which case 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.

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 illustration, 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 .

Referring to 8th a further embodiment of a monolithic component is shown, wherein the porous structure has curved membrane tubes 1 . In this embodiment, 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 blocked by the still cold housing 5 (cf. e.g. 3 ) prevented from doing so. The same applies to rapid temperature drops. The triple helix 1b or generally the helical shape acts like a helical spring. In this embodiment, the membrane filter 60 is made up of seven triple helixes 1b 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.

9 shows a membrane tube bundle segment consisting of three helically shaped membrane tubes, which together form the triple helix 1b. In this embodiment, 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.

Referring to the 10 until 11 further possibilities are shown which can be implemented in a particularly simple and efficient manner with the present invention, namely the introduction of variable cross-sectional geometries of membrane tubes 1. So shows 10 a sectional view through a membrane tube 1 with variable cross-sectional geometry. The cross-section of the membrane tube is varies in the direction of flow. 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.

10a shows a top view of a correspondingly shaped membrane tube 1 with a variable cross-section, the section line BB also containing 10d shows the widest cross-sectional geometry shown, the intersection line CC also with 10c narrowest cross-sectional geometry shown.

10b shows a top view of an inlet opening 3 of the membrane tube 1, the plane AA being the sectional plane of the 10 clarified.

10e Finally, FIG. 1 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.

11a shows a perspective view of another embodiment of a membrane tube with variable cross-sectional geometry 19. Here, too, 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 in the middle area is for material exchange or Mass exchange of the carrier fluid with the enveloping fluid is formed. The membrane tube segment has a variable elliptical cross-section, with the long axis of the elliptical cross-sections alternating in the starting position according to the in 11d shown section BB and rotated by 90°, as shown in 11e , is aligned. A longitudinal section along the in 11c marked cutting line AA is in 11 played back. The changes in the direction of flow and thus, depending on the fluid, also the mixing can be more pronounced here than with the circular cross-sections.

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. In membrane tubes, however, this does not work easily, but at least not permanently. 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.

Due to the advantageous method in which the component is built up monolithically, it is now possible to form turbulators 29 in one piece with the porous structure 60, so that in any case the problem of relative movement no longer arises. The individual segments 29a of the turbulators or the static mixers are therefore an integral part of the porous structure 60, i.e. in particular the tubular membrane 1, 19, 28. The monolithic combination of turbulators 29 with a porous structure 60 as an integrated component eliminates the problem of relative movements, so that Damage to the membrane at this point is reduced or even ruled out, thus ensuring reliable long-term operation.

12b shows the embodiment of 12a in perspective view

12c shows a membrane tube 28 with a plurality of turbulators 29 arranged next to one another 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 ensure far greater mixing of the carrier fluid and thus better mass transfer with the enveloping fluid.

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 being the sectional plane of the 12c clarified.

12e finally shows a perspective representation of the membrane tube 28.

Referring to 13 Another embodiment of the monolithic component 50 is shown, 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 subsequently to the production of the porous structure as a coating 30 is applied. This can involve one or more layers 30 on the inside 9, which have a different porosity and/or pore size distribution.

In 13a this is shown enlarged, with the coating 30 being applied to the inner surfaces 9 of the membrane tubes 1 . The coating 30 is also extended to the surface of the end plate 2 to the transition from To further improve 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.

These traces for producing the coating 30 can be laid by a separate print head, which deposits a ceramic mass, for example, which leads to a finer pore structure than in the case of 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.

13b finally shows a top view of the end face 2, the line AA being the sectional plane of the 13 represents.

Referring to 14 a heap 31 of the porous structure 60 that can be achieved with the method of the present invention is shown as an example. The heap 31 has a plurality of pores 32 . The resulting pore structure, as in 14 shown, can be produced, for example, with additive manufacturing using the principle of thermal phase separation.

For the membrane filter 60a according to the invention, it typically applies that 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. Rather, 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, 71, 73, 74, such as the sintering of green ceramic bodies.

For ceramic materials, 3D extrusion can be used as a manufacturing process to produce so-called green bodies or precursors for subsequent sintering in a sintering furnace. Another advantage here is the reduced possible wall thickness compared to extruded ceramic filter elements. This results in shorter times in the sintering furnace due to the lower heat storage, which has an advantageous effect on the production costs.

