Apparatus and method for recovering value materials

Abstract

Membrane filter press comprising two end elements and a plurality of filter elements, in which a main space is formed in each case between two filter elements and an associated frame section, which is separated from a rear or filtrate space by a filter medium, wherein at least one filter element is formed from two filter elements forming a main space as a membrane filter element and comprises a fluidizable interior which is delimited in the direction of the filter medium by at least one flexible membrane, and wherein the main space has at least one feed channel for a substance mixture to be separated, the rear or filtrate space comprises at least one filtrate channel for filtrate, in particular at least one filtrate channel leading to a collection channel, and wherein the main space comprises not only a feed channel, but also at least one discharge opening, in particular a discharge opening arranged vertically above the feed channel. The invention further includes apparatuses and methods for producing solid products and / or valuable materials.

Description

Technical Field

[0001] This invention relates to membrane filter presses, apparatuses, and methods for improved separation of solid products or valuable materials. Background Technology

[0002] Various methods and apparatuses are known in the chemical industry for separating solid products and / or valuable materials from byproducts or by-products in single-stage or multi-stage processing downstream of actual chemical reactions. These typically employ filtration or separation devices that operate continuously or intermittently.

[0003] Intermittently operating vertical filter presses or membrane filter presses with filter plates suspended adjacent to each other exhibit high dehumidification rates and are known, for example, conventional embodiments for solid-liquid filtration from DE 20 2021 101 89 U1, DE 20 2018 104 129 U1, or DE 10 2015 007 535A1. Membrane filter presses comprise up to 200 membrane filter plates arranged parallel to each other between a top plate and end plates. Combining membrane-free rigid filter plates with membrane filter plates to provide plate sets is also known. Flexible or movable membranes are disposed on both side surfaces of the membrane filter plates and are driven and restored by filling the internal space with, for example, water. This step is used for pressing and dewatering the resulting filter cake at the end of the loading phase, after which the membrane filter press needs to be opened and emptied. The membrane can form a single integral assembly with the membrane filter plates or can be a replaceable assembly. The membrane filter press disclosed in DE 20 2018 104 129 U1 has a central feed and each plate has a central opening through which the mixture of substances to be separated (feed) can flow from one filter space to an adjacent filter space. Four collection channels for discharging filtrate are formed by channel sections in each plate, which form a corresponding common flow channel in the closed structure of the membrane filter press.

[0004] DE 10 2007 027033 B4 discloses a membrane filter press that achieves deeper treatment of the filter cake by allowing unwanted substances to be washed out through flushing. For this purpose, the plates have continuous flushing channels on both edges. An inlet element leads from the supply flushing channel to the corresponding filter space, while an outlet element leads to the outlet flushing channel and exits the filter space without passing through the filter media. Thus, the filter cake can be flushed, for example, with water or a liquefied medium, and unwanted adhering substances can be removed.

[0005] In well-known methods of methionine production, it is known to use a filtration device to discharge and treat the mother liquor from methionine production, removing unreacted liquid substances and inhibitors. The amino acid methionine is used in many fields, such as pharmaceuticals, health and fitness products, but particularly as a feed additive in many feeds for various livestock. On an industrial scale, methionine is chemically produced via the Bucherer-Bergs reaction, a variant of the Strecker synthesis. The starting material 3-methylmercaptopropionaldehyde (MMP, produced from 2-propenal and methylthiol), hydrogen cyanide, ammonia, and carbon dioxide are reacted to give 5-(2-methylmercaptoethyl)hydantoin (methionine hydantoin), and this is subsequently subjected to alkaline hydrolysis with alkali metal hydroxides and / or alkali metal carbonates and alkali metal bicarbonates, such as potassium hydroxide and / or potassium carbonate and potassium bicarbonate, to give an alkali metal methionine salt (e.g., potassium methionine) (see Formula 1).

[0006] Formula 1: Methionine hydantoin saponification

[0007]

[0008] The solid product methionine is ultimately released from its alkali metal salt by acidification, such as with carbon dioxide (carbonation) (see Formula 2), and filtered out as a precipitate from a suspension containing alkali metal carbonates and alkali metal bicarbonates (e.g., potassium carbonate and potassium bicarbonate).

[0009] Formula 2: Carbonation

[0010]

[0011] Continuous filtration is performed, for example using a separation or filtration unit, in which the filtrate, i.e., a mother liquor (first mother liquor) containing alkali metal bicarbonates (e.g., potassium carbonate and potassium bicarbonate), is recycled to saponify methionine hydantoin. Such a method is disclosed, for example, in EP 780 370A2.

[0012] As with all recycling methods, this approach requires filtrate discharge to ensure that the various precursors and formed byproducts, particularly formate, do not increase to acceptable levels, as these are inhibitors. However, the discharged filtrate still contains the product methionine, alkali metal carbonates and alkali metal bicarbonates (e.g., potassium carbonate and potassium bicarbonate) that can be used for the saponification of methionine hydantoin. To recover as much methionine and potassium bicarbonate as possible from the filtrate, a secondary carbonation of the discharged filtrate can be performed.

[0013] Obtaining methionine and potassium bicarbonate from the first mother liquor via secondary carbonation is the subject of various methods disclosed, for example, in DE 2 421167A1, which proposes separation by centrifugation after carbonation. Alternatively, EP 839804A2 proposes using a water-soluble liquefaction medium to precipitate methionine, which introduces additional effort and potential impurities.

[0014] Although the separation devices are known and tested, the separation process often requires extensive manual effort to thoroughly clean the separation device, especially for separation devices that can achieve particularly high dryness values, such as filters or membrane presses. Summary of the Invention

[0015] Therefore, one object of the present invention is to provide an improved separation apparatus that enables higher performance of apparatus or methods for solid products and / or solid valuable materials.

[0016] The objective is achieved by an apparatus for producing solid products and / or valuable materials having the features of claim 1 and a method for producing solid products and / or valuable materials having the features of claim 10.

[0017] The apparatus is configured for producing solid or solidifiable products and / or valuable materials, particularly for producing at least one product and / or at least one valuable material in a mixture of liquid substances. It includes a process unit and at least one connected separation unit, wherein the process unit comprises the following:

[0018] - At least one reactor for precipitating or solidifying the valuable material.

[0019] - At least one feed conduit leading to the processor unit and / or the reactor, for introducing at least one reactant and, if necessary, additional (auxiliary) substances.

[0020] - A connecting conduit for discharging a suspension containing at least one precipitated solid valuable material as a liquid mixture to a separation unit, wherein the separation unit is configured to separate the solid valuable material from the suspension. The separation unit includes at least one membrane filter press, wherein the membrane filter press is connected via...

[0021] • The conduit connects to the receiving and conditioning unit, and via

[0022] • The return conduit connects to the process unit.

[0023] In this document, "solid products and / or solid valuable materials" are collectively referred to as "valuable materials," wherein, unless otherwise specified, valuable materials should be understood to mean substances or mixtures thereof that have a positive effect on the method when recycled upstream of the apparatus used for solid separation of valuable materials and / or liquefaction according to the present invention. In particular, valuable materials are not inhibitors or contaminants, and / or do not adversely affect the quality of the corresponding method and / or product. In the context of the present invention, valuable materials may be selected accordingly from, for example, reactants, byproducts, auxiliaries, and / or final products of the corresponding method used for the final product. Products and / or valuable materials are, in particular, chemical substances or mixtures of substances. In the context of the present invention, unless otherwise specified, "byproduct" is also used synonymously for all substances in the mixture that do not constitute solid "valuable materials."