Different priorities can be generated here by different recipes of the ceramic masses. The prerequisite is a multi-head system with an extrusion head for each desired porosity, with which the corresponding ceramic paste is deposited at the intended location. In other words, the porosity is adjusted in this example by the corresponding head of the system depositing a corresponding starting material 70 , 71 , 73 , 74 and this being monolithically connected to the rest of the component 50 .

Referring to the 14 a pile 31b is shown, which can be achieved with a manufacturing method, the pile having, for example, ceramic particles which form cavities 32b between the particles. To produce ceramic membranes 60a, for example, a green body (precursor) can first be produced from a ceramic paste. For example, the paste essentially consists of ceramic particles, organic binders and additives. After the paste has dried or solidified, the green body is obtained, which is formed into a microporous ceramic body 60 in a subsequent firing step, depending on the composition of the paste. The resulting pore structure is essentially determined by the ceramic particles. The ceramic particles 31b are connected to one another by the sintering process, but retain their particle shape to a certain extent. There are cavities 32b between the ceramic particles, which are advantageously connected to one another to form a common cavity. The size of the cavities depends on the size and shape of the ceramic particles. The organic components of the starting material 70, 71, 73, 74 decompose at the high firing temperatures. The resulting microporous structure is fundamentally suitable as a filter medium for micro and ultra filtration. The pore size desired in each case can be set by suitably selecting the particle size, with the particles being larger than the pores. Sintering or baking of the green bodies can be carried out at 1600° C. or more.

Referring to 15 the sequence of the method for producing a component 50 is shown in a schematic diagram representation. In the provision step 100, the porous or porous starting material 70, 71, 73, 74 is provided. Starting material 70, 71, 73, 74 can be provided, for example, but not exclusively, as a powdered starting material 71, as a solid starting material 73 or as a pasty starting material 74. The starting material 70, 71, 73, 74 is set, adjusted or prepared to be intrinsically porous. The starting material 70, 71, 73, 74 can be provided in various ways. For example, providing 100 the starting material 70, 71, 73, 74 includes storing 102 an extruder device with starting material 70, 71, 73, 74. The providing step 100 can also include placing or preparing 104 powdered starting material 71, at for example by means of a depositing device 80. The step of providing 100 can also include the mixing 106 of the starting material 70, 71, 73, 74 or the heating 108 of the starting material 70, 71, 73, 74. The provision 100 thus includes the possible preparation of the starting material 70, 71, 73, 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. Thus, 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.

After the preparation, the porosity of the porous or porous starting material 70, 71, 73, 74 is adjusted 110 for the material application to be carried out. The setting can also be done in different ways. Thus, the admixture 112 of additive or filler to the starting material 70, 71, 73, 74 can be included to adjust the porosity at the moment the material is applied. Furthermore, the setting of curing parameters 114 can be included in order to set the porosity of the porous or porous starting material 70 , 71 , 73 , 74 in step 110 .

The setting step 110 can also include the selection 116 of a starting material 70, 71, 73, 74 to be used from a plurality of at least two starting materials 70, 71, 73, 74. The selection can also lead to a mixture if the starting material 70, 71, 73, 74 comprises two starting materials 70, 71, 73, 74, which can be fed in simultaneously or alternately in order to produce a material mix at the point to be approached the point target - Create matrix.

The aim of the adjustment step 110 is that the porous or porous starting material 70, 71, 73, 74 is designed or prepared during material application in such a way that it can form a coherent porous material structure in the component, which preferably at the respective point to be approached the point target Matrix can be adjusted with respect to the porosity in order to build up 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. Finally, 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. Particularly preferably, the entire monolithic component 50 consists of mutually compatible material or of the same starting material 70, 71, 73, 74, to which different filling materials or additives may be added if necessary.

The set starting material 70, 71, 73, 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 , 71 , 73 , 74 by means of an application machine according to step 122 . Such an application machine is, for example, an extruder. It can also include an 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, 71, 73, 74 being applied to the monolithic component 50 in such a way that there are 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 subdivided further are in areas with different porosity.

Finally, in step 130, the application 120, the setting 110 and any sub-steps thereof are continued until the monolithic component 50 is finally completed. Depending on the selected underlying method, 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, 71 , 73, 74 are initially set in step 110, for example for contiguous areas of the monolithic component, and then approached or applied throughout step 120.

the 16 until 25 show by way of example how some of the methods described above steps can be taken. 16 shows the application 104 of powdered starting material 71 on a partially finished monolithic component 50 by means of a depositing device 80. The starting material 70 is deposited in step 104 in such a way that, for example, the powdered starting material 71 is deposited in a matrix plane 90 in a depositing area 92, whereas in a Area 94 no starting material 71 is deposited.