[0024] In the first embodiment, the receiving and conditioning unit is a heat exchanger or heating device by means of which the liquefied medium is brought to a temperature at least equal to the melting or dissolution temperature of the solid valuable material, ideally at least 5% higher than the liquefaction or dissolution temperature of the solid valuable material. In the case of producing methionine and its liquefaction, it is advantageous to establish a temperature not lower than 60°C, ideally not lower than 70°C.

[0025] The receiving and conditioning unit can also be an adjacent process unit or device unit from which a suitable liquefied medium can be obtained.

[0026] The term "reactants" should be understood to refer to all starting materials and auxiliaries, and optionally flowable or liquid catalysts, collectively referred to as reactants in simplified terminology. Unless otherwise indicated, the state of matter generally refers to standard conditions of 1 bar and 20°C, or typical process conditions known to those skilled in the art, such as those outside the scope of this invention.

[0027] Furthermore, the numerical indication of “one (a)” unit, such as “one reactor”, should be understood to include two or more units, and is not necessarily limited to a “single” unit.

[0028] Finally, the term "connection" should be understood not only to refer to a direct connection, but also to a conduit or conduit connection in which secondary units for the present invention are arranged, such as valve manifolds, storage tanks, or indirect heat exchangers.

[0029] The membrane filter presses included in this device include the following:

[0030] The filter press comprises two end frames, a plurality of filter elements arranged between the end frames, at least one feed channel for the suspension, and at least one collection channel for discharging the filtrate. In each case, a filter chamber is formed between the two filter elements and the associated frame segment, which is divided into a main space and a post-filtrate space by an insertable filter medium. At least one filter element is formed as a membrane filter element by the two filter elements forming the main space and has a fluidizable interior. The fluidizable interior of the membrane filter element may also be formed by a plurality of subspaces interconnected by channels or conduits. The at least one interior is demarcated by at least one flexible membrane in the direction of the main space / inserted filter medium. The flexible membrane ideally forms at least one wall or wall segment of the interior and can be moved, stretched, or expanded in the direction of the main space by increasing the internal pressure. The main space has at least one feed channel for or connected to the mixture of substances to be separated. The post-filtrate space has at least one filtrate channel for discharging the filtrate or is connected to such a filtrate channel, wherein advantageously, the at least one filtrate channel leads to the collection channel, thereby allowing the filtrate to be discharged from the membrane filter press. The collection channel is advantageously formed by multiple channel segments, each channel segment being arranged in the filter element and together forming the entire collection channel.

[0031] The main chamber includes not only the feed inlet but also at least one discharge outlet, particularly the discharge outlet arranged vertically above the feed channel.

[0032] In other words, a liquefied medium can be established to traverse the main space directly from the inlet of the mixture of substances to be separated to the additional outlet, without passing the liquefied medium through the filter medium, particularly the passage leading to the filtrate and / or the filtrate collection passage. This also differs from known filter presses or membrane filter presses, where the main space with the formed filter cake can be flushed by injecting, for example, fluid via an upper inlet flushing passage, which is then discharged again via a lower outlet flushing passage, where no inlet or feed passage is integrated.

[0033] The filter element can, in principle, have any polygonal, circular, or elliptical shape. Advantageously, the filter element has a basic shape of square, rectangular, or up to octagonal. The element has a lower frame section, an upper frame section, and side frame sections. In the case of a square filter element, these are the lower frame section, the upper frame section, and two side frame sections, with framed or edge regions.

[0034] Although the location of the filter media describes the membrane filter press and the space it forms, as well as its flow channels, and that the membrane filter press can only work effectively with the filter media, the filter media is a consumable component and is not usually part of the membrane filter press.

[0035] The terms “fram” or “edge area” should not be understood as geometrically restricted, and in particular as the area of ​​a filter element that contacts adjacent filter elements and / or to which the filter media is attached.

[0036] Furthermore, the term "filter element" should be understood to also include a group of elements, especially frame-type or plate-type elements, which together form a filter element, particularly a group of elements stacked together parallel to the plane spanned by the filter medium to form a filter element, and also include corresponding fluid channels, particularly internal fluid channels.

[0037] Therefore, for example, two circumferential elements or frames can each carry the filter media, while the central element forms a partition and support wall, so that the three elements together form a filter element. In a similar manner, the circumferential elements or frames can each carry the filter media, while the central element has at least one expandable membrane and does not itself include the filter media; together, these elements form a complete membrane assembly.

[0038] Other aspects of the basic construction of a filter press or membrane filter press, and their further details, are well known, such as the external support structure, sealing devices, internal geometry, drive mechanisms for opening, closing, and compressing the filter elements, membrane filter frames and their different sequences, discharge devices, connecting elements for the media to the top plate, etc., so that these and other aspects can be added and / or combined by those skilled in the art as needed. This also applies to the process engineering requirements for operating the filter or membrane filter press. In particular, one of the two end elements, namely the top plate / element, includes at least one connecting element, such as a flange or quick-connect fitting for each (internal) channel or conduit.

[0039] In a known manner, the head element is particularly the idle side, while the opposite end element is the movable side, which is moved by means of a motor to seal and compress the membrane filter press.

[0040] In an advantageous embodiment, the at least one feed conduit may be positioned in the lower vertical frame section. This has the advantage that, upon feed introduction, any accumulated gas is directed upwards to, for example, a discharge port or filtrate channel and can be released. Furthermore, during the liquefaction step, the filter cake is positioned vertically below the introduced liquefaction medium so that the discharge port remains largely open, and the most intense possible mixing of the solids (filter cake / filter cake block) with the flowing liquefaction medium is achieved.

[0041] In a further advantageous embodiment, it can thus be similarly ensured that the at least one discharge port arranged vertically above the feed channel is arranged in the vertical upper frame section.

[0042] Since the liquefied medium must bridge the main space that is largely filled with filter cake, i.e., experience high flow resistance at least temporarily, a further advantageous embodiment may specify that the number of lower feed channels or supply channels is at least one more than the number of outflow / discharge channels.

[0043] It has proven particularly advantageous to have two lower feed ports and / or feed channels and one upper discharge port / one upper discharge channel in the filter element.

[0044] Therefore, in a further advantageous embodiment, the ratio of the total flow cross-section of the feed channel to the total flow cross-section of the discharge channel is specified to be in the range of 1:3 to 2:1, ideally in the range of 1:2 to 1:1. This ensures that fresh liquefied medium can flow in at any time without excessive flow resistance, and furthermore, smaller fragments of the filter cake are discharged as solids and optionally completely dissolved during subsequent transport.

[0045] Advantageously, the separation unit includes two, three, or four filtration devices and / or two, three, or four sub-units, said sub-units including a sedimentation reactor and subsequent filtration devices, which are connected in series for optimal discharge of valuable material. Depending on the valuable material to be separated, the filtration devices can be connected in series with increasing fineness, i.e., decreasing average sieve mesh size or average pore size, and / or multiple sedimentation steps and respective subsequent solid-liquid separations can be performed, particularly using filtration devices. It will be apparent to those skilled in the art that, depending on the volumetric flow rate to be treated, the separation unit may include multiple parallel flow paths for a portion of the volumetric flow to separate valuable material from the respective portion of the volumetric flow, wherein each flow path for the portion of the volumetric flow may similarly include a sub-unit, a sedimentation reactor, and / or a filtration device.

[0046] In the improvement of this device, it may be advantageous to configure the membrane filter press according to one of the aforementioned embodiments and / or variations.

[0047] It may be particularly advantageous that the last sub-unit and / or the last filtration device is a membrane filter press according to the invention or a similar filter press that can be emptied and / or regenerated using a liquefied medium.

[0048] It may be advantageous that at least two of the flow paths of the separation unit (each guiding a portion of the volumetric material flow) are connected to a common membrane filter press according to the invention, which can be emptied and / or regenerated using a liquefied medium. It may be particularly advantageous that, in one to n filtration or separation units for valuable materials, the nth filtration unit along the main processing direction or the main flow direction, i.e., the last filtration unit, is a membrane filter press according to the invention. All aspects and advantages already set forth with respect to the membrane filter press should apply in the same manner or in similar applications to the device, and vice versa, unless these aspects and advantages are excluded for physical or chemical reasons.

[0049] In a further improvement to the apparatus, it may be advantageous for the membrane filter press to include multiple filter elements, wherein in each case a main space is formed between two adjacent filter elements, wherein at least two main spaces are connected to at least one discharge channel of the membrane filter press via their respective discharge ports, and wherein said at least one discharge channel is connected to a process unit, particularly the reactor of the process unit. The discharge channel is advantageously connected to a container or storage tank arranged upstream of the process unit.

[0050] The collection conduit, particularly the internal collection conduit, is to be understood as meaning that the conduit is formed by channel sections of various filter elements, and advantageously, each channel section is an integral part of its respective filter element.

[0051] The connection between the collection conduit and the process unit or the reactor of the process unit can also be achieved through post-treatment stages, intermediate treatments, etc.

[0052] In a further improvement to this device, it may be advantageous to connect the feed channel / inlet of the corresponding main space of the membrane filter press as follows:

[0053] I. Filtrate conduction conduit (outflow) connected to the upstream separation unit,

[0054] II. Flow paths (outflows) connected to the outlets of the process unit, particularly direct flow paths, and / or

[0055] III. Connected to a receiving and conditioning unit for providing the liquefied medium, particularly a separate receiving and conditioning unit. Here, "separate" should be understood as meaning that the unit is not integrated into the main process and is connected to the main process only for the liquefaction / regeneration step of the separation unit.

[0056] In Alternative Option I, it is particularly likely that the membrane filter press is the last filtration unit in the system at position n, and serves as the liquefaction medium, with the filtrate, if required to be conditioned, originating from the upstream filtration unit at position n-1. In this case, the number of filtration units n can be particularly 2, 3, 4, or 5. It may be particularly advantageous that at least one or more filtration units at positions 1 to n-1 are continuously operating filters or separation units.

[0057] In other words, the liquefied medium is particularly a suspension, mixture of substances, or filtrate originating from one of the following three flow paths, wherein

[0058] - In Case I, optionally after further chemical and / or physical conditioning, at least part of the filtrate from the upstream separation unit is utilized.

[0059] - In Case II, at least one separation device, at least partially or completely bypassing the separation unit, is used to guide the flow path of the suspension or mixture of substances to the liquefaction of the valuable material.

[0060] - In Case III, the liquefied medium is removed from a separate receiving and conditioning unit for liquefaction.

[0061] A key aspect of variant I may be that a more significant concentration of potentially detrimental inhibitors or contaminants may occur during recycling back to the process unit, depending on the respective process.

[0062] Variant III enables optimal conditioning and selection of the liquefaction medium, but its drawback is that it requires the greatest construction effort. Therefore, Variant I may have particular advantages for liquefaction, as it allows the direct use of the filtrate, which is present in the method and has already been depleted of at least one valuable material, i.e., the filtrate, which is also depleted in terms of total volume, as the liquefaction medium.

[0063] In variants I or II, conditioning can also be performed on the flow path leading to the separation unit to be regenerated, for example, temperature regulation for optimal liquefaction.

[0064] In an advantageous configuration of the apparatus, the device is used to produce methionine. Methionine is precipitated from a mixture of substances by carbonation. The apparatus advantageously includes at least two separation units, wherein the first separation unit is advantageously a continuous separation unit, such as a centrifuge, a rotary vacuum filter, or a vacuum belt filter. Advantageously, for the precipitation of valuable material, each separation unit has a carbonation reactor arranged upstream thereon, particularly a gas conduit (e.g., for CO2 introduction) connected to the carbonation reactor.

[0065] Advantageously, the last separation unit is a membrane filter press configured according to one of the above embodiments or variations.

[0066] The present invention further relates to a method for producing solid products and / or solid valuable materials using an apparatus, particularly for producing at least one of the products and / or at least one valuable material in a mixture of liquid substances, comprising the following steps:

[0067] a. Provide process units and separation units,

[0068] b. Introducing at least one reactant and, if necessary, additional (auxiliary) substances into a process unit to produce and precipitate at least one solid valuable material in a suspension, particularly downstream of production / downstream of the unit and / or downstream of the production (synthesis) site.

[0069] c. In the separation unit, at least one separation device is used to separate the at least one solid valuable material and discharge the at least one by-product.

[0070] d.

[0071] This includes performing the following steps:

[0072] e. At least one fraction of the separable valuable material is collected as a filter cake in the at least one separation device. Collection is specifically understood here to mean the temporary enrichment, accumulation, or filling of valuable material within the separation device by inflow via at least one feed channel. This results in an increase in pressure within the separation device, particularly the main space, while displacing gas and / or filtrate is discharged. The filtrate and, at least temporarily, the gas passes through their respective filter media and exits the separation device via a filtrate channel and advantageously via at least one collection conduit. The gas may also be discharged via other (gas) channels, temporarily or permanently adapted thereto, such as the discharge channel for the liquefied medium described below, which is vacant during this method step.

[0073] f. The at least one quantity of valuable material is dehumidified in the at least one separation device, wherein, advantageously, the dehumidification of the valuable material is carried out at least until a residual moisture content of less than 60%, ideally to a residual moisture content of not less than 35% and not more than 10%. Dehumidification can be carried out in one or more stages, particularly also pneumatically by introducing a gas or gas mixture and / or mechanically by pressure generated by a fluid. The pressure in mechanical dehumidification is advantageously generated by an incompressible medium, particularly using a liquid that presses against the pressing membrane in the direction of the filter cake (valuable material).

[0074] g. The at least one amount of valuable material collected in the at least one separation device and solidified into a filter cake is liquefied within the separation device using a liquefaction medium.

[0075] The term "within the separation unit" should be understood to mean that the valuable material to be liquefied is not discharged, and therefore the separation unit is not opened after collection and single or multi-stage dehumidification. The liquefied medium is advantageously introduced into the main space of the filter element of the membrane filter press via one or more feed channels and inlets after complete filling (collection).

[0076] h. Recycle the liquefied valuable materials back into the process unit and / or discharge them into storage tanks.

[0077] This step, and therefore an alternative variant of the method, may stipulate that the valuable material dissolved in the liquefaction medium is at least temporarily stored in a tank, particularly in an intermediate storage, and, if necessary, further conditioning is carried out before being introduced upstream of the separation unit at a location relevant to the main production process.

[0078] In an alternative embodiment of the method, a purging step may precede the liquefaction step f, in which the separation device is opened and the filter cake, or a portion thereof, is discharged by gravity, i.e., falls off, especially if this is possible without manual and / or mechanical intervention. In other words, the purging step in these method variants involves incomplete purging and avoids greater manual cleaning work.