17 shows an example of the heating 108 of solid starting material 73 in a heating furnace 81 by means of heat 81a.

18 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 that can be adjusted by means of the quantity controller 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. Depending on the process conditions, at least one of the quantity regulators 82a, 82b may also be unnecessary. The mixing device 82 can also have three filling containers if additive 75 or filler 76 is to be provided separately. The representation of 18 does not differ in the shown, basic form, if either additive 75 or filler 76 or both are to be admixed together with the starting material 70, so that these variants for the sake of brevity in one 18 are summarized.

The one or more quantity regulators 82a, 82b allow/allow the setting 110 of the later 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. The mixing container 82c has an output quantity regulator 82e in the outlet, by means of which the quantity to be applied for the application 120 can be adjusted. For example shows 18 for this purpose a punctiform application 120 of the starting material 70a onto the outlined monolithic component 50, the punctiform application 120 being achievable, for example, by opening and closing the output quantity regulator 82e.

19 shows a further embodiment of a storage device or application machine 80 for the application of 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. By means of 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.

Yet another alternative to adjust the porous or porous starting material 70 is in 20 shown with the provision of two storage devices 80, 80'. According to step 116, an already preset starting material 70, 71, 73, 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'.

with 21 the application 122 of starting material 70, 71, 73, 74 by means of a depositing device 80 on a component 50 that has already been partially deposited is shown. 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. Alternatively or cumulatively, 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 . Application 122 of starting material 70 , 71 , 73 , 74 “in strands” or “bead-like” is shown.

Referring to 22 the annular or snail-shaped application 126 of pasty starting material 74 by means of a depositing device 80 is shown.

with 23 the firing 132 of a green body is shown in the case where the green body is first built up from starting material 70 , 71 , 73 , 74 and is completed as a whole in the firing step 132 . In this case, the green body is inserted into the heating device 81, ie, for example, into a combustion chamber, and heated by means of a heat source 81a.

Referring to 24 a washing-out step 134 is shown, with any auxiliary materials required for the application of the starting material 70, 71, 73, 74 or for the production of the component 50 being washed out of the component 50 so that they can be removed. For this purpose, the component 50 is placed in a bath 85 with rinsing solution 85a and rinsed.

25 Finally, FIG. 13 shows the removal of any excess powder that may occur in step 136 in a rinsing chamber 86, for example by means of compressed air.

The present application describes a partial aspect of the production of monolithic components and monolithic components, namely manufacture and construction of ceramic monolithic components. The present application therefore does not extend to polymeric monolithic components and their production, and also does not cover production using the TiPS method; rather, the aforementioned areas are hereby explicitly excluded.

It is obvious to the person skilled in the art that the embodiments described above are to be understood as examples and that the invention is not limited to these, but can be varied in many ways without departing from the scope of protection of the claims. Furthermore, it is evident that the features, regardless of whether they are disclosed in the description, the claims, the figures or otherwise, also individually define essential components of the invention, even if they are described together with other features. In all figures, the same reference symbols represent the same objects, so that descriptions of objects that may only be mentioned in one or at least not with regard to all figures can also be transferred to these figures, with regard to which the object is not explicitly described in the description.

Reference List

1

Carrier side, membrane tube, filter capillary

1a

membrane tube bundle

1b

triple helix

2, 2a

face, end plate

3

membrane inlet

4

Transition or fillet

4a

flow guidance

5

casing, casing

6

crossing

7

inflow, outflow

8th

Sheath fluid inlet or outlet, filtrate connection

9

side surface of the membrane tube

10

Shell side, filtrate space

11

groove

12

sealing element

13

inlet or outlet piece

14

flat sealing element

15

clamping ring

16

Got over

17

web

17a

housing bar

19

Membrane tube with variable cross-section

20

narrow cross section

21

another cross section

22

longitudinal section

23

elliptical cross-section

24

starting position

25

rotated 90°

26

longitudinal section

27

longitudinal section

28

tubular membrane

29

turbulator, static mixer

29a

turbulator edge

30

coating

31

Connected heaps of porous structure

32

pore in heaps

50

monolithic component

50a

target point

52

Carrier fluid collection port

54

carrier fluid chamber

56

Sheath Fluid Collection Port

58

connection collar

60

porous structure

60a

membrane or membrane filter

62

separate housing

64

impervious area

70

starting material

70a

mixed source material

71

Starting material, in powder form

72

starting material, liquid

73

starting material, solid

74

Starting material, pasty

75

additive

76

filler

77

Absorption Modifier, Ink

80

Storage device or application machine

80'