[0079] The separation unit is then shut off again, sealed by compression, and the remaining adherent filter cake or fragments thereof are liquefied. It may be advantageous to remove, for example, the deposits on at least the sealed surfaces before shutting off the separation unit and liquefying, using a brush or compressed air.

[0080] In a further improved variation of the method, it can be specified that the dehumidification of valuable materials is carried out in at least two series-connected separation devices in at least two sub-steps, wherein

[0081] - In the first sub-step, a first quantity of valuable material is separated and dehumidified, wherein the filtrate separated in the first separation device is sent to a second separation device, and wherein...

[0082] - In the second sub-step, valuable materials present in the filtrate are separated and dehumidified.

[0083] It may also be advantageous that the first separation device is a continuously operating separation device, particularly a vacuum filter, such as a drum filter or a belt filter, or a continuously operating centrifuge or another centrifugal separator, and wherein the second separation device is a chamber filter press, particularly a chamber filter press or a membrane chamber filter press.

[0084] In a further improved variation of the method, it can be specified that dehumidification in the first sub-step is carried out until the residual moisture content of the separated valuable material is 60% to 30%, and dehumidification in the second sub-step is carried out until the residual moisture content of the separated valuable material is in the range of 45% to 10%. Specific separation performance is highly dependent on the respective substances to be separated and the separation apparatus. Ideally, the first sub-step includes dehumidification until the residual moisture content of the separated valuable material is 60% to 40%, and the second sub-step involves dehumidification until the residual moisture content of the separated valuable material is in the range of 35% to no more than 15%, ideally in the range of 30% to 10%.

[0085] It is potentially advantageous that the filter media is exempt from the burden of passing through the liquefied medium. Therefore, in an improved variation of the method, a pressure increase is specified in the filtrate space or downstream space during the process of supplying the liquefied medium into the main space and discharging it via one or more discharge channels. This pressure in the filtrate space or downstream space should be at least equal to or slightly higher than the pressure in the main space, and can be achieved by introducing a fluid, particularly a gas. To prevent sedimentation, the fluid is advantageously heated, particularly to the temperature predominant in the main space / to the temperature of the liquefied medium.

[0086] In a further improved variation of the method, it may be specified that the liquefaction medium used for liquefying valuable materials collected within the at least one separation device is an acid and / or a base, specifically not a mixture of substances, not a filtrate, or not a suspension, i.e., not an acid or base removed from the device or the method at an upstream location.

[0087] It may be advantageous that liquefaction includes conditioning the liquefaction medium, particularly heating and / or adjusting the pH. pH adjustment is carried out in known ways by adding an acid or alkali. Particularly advantageous is that the liquefaction medium is derived as a filtrate from an upstream process stage of the separation unit, where it may be advantageous to condition the filtrate for dissolving valuable materials.

[0088] In a similar manner, it may be advantageous to supply the filtrate from the first separation unit to the conditioning unit for a conditioning step before introducing the second separation unit / second separation step, wherein the conditioning step is for deeper precipitation of valuable materials and filtrate.

[0089] - Post-reaction with reactants / by adding reactants, and / or

[0090] - To change process parameters, such as temperature and pressure.

[0091] In a further improved variation of the method, it may be specified that, during the liquefaction process, the (separated) valuable material collected inside the at least one separation device is subjected to a flow of liquefying medium from below in the direction of gravity, and is discharged from its respective main space and its respective filter element in the direction of gravity above and / or above the feed channel.

[0092] The introduction of the liquefied medium is ideally achieved via the at least one feed channel for feeding. For this purpose, conduit connections, ports, connecting elements, valves, etc., can be provided.

[0093] A particular advantage is that portions or fragments of valuable material that are optionally dissolved but not yet liquefied fall toward the incoming fresh liquefied medium, while the discharge port remains open. In contrast, small fragments of valuable material that are still solid may be entrained, which could be intentional.

[0094] In one development of this method, a screen or mesh structure can be provided in or upstream of the discharge port to specify the maximum size of the filter cake / fragments of valuable material that can be washed out.

[0095] It is highly advantageous to use sensors to monitor the liquefaction process. This can be achieved, for example, by measuring flow rate, pressure, pressure differential, vibration, conductivity, capacitive load, or their progression over time. Particularly advantageous in batch operations is the ability to determine the end or extent of liquefaction, and thus the output of valuable material, allowing for the termination of the cycle. Such sensors are advantageously included in each main chamber or each discharge port. This allows the separation unit to be opened at defined points and individual faulty filter elements to be replaced as needed. This is particularly advantageous because, compared to the typical operating mode of a membrane filter press, continuous optical inspections via manual evacuation of the filter press by the operator are not required.

[0096] The method according to any one of the preceding claims is characterized in that the method is used to produce solid valuable materials methionine and / or methionyl-methionine (a dipeptide of methionine; met-met).

[0097] The liquefaction medium is advantageously a mixture of substances from an upstream unit, particularly from the effluent suspension of the first or second carbonation unit or from the filtrate of an upstream separation unit, such as a continuous filtration unit. Pre-conditioning can be provided, which may specifically consist of a temperature increase. Advantageously, the temperature of the mixture is increased to above 65°C, ideally above 75°C. The temperature of the liquefaction medium is not greater than 115°C, ideally 110°C.

[0098] It may be entirely advantageous to provide a membrane filter press and / or apparatus with at least one configuration according to the exemplary embodiments or variations described herein for the method.

[0099] All aspects and advantages already set forth above with respect to the membrane filter press or the apparatus should be applied in the same manner or in similar applications to this method, and vice versa, unless such aspects and advantages are excluded or not applicable for physical or chemical reasons.

[0100] The invention is described more specifically below with reference to exemplary embodiments and accompanying drawings. Attached Figure Description

[0101] In the attached diagram:

[0102] Figure 1 A first exemplary embodiment is shown as a schematic diagram of the apparatus and method.

[0103] Figure 2 Another exemplary embodiment is shown as a schematic diagram of the apparatus and method.

[0104] Figure 3 Two exemplary embodiments of a membrane filter press are shown in two partial diagrams, A) and B).

[0105] Figure 4 Further exemplary embodiments of the membrane filter press are shown in two partial diagrams, A) and B).

[0106] Figure 5 Further exemplary embodiments of the membrane filter press are shown in two partial diagrams, A) and B), and

[0107] Figure 6 This diagram shows different feeds on the end or head components.

[0108] Figure 1This apparatus is shown for producing at least one solid or solidifiable valuable material. The apparatus 100 includes a process unit 200 having a feed conduit 204 for reactants not further specified or distinguished and an outlet 216. For post-processing of the liquid mixture, the outlet 216 is connected via a connecting conduit 206 to a separation unit 300. The separation unit 300 includes a first separation device 302 and a second separation device 304. The first separation device 302 includes a discharge conduit 318 for valuable materials, particularly solid valuable materials, and a connecting conduit 314 leading to the second separation device 304, into which the filtrate from the first separation device 302 is conveyed. A receiving and conditioning unit 400 is disposed in the connecting conduit 314 and upstream of the second connecting conduit 304. The receiving and conditioning unit 400 can be used to alter the chemical and / or physical properties of the depleted mixture of materials, such as the filtrate from the first separation device 302, to achieve deeper material separation. Further solid precipitation is particularly important for this purpose. The second separation device 304 is connected to the process unit 200 via a (recirculation) conduit 208. The conduit 314 connecting the two separation devices 302 and 304 includes a bypass conduit 326, thereby bypassing the receiving and conditioning unit 400.

[0109] Deeper solid precipitation can be achieved by lowering the temperature, for example, using an indirect heat exchanger, and, depending on the substance, by precipitating crystalline solids. This solid is particularly the same as or substantially the same as the solid previously separated in the first separation unit 302. Alternatively, separation stage 400 includes a feed conduit for reactants and a mixing unit and / or reactor to achieve a chemical reaction and precipitation of at least one of the substances carried in conduit 314. The solid material to be precipitated in the flow path from the first separation unit 302 to the second separation unit is particularly the same as the valuable material of process unit 200 / the solid material or valuable material separated by the first separation unit 302.

[0110] According to Figure 2 In the example shown, in the second separation device 304, the suspension is further depleted of valuable materials, and the (second) filtrate is discharged via conduit 312 and deposited in container 230. The second separation device 304 is a membrane filter press in which solids are collected and dehumidified in an intermittent operation.

[0111] After separating solid valuable materials through the first separation device 302 and discharging the at least one filtrate as a mixture of substances into the second separation device 304, the first method step includes collecting the precipitated valuable materials as a filter cake in the second separation device 304, wherein optionally, further conditioning of the filtrate and precipitation of the solid valuable materials have been performed beforehand. A further method step includes single-stage or multi-stage dehumidification of the separated valuable materials in the second separation device 304, wherein the encapsulated filter cake is subjected to gas, particularly air or inert gas, under increased pressure in the filter space and / or the main space for a period of time, and / or mechanically squeezed via a hydraulically activated membrane 360. Figure 3 ).

[0112] This separates the valuable material from the attached liquid phase, thus also largely removing harmful byproducts and inhibitors, where the valuable material has a residual moisture content of no more than 30% to 15%.

[0113] Filtration using a membrane filter press is highly efficient, and liquid contaminants or inhibitors can be effectively separated from the filter cake in this way. However, emptying a membrane filter press is typically very time-consuming and often requires manual operation. Furthermore, depending on the type of filter cake and / or mixture present, the membrane filter press may need to be operated while taking specific protective measures, as the mixture or solid filter cake may contain hazardous substances.

[0114] Therefore, according to the present invention, in subsequent method steps, the membrane filter press is not opened for evacuation and regeneration; instead, liquefaction of the filter cake / solid valuable material is achieved by passing the liquefied medium through the main chamber of the membrane filter press. Advantageously, the liquefied medium is passed through the main chamber of the filter element of the membrane filter press in a manner that prevents or substantially prevents the flow of the liquefied medium through the filter medium.

[0115] The liquefied medium, which enriches and liquefies valuable material (filter cake), is recycled to process unit 200 via conduit 208.

[0116] exist Figure 1 In the example shown, the liquefaction medium is the filtrate from the first separation unit 302, which is conducted in conduit 314 and has previously been conditioned in the receiving and conditioning unit 400, particularly by increasing the temperature to liquefy the collected filter cake. After liquefaction inside the second separation unit 304, the filtrate / enriched liquefaction medium containing valuable materials is recycled to the process unit 200 via conduit 208.

[0117] Figure 2 Display and Figure 1A corresponding apparatus and accompanying method. Process unit 200 includes a first reactor 201 and a second reactor 202, wherein reactants are introduced into the first reactor 201 and at least one reaction or synthesis step is carried out. The second reactor 202 is a precipitation reactor, in which, for example, crystallization of a solid valuable material is initiated. Additional reactants or auxiliaries may be introduced into the second reactor 202 for precipitation or crystallization, but this is not shown in this case. Apparatus 100 includes a central control unit 500, and the various units and devices are connected to the central control unit 500 via control and data lines 210.

[0118] The outlet 216 of process unit 200 is connected via connecting conduit 206 to a first separation unit 302, which is in the form of a continuously operating vacuum filtration unit and includes a vacuum unit 310. The suspension conducted in connecting conduit 206 is applied via application unit 306 to a continuously recirculating belt filter 308 that interacts with the vacuum unit 310 in a known manner. The separated solid valuable material, having a first residual moisture content, is conveyed through transport section 318 and collected in container 320. The filtrate from the vacuum unit 310 is temporarily supplied via conduit 314 to container 322 for subsequent supply to a second discontinuously (intermittently) operating separation unit 304. A reactor 330 is provided downstream of the vacuum unit 310, to which reactants are supplied in an unspecified manner to achieve deeper precipitation of the same or different solid valuable materials from the effluent mixture (filtrate) of the first separation unit 302. The reactor 330 downstream of the first separation unit 302 typically precipitates the same valuable material from the filtrate in an enhanced manner. As described above, in the first stage of this method, the suspension is supplied via conduit 314 to a second separation device 304 in the form of a membrane filter press 340, and as specifically combined Figures 3 to 6 The process involves collecting valuable solid materials into a filter cake, and then dehumidifying the filter cake.

[0119] In order to provide a liquefaction medium for liquefying filter cake in a closed membrane filter press 340, Figure 2 A total of three alternative implementation schemes are displayed, of which only one is typically provided permanently:

[0120] I. As a first alternative, the liquefaction medium can be generated via conduit 314 as a conditioning filtrate from the filtrate of the first separation unit 302, wherein the conditioning unit 400 consists essentially of a heat exchanger 420 arranged upstream of the second separation unit 304. In a variant, the size and connection of the reactor 330 provided for the precipitation reaction are such that, during the regeneration of the second separation unit 304, the reactor also serves purely as a buffer vessel and / or as part of the conditioning unit 400 to provide the liquefaction medium required for the liquefaction of valuable materials.

[0121] In one variant of this alternative, reactor 330 is bypassed to carry out the filter cake liquefaction step in the second separation unit 304.

[0122] II. A second alternative involves supplying a mass of the mixture or suspension of substances directly from process unit 200 to second separation unit 304, bypassing first separation unit 302. For this purpose, the flow path leads to conduit 314 via outlet 216, first valve unit 220, conduit 214 acting as a bypass to first separation unit 302, and second valve unit 226 upstream of heat exchanger 420. In this alternative, heat exchanger 420 essentially forms conditioning unit 400.

[0123] Advantageously, a second quantity of the mixture or suspension of materials from process unit 200 is simultaneously supplied to the first separation unit 302, and the filtrate is piled in a suitable container or reactor until the downstream separation unit 304 is regenerated (emptied) via bypass conduit 214. In particularly advantageous method modes and apparatus configurations, the main production process of the valuable materials does not need to be completely interrupted.

[0124] III. A third alternative includes a completely separate receiving and conditioning unit 400, such as in Figure 2 The lower right side is shown schematically and outlined by a dashed line. This receiving and conditioning unit 400 provides the liquefaction medium required for the liquefaction of valuable solid materials from the second separation unit 304, for example in the form of a pure solvent, such as an alkali or acid, and can condition or meter it as needed. As shown, the solvent thus provided enters the supply conduit 314 via another valve unit 222 upstream of the second separation unit 304, which can also be implemented at different suitable locations upstream of the second separation unit 304 and / or directly introduced into the separation unit 304.