second storage device

80a

feeding

80b

component carrier

81

heating device

81a

Heat generation by means of the heating device 84

82

mixing device

82a

Feedstock quantity regulator

82b

Quantity regulator additive / filler

82c

mixing tank

82d

rotary mixer

82e

output volume control

83

excitation or activation arrangement

85

bath

85a

rinsing solution

86

chamber

90

matrix level

92

storage area

94

further area

100

Provide

102

Stock up

104

Place

106

Mix

108

Warm up

110

Set

112

mixing

114

Setting curing parameters

116

Selection of starting material

120

Instruct

122

Outputting or aligning the application machine

124

Depositing powdered starting material

126

(Manual) application of starting material

130

Continue or end the manufacturing process

132

Firing a green body

134

Washing out of excipients

136

Remove excess powder

QUOTES INCLUDED IN DESCRIPTION

This list of documents cited by the applicant was generated automatically and is included solely for the better information of the reader. The list is not part of the German patent or utility model application. The DPMA assumes no liability for any errors or omissions.

Patent Literature Cited

• EP88108462A [0009]

Claims (36)

Additive manufacturing method for manufacturing a ceramic component (50) with an at least partially or at least regionally porous material structure (60), in particular as a ceramic filter element (60a) or filter device, comprising the steps: Providing (100, 102, 104, 106, 108) a porous or porous ceramic starting material (70, 70a, 71, 73, 74), Applying (120, 122, 124, 126) the porous or porous ceramic starting material to build up the ceramic component, and during the application adjusting (110, 112, 114, 116, 118, 119) the porosity of the porous or porous ceramic starting material. Additive manufacturing method according to the preceding claim, wherein the step of applying (120, 122, 124, 126) the porous or porous ceramic starting material (70, 70a, 71, 73, 74) means pointwise, line-like or layered application of the porous or porous ceramic starting material includes, in particular in a point target matrix or in a layer target matrix. Additive manufacturing method according to the preceding claim, wherein the spot application comprises (120, 122, 124, 126). Approaching (120) a point of the point target matrix to be approached, at which point the porous or porous ceramic starting material (70, 70a, 71, 73, 74) is to be applied, and setting (110, 112, 114, 116, 118, 119) the porous or porous ceramic starting material at the point of the point target matrix to be targeted and applying the adjusted porous or porous ceramic starting material to the point. Additive manufacturing method according to either of the preceding claims, further comprising the steps Approaching at least one first point of the point-target matrix and setting (110, 112, 114, 116, 118, 119) the porous or porous ceramic starting material (70, 70a, 71, 73, 74) at the at least one first point such that a porous material structure (60) is formed at the at least one first point, and/or Approaching (120) at least one second point of the point-target matrix and adjusting (110, 112, 114, 116, 118, 119) the porous or porous ceramic starting material at the at least one second point in such a way that at the second point a impermeable material structure (64) is formed. Additive manufacturing method according to one of the three preceding claims, wherein the points of the point target matrix are arranged in storage layers, and wherein the approach (120) of the points of the point target matrix is carried out in layers, so that initially the points of a first storage layer are approached and then the points of a second storage layer. Additive manufacturing method according to the preceding claim, wherein the step of applying (120) comprises applying the porous or porous ceramic starting material (70, 70a, 71, 73, 74) such that at least one storage layer has areas with an impermeable material structure (64), and/or at least one storage layer has areas with a porous material structure (60), and/or at least one deposit layer has both an impermeable material structure (64) and a porous material structure (60), which is applied with the same porous or porous ceramic starting material. Additive manufacturing process according to one of the preceding claims, wherein the application (120) of the porous or porous ceramic starting material (70, 70a, 71, 73, 74) is carried out in such a way that the partially or regionally porous material structure (60) of the component (50) is arranged or built up chaotically, and/or the partially or regionally porous material structure (60) of the component (50) is created with the application (120) of the starting material in or on the component and has a non-repetitive structure or arrangement. Additive manufacturing process according to any one of the preceding claims, wherein the ceramic starting material (70, 70a, 71, 73, 74) is made or prepared to be intrinsically porous, and/or the porous material structure (60) has an open porosity, and/or the impermeable material structure (64) has a closed porosity, and/or wherein the porous material structure (60) is characterized in that it is at least partially permeable to the fluid or components of the fluid, and/or the porous material structure (60) being characterized in that there is less resistance to the flow or penetration of