[0125] The receiving and conditioning unit 400, integrated in Alternative Option III and providing additional liquefied media, is shown in a highly simplified and schematic form. It includes a receiving tank 410 with a feed conduit indicated by arrows, a conduit 412, a heat exchanger 422, and a valve unit 224, optionally including conveying devices and other units (not shown). Valve unit 224 is connected via conduit 316 to valve unit 222 located upstream of the second separation unit 304 (here, a membrane filter press 340), wherein valve unit 222 is integrated into the supply conduit 314 of the second separation unit 304. The connecting conduit shown in dashed lines indicates an alternative or additional connecting conduit 414 leading to another valve unit 226 in conduit 314. Through this connecting conduit 414, liquefied media from the receiving tank 410 can be introduced together with a mixture of substances from conduit 214 or from conduit 314 upstream of the heat exchanger 420 on the suction side of the pump 324, and mixed to form the final liquefied media.

[0126] A liquefied medium rich in fully or substantially liquefied valuable material (filter cake) is fed via conduit 208 into container 232, which is used for stacking and controlled release via conduit 212 into process unit 200 / second reactor 202. In an alternative method (not shown), the enriched liquefied medium is at least partially introduced into first reactor 201.

[0127] The filtrate from the vacuum device 310 enters through the conduit 314 and is at least temporarily stored in the container 322, enabling the process unit 200 and the first separation device 302 to operate continuously or substantially continuously.

[0128] In another exemplary embodiment (not shown), the separation device 300, downstream of the first filtration device 302 and upstream of the end (final) membrane filter press 340 in the filtrate flow path 314, includes one or two (additional) sub-units comprising at least one sedimentation reactor, such as reactor 330, and a filtration device. The filtration device of this (additional) sub-unit is, for example, a continuously operating filtration device, such as a belt or drum vacuum filter, or may be a centrifugal separator.

[0129] Figure 3 The basic construction of the membrane filter press 340 in the two embodiments is shown as a vertical sectional view in two partial diagrams A) and B), wherein the second separation device 304 can be configured according to... Figure 1 or Figure 2 Configuration. These illustrations are greatly simplified so that, for example, media connections, support structures, drive units, fluid connections, or control components of the end or head elements are not shown, as these are known in principle to those skilled in the art. In both partial illustrations, the membrane filter press 340 is shown in the open position, with the membrane filter frames 370 spaced apart from each other. Partial illustration A) shows the membrane filter press 340 having two edge or end elements 342, with only the membrane filter frames 370 arranged between them as filter elements 344.

[0130] Both embodiments include a central feed channel 364 for the mixture of substances to be separated (feed), and collection channels 366 for discharging the filtrate are arranged at the top and bottom of the corners of the filter element 344. The membrane filter press 340 and the individual filter elements 344 can be oriented and operated together at any desired angle or orientation; therefore, terms such as “top,” “above,” “bottom,” or “below” are used for simplicity of description and refer to typical advantageous orientations and arrangements without any intention of general limitation. In the present case, the membrane filter frame 370 and the (rigid) filter frame (without membrane) 372 are shown together as the filter element 344. The indications regarding the filter frame 372 similarly apply to the edge or end elements 342 and their interaction with adjacent filter elements 344.

[0131] Unlike partial illustration A), the membrane filter press 340 according to partial illustration B) is formed by filter elements 344 that alternately include membrane filter frames 370 and filter frames 372, in addition to two edge or end elements 342. All filter elements 344, 370, and 372 are in a vertically suspended orientation.

[0132] Filter elements 344, 370, and 372 each have filter media 354 on both sides, configured as filter fabric or filter pads. In the illustrated embodiment, the filter media 354 is formed by two parallel filter pads connected via a tubular section in a manner not further specified. In the installed state, this tubular section bridges the corresponding central feed port 374 of the filter element 344. The two filter elements 344 / a pair of end elements 342 and adjacent filter elements 344 form a common main space 352, in which the mixture of substances to be separated (feed) is introduced via an uninterrupted feed channel 362 and the feed port 374 in the corresponding filter element 344, and a filter cake is formed therein during collection. In the left end element 342 (also referred to as the head element), the feed channel 362 also serves as the feed port to the subsequent main space 352.

[0133] Viewed from the main space 352, a corresponding filtrate space or rear space 356 is formed at the rear of the filter medium 354, through which one or more filtrate channels 364 lead to one of the four collection channels. The discharge of the filtrate is achieved via the end element 342 (head element) shown on the left, which also facilitates the feeding of the mixture of substances.

[0134] According to the present invention, two discharge ports 376 are provided in each main space 354, thereby discharging and supplying liquefied media and liquefied valuable materials to downstream process units 200. Each discharge port 376 is connected to a discharge channel 378, which in turn is connected to... Figure 1 and Figure 2The return conduit 208 is shown.

[0135] Therefore, the membrane filter press 340 can be regenerated after the filled membrane filter press 340 to generate a short-circuit flow of liquefied media, which flows through the feed channel 362 and through the feed port 374 and the corresponding main chamber 352 in each filter element 344 to the discharge port 376 and into the common discharge channel 378. Detailed Implementation

[0136] Exemplary Implementation

[0137] In the method for producing methionine (MET) described at the beginning of the configuration of the present invention, methionine hydantoin saponification is carried out in reactor 201 according to Formula 1.

[0138] Subsequently, in reactor 202, methionine is released from its alkali metal salt by carbonation with carbon dioxide according to formula 2, and is filtered as a solid from a mixture of substances containing alkali metal carbonates and alkali metal bicarbonates (e.g., potassium carbonate and potassium bicarbonate) in first filtration device 302.

[0139] Prior to the first carbonation, the mixture of substances in feed conduit 204 still contains 119 to 151 g / kg of active potassium cations (a.K+), such as in the form of KHCO3 or K2CO3, and 7.1 to 9.0 g / kg of formate as potassium formate salt. Formate is an inhibitor or contaminant in the methionine process, and it is advantageous to remove it as completely as possible.

[0140] Following the first separation unit 302, the filtrate, having an a.K+ concentration of 61.5 to 78.5 g / kg and a formate concentration of 8.8 to 11.2 g / kg, is subsequently thermally concentrated in an evaporator (not shown). The mixture then enters reactor 330 with a corresponding a.K+ concentration of 114.5 to 145.5 g / kg and a formate concentration of 15.8 to 20.2 g / kg.

[0141] Finally, valuable materials such as methionine, potassium carbonate, potassium bicarbonate, and a certain proportion of byproducts, such as methionyl-methionine (met-met), are filtered out in the second separation unit to obtain a highly concentrated product.

[0142] The equipment for methionine production is based on Figure 2 The configuration may include additional sub-units, such as sedimentation reactors and filtration devices.

[0143] The valuable material methionine is thus fully depleted, and potassium carbonate, potassium bicarbonate and byproduct met-met can be recycled in liquefied form via conduit 208 without any adverse effect on process unit 200.

[0144] Significant performance enhancements were achieved in the entire methionine production process by eliminating the need to open, clean, and reseal the second terminal separation unit 304 configured as a membrane filter press.

[0145] In particular, low system complexity is achieved by eliminating the separate process unit for removing and discharging the filter cake, which would otherwise require encapsulation to prevent condensation and odor carryover to adjacent units. Furthermore, the elimination of the very frequent plate movement per filtration cycle reduces mechanical wear on the filter press components. Plate conveying at the filter press can be largely eliminated. Finally, the filter fabric is also protected, resulting in a longer service life, and clogging of the filter media is minimized. Figure 4 Alternative embodiments of the membrane filter frame 370 (partial view A) and the associated filter frame 372 (partial view B) are shown in two partial views A) and B), where the desired vertical orientation is shown. Figure 3 Unlike previous embodiments, feed channels 362 / two feed channels 362 are arranged in the lower frame section 346, while discharge channel 378 is centrally located in the upper frame section 348. For introducing suspension from the feed channels 362, each filter frame 372 has a shaft-shaped or trough-shaped feed port 374 and a corresponding discharge port 376. Since these feed ports 374 and discharge ports 376 allow the corresponding mixture of substances to pass through the edge of the corresponding filter medium 354, in one embodiment without further specification, the feed ports 374 and discharge ports 376 are in the form of fully or partially enclosed shaft or channel elements extending from the feed channel 362 beyond the edge of the inserted filter medium 354, and are, for example, additionally secured to the filter medium 354 by clamping. Figure 6 Detailed description based on Figure 4 or Figure 5 The operation of the membrane filter press 340 in the implementation scheme.

[0146] Figure 5 Display similar to Figure 4 The membrane filter press 340. Like... Figure 4In this design, the main space 352 is formed on one side by a membrane filter frame 370 (partially shown in Figure A) and on the opposite side by a rigid filter frame 372 (partially shown in Figure B), shown in an open position. The main space 352 has a basic octagonal shape. Two sections of the feed channel 362 are arranged in the lower frame section 346, while the discharge channel 378 is located in the upper frame section 348. Furthermore, a plurality of filtrate channels 364, connected to one of the filtrate collection channels 366, extend out of the main space 352. Corresponding feed ports 374 open into the main space 352 from each feed channel 362. Similarly, discharge ports 376 open into the discharge channel 378 from the main space 352. These feed ports 374 and discharge ports 376 can be combined as follows. Figure 4 The configuration is described.

[0147] Figure 4 and Figure 5 The common feature of the implementation schemes is that the suspension to be filtered (feed) and the liquefied medium are both introduced through the lower feed channel 362.

[0148] according to Figure 4 and Figure 5 The advantage of this implementation is particularly that, when the liquefied medium is introduced into the main space 352, a confined flow is formed, and the fragments of the filter cake fall toward the incoming fresh liquefied medium. Smaller fragments are screened out by the upward flow and are entrained when they reach a sufficiently small size.

[0149] Figure 6 The display shows the end element 342 of the membrane filter press 340, as well as all the feed and discharge options for different media. Figure 6 The following describes in detail the various methodological steps for operating the membrane filter press 340.

[0150] Starting with an empty membrane filter press 340:

[0151] (1) The suspension S is introduced from below via two feed channels 362, wherein the accumulated gas A (typically air) is released simultaneously via an upper collection channel 366 and / or a separate exhaust duct, and wherein the discharge channel 378 is closed (not shown) until the main chamber 352 is completely filled. The discharge channel 378 may be temporarily used to discharge gas A.

[0152] (2) The suspension S is further introduced into the main space via the feed channel 362, and the filter cake is compressed for the first time by the inflowing suspension S, wherein the filtrate FT is discharged via the collection channel 366.

[0153] (3) The main space 352 is completely filled with filter cake and the introduction of suspension S ends. Gas A is introduced into the main space 352 through the upper collection channel 366 to perform deeper dehydration of filter cake, and filtrate FT is discharged through the lower collection channel 366.

[0154] (4) Fluid, particularly water, is introduced into the interior of the membrane filter frame 370 via port 380 (as indicated by double arrow B), which may also be arranged at the top, and the filter cake is compressed and finally dewatered, wherein the compression of the filter cake and the resetting of the membrane form a flow path or flow slot in the main space 352 between at least one side of the (restored) membrane and the filter cake.

[0155] (5) Unloaded liquefied medium VM is introduced from below via two feed channels 362 and loaded liquefied medium VM+ is discharged via the upper discharge channel 378 until the filter cake is completely liquefied / sufficiently small fragments can be discharged.

[0156] (6) Gas A, particularly compressed air (as indicated by the double arrows), is introduced into the main space 352 via the upper collection conduit 366, optionally blocking the upper discharge channel 378. The waiting loaded liquefied medium VM+ is discharged countercurrently via the feed channel 362 by the introduction of gas A and the pressure increase in the main chamber 352, until the loaded liquefied medium VM+ is completely displaced. In this case, the displaced liquefied medium VM+ can be collected in a container, such as the container of the receiving and conditioning unit 400. When it contains, for example, volatile components or harmful substances of the liquefied medium VM, the discharged gas A is purified or filtered as needed.

[0157] (7) Introduce suspension S according to step (1), especially without pre-opening the membrane filter press.

[0158] The opening and closing of working and non-working channels are not performed separately, and are similarly obvious to those skilled in the art from the description of the required flow management / direction.

[0159] In this invention, the terms "suspension" and "mixture of substances to be separated" are used synonymously.

[0160] In this invention, the term "liquefying medium" specifically refers to mixtures, suspensions, or filtrates, or acids or bases of substances used for liquefying valuable solid materials and optionally conditioning them. Furthermore, the term "suspension" should be understood as a heterogeneous mixture of a (continuous) fluid and (dispersed) solids distributed therein.

[0161] List of reference numerals

[0162] 100 devices

[0163] 200 process units

[0164] 201 Reactor

[0165] 202 Reactor

[0166] 204 feed conduit

[0167] 206 Connecting catheters (to 300, 302)

[0168] 208 Return catheter (from 304 to 200)

[0169] 210 data cable

[0170] 212 Return catheter (from 232, 208 to 200)

[0171] 214 (Regenerated) Catheter

[0172] 216 Outlet

[0173] 220 valve unit

[0174] 222 Valve Unit

[0175] 224 Valve Unit (from 400)

[0176] 226 Valve Unit

[0177] 230 containers

[0178] 232 Container

[0179] 300 Separation Unit

[0180] 302 First Separation Device

[0181] 304 Second Separation Device

[0182] 306 Application Unit

[0183] 308 Conveyor Unit, Belt Filter

[0184] 310 Vacuum Device

[0185] 312 Discharge (from 304)

[0186] 314 Catheters (from 302, 310 to 304)

[0187] 316 Catheter (from 400 via 222 to 304)

[0188] 318 Material discharge (from P, from 302)

[0189] 320 container

[0190] 322 Container

[0191] 324 Conveying device, pump

[0192] 326 Bypass catheter

[0193] 330 reactor

[0194] 340 membrane filter press

[0195] 342 Edge / End Components

[0196] 344 Filter Element

[0197] 346 Lower frame section

[0198] 348 Upper frame section

[0199] 350 side frame section

[0200] 352 Main Space

[0201] 354 Filter Media

[0202] 356 Filtrate / Backspace

[0203] 358 Internal

[0204] 360 membrane

[0205] 362 Feed channel (from S)

[0206] 364 Filtration Channel (for FT)

[0207] 366 Collection Channel (for FT, 364)

[0208] 370 Membrane Filter Frame

[0209] 372 Filter Frame

[0210] 374 Inlet (to 352 in the filter frame)

[0211] 376 Discharge port (for S)

[0212] 378 Discharge channel (used for S after 376)

[0213] Port 380 (used for importing B)

[0214] 400 receiving and conditioning unit

[0215] 410 (receiving) tank

[0216] 412 catheter

[0217] 414 Connecting catheter

[0218] 420 heat exchanger

[0219] 422 Heat Exchanger

[0220] 500 control unit

[0221] Fluid 1: Gas, Air

[0222] B Fluid 2: Water

[0223] E reactants

[0224] FT filtrate

[0225] G - Gravity direction

[0226] S suspension

[0227] VM liquefied media

[0228] VM+ liquefied medium, carrying valuable materials

Claims

1. An apparatus (100) for producing at least one product and / or at least one valuable material, comprising a first process unit (200) and at least one connected separation unit (300), wherein the process unit (200) comprises the following: -At least one reactor (201, 202) for processing mixtures of substances, - At least one feed conduit (204) for introducing at least one reactant into said at least one reactor (201, 202), - A connecting conduit (206) for discharging a suspension containing at least one precipitated solid valuable material to the separation unit (300), wherein the separation unit (300) is configured for separating the at least one valuable material, characterized in that... The separation unit (300) includes at least one membrane filter press (340), and wherein the membrane filter press (340) is connected via - The conduits (214, 314) are connected to a receiving and conditioning unit (400) configured for conditioning a liquefied medium to liquefy the at least one valuable material, and via - A return conduit (208) leading to the process unit (200) is connected to recycle the at least one liquefied valuable material.