a fluid through the porous material structure than in the impermeable material structure (64). Additive manufacturing method according to any one of the preceding claims, wherein the porous Material structure (60) has an open microporous or mesoporous structure with an average pore size of less than 40 μm, preferably less than 5 μm, more preferably less than 1 μm. Additive manufacturing method according to any one of the preceding claims, wherein the porous material structure (60) has an average volume porosity of 20% or greater, preferably 35% or greater. Additive manufacturing method according to any one of the preceding claims, wherein the impermeable material structure (64) has a higher density than the porous material structure (60), wherein the ratio of the density in the impermeable material structure to the porous material structure is in particular 1.2: 1, further preferably at 1.5:1, even more preferably at 2:1. Additive manufacturing method according to one of the preceding claims, wherein the step of adjusting (110) the porosity of the porous or porous ceramic starting material (70, 71, 73, 74) comprises: Admixture (112) of additive (75) or filler (76) to the ceramic starting material to adjust the porosity at the moment the material is applied, in particular at the point (50a) of the point target matrix to be approached, and/or Selection (116) of a ceramic starting material to be used from a plurality of at least two ceramic starting materials, wherein the at least two ceramic starting materials can be supplied alternately or simultaneously, in particular at the point (50a) of the point target matrix to be approached in each case, for the production of the ceramic monolithic component (50). Additive manufacturing method according to one of the preceding claims, wherein the pores (31, 31A, 31B) of the porous or porous starting material (70, 71, 73, 74) are designed or prepared during material application such that these form a cohesive porous material structure (60) in the component (50) and/or the pores have a rounded or potato-shaped single structure. Additive manufacturing method according to one of the preceding claims, wherein the porous material structure (60) of the ceramic component (50) is constructed and arranged in such a way that it is suitable for separating a shell side from a carrier side in a permeable manner. Monolithic ceramic component (50), in particular as or for a device for separating components from a fluid, in particular produced according to one of the above methods, the monolithic ceramic component comprising: - a first and a second end face (2, 2a) opposite the first, - a porous structure (60) arranged between the first and the second end face and constructed and connected in one piece to the end faces, the porous structure being permeable at least partially or in certain areas, - wherein the porous structure is prepared and arranged in such a way that an envelope side is at least partially and/or at least regionally permeable to separate from a carrier side, - wherein a carrier fluid can be provided on the carrier side, - wherein the porous structure is prepared to ensure mass transfer of the carrier fluid with the shell side, in particular a transfer from the carrier fluid into a shell fluid and/or from a shell fluid into the carrier fluid. Monolithic ceramic component (50) according to the preceding claim, which is designed as a membrane element (62) for a filter device or which is designed as a filter device and which is constructed monolithically with the porous structure (60) as a membrane element. Monolithic ceramic component (50) according to one of the preceding claims, further comprising a housing (5) formed monolithically with the porous structure (60) and the first and second faces (2, 2a), wherein preferably the porous structure of the housing together with first and second face is enclosed. Monolithic ceramic component (50) according to one of the preceding claims, further prepared in such a way that on the cladding side (10) a cladding fluid can be provided so that both the carrier fluid and the cladding fluid can flow in or through the monolithic ceramic component and the carrier fluid is separated from the enveloping fluid by means of the porous structure (60), and/or wherein the porous structure (60) is designed to be semipermeable or selectively permeable, and/or wherein the porous structure (60) is designed to be permeable to substances and/or particles with a size less than 10 μm, preferably less than 2 μm, more preferably less than 0.5 μm. Monolithic ceramic component (50) according to one of the preceding claims, prepared for receiving and discharging the carrier fluid on the carrier side (1) and a cladding fluid on the cladding side (10), so that the carrier fluid and the cladding fluid can flow through the monolithic ceramic component to Provision of a carrier flow tion and an enveloping flow in the monolithic component. Monolithic ceramic component (50) according to one of the preceding claims, wherein the porous structure (60) comprises filter capillaries (1), in particular membrane capillaries. Monolithic ceramic component (50) according to any one of the preceding claims, wherein the first end face (2) is plate-shaped and the porous structure (60) is formed in one piece on the first end face, in particular is formed integrally therewith, and/or wherein the second end face (2a) is plate-shaped and the porous structure (60) is integrally formed on the second end face, in particular is formed integrally therewith. Monolithic ceramic component (50) according to one of the preceding claims, wherein the porous structure (60) comprises a plurality of elongate membrane tubes or filter capillaries (1) which integrally connect the first end face (2) of the monolithic component with the second end face (2a) associate. Monolithic ceramic component (50) according to the preceding claim, wherein the membrane tubes or filter capillaries (1) have an inside, wherein the insides of the membrane tubes or filter capillaries form the support side and/or the membrane tubes or filter capillaries forming the shell side (10) on their outsides. Monolithic ceramic component (50) according to one of the two preceding claims, wherein the membrane tubes or filter capillaries (1) have a tubular or tubular configuration, and/or wherein the membrane tubes or filter capillaries (1) extend in a substantially straight tubular manner, or, wherein the membrane tubes or filter capillaries extend helically or helically, in particular as a double helix or triple helix (1b), in which two or three membrane tubes or filter capillaries run around one another. Monolithic ceramic component (50) according to one of the three preceding claims, wherein the membrane tubes or filter capillaries (1) each have a first or second opening (3) through which a fluid can flow, which is integral with the first or second end face (2, 2a) is executed. Monolithic ceramic component (50) according to the preceding claim, wherein the mouth (3) has a flow-guiding surface design (4, 4a) which is constructed in particular concentrically around the mouth and merges integrally into the first or second end face (2, 2a). . A monolithic ceramic component (50) according to any one of the preceding claims, further comprising a first carrier fluid collection port (7) formed monolithically with the first end face (2) and the porous structure (60), and/or a second carrier fluid collection port (7a) formed monolithically with the second end face (2a) and the porous structure (60), and/or a sheath fluid port (8, 8a) formed monolithically with the porous structure (60). Monolithic ceramic component (50) according to one of the preceding claims, the porous structure (60) further comprising at least one connection, cross-connection, or reinforcement (17, 17a) made monolithically with the porous structure to increase the mechanical stability of the porous structure. A monolithic ceramic component (50) according to the preceding claim, wherein the joint, cross-joint, or stiffener (17, 17a) directly integrally connects the porous structure (60) to the casing (5). Monolithic ceramic component (50) according to any one of the preceding claims, wherein the porous structure (60) has at least one turbulator (29, 29a) for mixing the carrier fluid and/or for mixing the enveloping fluid, and/or wherein the porous structure (60) provides a flow cross-section that is variable over the length for the carrier fluid and/or the sheath fluid. Monolithic ceramic component (50) according to any one of the preceding claims, wherein the porous structure (60) has a higher or lower porosity and/or pore size distribution in some areas or in part., and/or the porous structure (60) having impermeable areas (64), permeable areas and other areas having a different porosity compared to both the impermeable areas and the permeable areas. Monolithic ceramic component (50) according to one of the preceding claims, wherein the first and/or the second end face (2, 2a) has an integral fluid barrier or is designed as an integral fluid barrier, the fluid barrier (n) separates the flow of carrier fluid from the sheath flow. A monolithic ceramic component (50) according to any one of the preceding claims, wherein the monolithic ceramic component is composed of the porous or porous starting material. Monolithic ceramic component (50) according to the preceding claim, wherein the porous or porous starting material comprises ceramic components, in particular ceramic paste. A monolithic ceramic component (50) as claimed in any one of the preceding claims made by any of the methods listed above. Monolithic ceramic filter module (50) for a device for separating components from a fluid, the ceramic filter module comprising: - a first and a second end face (2, 2a) opposite the first, - a filter housing (5, 62), in particular elongate or tubular, formed in one piece with the first and second end faces, - a porous structure (60, 64) arranged in the filter housing and constructed and connected in one piece with the end faces and the filter housing, the porous structure being permeable at least partially or in certain areas, - at least one carrier fluid collection port (7, 7a), - at least one sheath fluid connection (8, 8a), - wherein the first end face and the second end face are each designed as an integral fluid barrier to prevent a cross flow between the carrier fluid collection connection and the sheath fluid connection, - wherein the porous structure is prepared and arranged in such a way that an envelope side (10) is separated from a carrier side (1) at least partially and/or at least in regions in a permeable manner, - wherein a carrier fluid can be provided on the carrier side, - wherein the porous structure is prepared to ensure a mass transfer of the carrier fluid with the shell side.

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