2. The apparatus according to claim 1, characterized in that... The membrane filter press (302) includes two end elements (342) and a plurality of filter elements (344), wherein in each case a filtration space is formed between the two filter elements (342, 344, 370, 372) and associated frame sections (346, 348, 350), which may be divided by the filter medium (354) into a main space (352) and a downstream or filtrate space (356), wherein at least one filter element (344) is formed by the two filter elements (344) forming the main space (352) as a membrane filter frame (37). 0) is formed and includes a fluidizable interior (358), which is demarcated in the direction of the filter space by at least one flexible membrane (360), and wherein the main space (352) has at least one inlet (374) for the mixture of substances to be separated, particularly an inlet (374) leading to the feed channel (362), and the rear or filtrate space (356) has at least one filtrate channel (364) for filtrate (FT), particularly at least one filtrate channel (364) leading to the collection channel (366), characterized in that The main space (352) includes not only an inlet (374) for the mixture of substances, but also at least one outlet (376), particularly an outlet (376) arranged vertically above the inlet channel (362).

3. The apparatus according to any one of the preceding claims, characterized in that... The membrane filter press (340) includes a plurality of filter elements (344), wherein in each case a main space (352) is formed between two adjacent filter elements (304), wherein at least two main spaces (352) are connected to at least one discharge channel (378) of the membrane filter press (340) via a discharge port (376) in each case, and wherein the discharge channel (378) is connected to the process unit (200).

4. The apparatus according to any one of the preceding claims, characterized in that... The feed channel (362) and the connected main space (352) of the membrane filter press (340) are connected as follows: I. A filtrate transfer conduit (314) connected to the upstream separation device (302), II. The outlet (216) of the process unit (200) is connected via flow paths (214, 314), and / or III. Connected to the receiving and conditioning unit (400) for providing liquefied media.

5. The apparatus according to any one of the preceding claims, characterized in that... The separation unit (300) includes two, three, or four filtration devices (302, 304) and / or two, three, or four sub-units, the sub-units including a sedimentation reactor (330) and a subsequent filtration device (304).

6. The apparatus according to any one of the preceding claims, characterized in that... The at least one feed channel (362) is located in the vertical lower frame section (346).

7. The apparatus according to any one of the preceding claims, characterized in that... The at least one discharge port (376) arranged vertically above the feed channel (362) is located in the vertical upper frame section (348).

8. The apparatus according to any one of the preceding claims, characterized in that... The number of the lower feed channels (362) is at least one more than the number of the upper discharge channels (378).

9. The apparatus according to any one of the preceding claims, characterized in that... The ratio of the total flow cross-section of the feed channel (362) to the total flow cross-section of the discharge channel is in the range of 1:3 to 2:1, ideally in the range of 1:2 to 1:

1.

10. A method for producing at least one solid product and / or solid valuable material in an apparatus (100), comprising the steps of: a. Provide process unit (200) and separation unit (300), b. Introducing at least one reactant into the process unit (200) and generating at least one solid valuable material and byproduct in the mixture of materials. c. In the separation unit (300), at least one separation device (302, 304) is used to separate the solid valuable material and discharge the at least one by-product. Its features d. In the at least one separation device (302, 304), at least one fraction of the separable valuable material is collected as a filter cake. e. The at least one quantity of valuable material is dehumidified in the at least one separation device (302, 304), particularly through multi-stage dehumidification. f. The at least one fraction of valuable material collected in the separation devices (302, 304) and solidified into a filter cake is liquefied inside the separation devices (302, 304) using a liquefaction medium, and g. Recycle the liquefied medium containing valuable materials dissolved therein into the process unit (100) and / or discharge it into the storage tank (232).

11. The method according to claim 10, characterized in that... The valuable material is dehumidified in at least two series-connected separation devices (302, 304) in at least two sub-steps, wherein - In the first sub-step, a first quantity of valuable material is separated and dehumidified, wherein the filtrate (FT) separated in the first separation device (302) is fed into a second separation device, and wherein... - In the second sub-step, valuable materials present in the filtrate (FT) are separated and dehumidified.

12. The method according to claim 11, characterized in that... The dehumidification in the first sub-step is carried out until the residual moisture content of the separated valuable material is as low as 30%, and the dehumidification in the second sub-step is carried out until the residual moisture content of the separated valuable material is no more than 30%.

13. The method according to any one of the preceding claims, characterized in that... The liquefaction medium used for liquefying valuable materials collected inside the at least one separation device (302, 304) is a mixture, suspension and / or filtrate of substances from the upstream portion of the device and / or prior process steps, particularly a conditioned mixture, suspension and / or filtrate of substances.

14. The method according to any one of the preceding claims, characterized in that... The liquefaction medium used for liquefying valuable materials collected inside the at least one separation device (302, 304) is an acid or alkali that is not derived from a mixture, suspension, and / or filtrate of substances from the upstream portion of the device and / or prior process steps.

15. The method according to any one of the preceding claims, characterized in that... During the liquefaction process, the (separated) valuable materials collected inside the at least one separation device (304) are subjected to a flow of liquefying medium from below in the direction of gravity, and are discharged in the direction of gravity above and / or above the feed channel (362) from their respective main spaces (352) and their respective filter elements (344).

16. The method according to any one of the preceding claims, characterized in that... The apparatus (100) for producing at least one of the products or valuable materials is configured according to any one of claims 6 to 10.

17. The method according to any one of the preceding claims, characterized in that... The method is used to produce solid valuable materials methionine and / or methionyl-methionine.

18. The method according to claim 17, characterized in that... The process involves at least two precipitation steps and at least two separation steps, wherein the precipitation step of the at least one valuable material, methionine, is performed before the at least two separation steps, and wherein at least one of the precipitation steps, particularly both precipitation steps, is a carbonation step, particularly carbonation using CO2.

19. The method according to any one of claims 17 or 18, characterized in that... The final separation step of the at least one valuable material, methionine, is carried out using an apparatus (100) according to any one of claims 1 to 9, the apparatus (100) comprising a separation device (304) configured as a membrane filter press (340), wherein after dehumidification, the membrane filter press (340) is emptied and / or regenerated by means of liquefaction of the filter cake, particularly by means of a closed membrane filter press (340), and wherein after the filter cake is liquefied, the liquefied medium carrying the valuable material is discharged via at least one internal discharge channel (378) of the membrane filter press (340).

Images