Discontinuously operating sublimator having at least one baffle

Abstract

The present invention relates to a discontinuously operating sublimator (1) for removing at least one gas component to be sublimated from a gas mixture flow, the sublimator comprising: a housing wall (7); an inlet (2) in the housing wall (7) for feeding the gas mixture flow entering the sublimator (1); an outlet (6) in the housing wall (7) for discharging the treated gas mixture flow from the sublimator (1); a sublimation zone (4) having temperature-controllable channel walls, the channel walls being temperature-controllable so that during a loading process, the at least one gas component to be sublimated sublimes on the channel walls, and during a subsequent melting process, the at least one gas component sublimated during the loading process melts on the channel walls; a gas inlet distribution chamber (3) located between the inlet (2) and the sublimation zone (4); and a gas outlet distribution chamber (5) located between the outlet (6) and the sublimation zone (4). According to the present invention, a flow disruptor (8) is located in the gas inlet distribution chamber (3) to uniformly distribute the gas mixture flow through the channel originating from the channel wall of the sublimation zone (4), and the geometric center of gravity of the flow disruptor is spaced (A) from the geometric center of gravity of the inlet face (9). T ) is in the range of 0.2×D to 10.0×D, preferably in the range of 0.5×D to 3.0×D, where D corresponds to the equivalent diameter of a circle having the same area as the inlet face (9), and the spacing (AT) is measured along the normal vector (nE) of the inlet face (9). The present invention also relates to a method for operating the sublimator (1) according to the present invention.

Description

[Technical Field]

[0001] The present invention provides a discontinuously operating sublimator for removing at least one gas component to be sublimated from a gas mixture flow, the sublimation zone having a housing wall, an inlet in the housing wall for supplying the gas mixture flow, an outlet in the housing wall for removing the treated gas mixture flow, and a temperature-controllable channel wall; The sublimator relates to a flow channel wall whose temperature is controllable so that during a loading process, at least one gas component to be sublimated sublimes on the flow channel wall, and during a subsequent melting process, at least one gas component sublimated in the loading process melts on the flow channel wall.

[0002] The sublimator further comprises a gas inlet distributor space between the inlet and the sublimation zone, and a gas outlet space between the outlet and the sublimation zone. [Background technology]

[0003] Known discontinuously operating sublimators have flow channel walls in their interior, which can take the form of a bundle of finned tubes. Finned tubes are characterized by the fact that the tubes are surrounded by fins that can be heated or cooled by the fluid flowing through the tubes. Thus, during the loading process, the gas components to be sublimated present in the gas or gas-vapor mixture are obtained by sublimating them on the cooled fins. In the subsequent melting process, the sublimated gas components are melted on the now heated walls of the finned tubes and discharged from the sublimator. Instead of finned tubes, other flow channel wall embodiments, such as lamellae or honeycombs, may also be arranged in the sublimator. When lamellae are used, the cooling or heating medium typically passes through fluid conduits generally arranged outside the housing wall, so that heat is essentially transferred between the outer fluid conduit and the housing wall, and between the housing wall and the lamellae.

[0004] In such above-mentioned sublimators, the gas mixture flow during the loading process has a less uniform distribution with respect to the flow through the channels, which means that the gas components to be sublimated sublimate unevenly on the channel walls. As a result, during the loading process, the pressure drop between the inlet and outlet of the sublimator increases more quickly, and therefore the sublimator must be regenerated at shorter time intervals, even though its maximum loading capacity has not yet been reached. The sublimator here is typically regenerated by a melting process and an optional subsequent re-cooling process.

[0005] Patent Document 1 discloses a discontinuously operating sublimator for separating products from a gas mixture, having internal lamellae as flow passage walls fixed to the lateral housing walls. A coolant or heat transfer medium passes through fluid conduits located only on the outside of the lateral housing walls. When heating the lamellae, heat is transferred from the fluid conduits to the lateral housing walls and from the lateral housing walls to the lamellae, while when cooling the lamellae, heat is transferred from the lamellae to the lateral housing walls and from the lateral housing walls to the fluid conduits. These sublimators are used, for example, in the production of phthalic anhydride (PA).

[0006] However, here there is a greater parasitic heat loss to the environment, since the sublimator is heated or cooled only from the outside. 3 For larger sublimators with an internal volume exceeding 1000 kJ / cm, the heat transfer between the side housing walls and the lamellae further away from the side housing walls during operation of the sublimator is generally too low, so that a temperature gradient within the lamellae is established during the loading process, which results in different rates of sublimation. As a result, there is a faster rise in pressure drop during the loading process, and therefore the sublimator must be regenerated at shorter time intervals, even though its maximum loading capacity has not yet been reached.

[0007] Patent document 2 discloses a cylindrically designed discontinuously operating sublimator for removing gas components to be sublimated from a gas stream. The sublimator comprises a housing with an internal fluid conduit and a lamella as a flow channel wall arranged on the inner surface of the housing wall and directed inwards. The lamella can also be cooled here by a coolant flowing through the internal fluid conduit or heated by a heat transfer medium flowing through the internal fluid conduit. However, it is difficult to know if such a sublimator is used for a long time, e.g., 1 m 3 , the heat transfer from the inner fluid conduit to the parts of the lamella further away from the fluid conduit is generally too low, so that a temperature gradient is established in the lamella, resulting in different rates of sublimation during the loading process. The longer designs of such sublimators have the disadvantage that sublimation occurs especially in parts of the lamella close to the inlet of the gas mixture flow. As a result, the lamella in the inlet area can become blocked quickly, even if sublimation does not occur on all of the walls of the lamella. As a result of the above-mentioned disadvantages, there is a faster rise in pressure drop during the loading process, and therefore the sublimator must be regenerated at shorter time intervals, even though its maximum loading capacity has not yet been reached. [Prior art documents] [Patent documents]

[0008] [Patent Document 1] DE 3407104 A1 [Patent Document 2] German Patent Application Publication No. 102015101398 Summary of the Invention [Problem to be solved by the invention]

[0009] The problem addressed was therefore to provide a sublimator that achieves maximum uniformity of distribution of the gas mixture flow through the flow passage of the sublimation zone during the loading process. A further problem addressed was to significantly slow down the increase in pressure drop between the inlet and outlet of the sublimator during the process of loading the sublimator, thus allowing for regeneration of the sublimator at longer time intervals. Another problem addressed was to provide a sublimator with a larger loading capacity for sublimating gas components at a given maximum pressure drop between the inlet and outlet of the sublimator or at a given maximum loading time for the loading process. [Means for solving the problem]

[0010] These problems are solved according to the invention by a discontinuously operating sublimator according to claim 1 and a method for operating a sublimator according to claim 17. Advantageous embodiments of the sublimator are given in claims 2 to 16.

[0011] The discontinuously operating sublimator of the present invention for removing at least one gas component to be sublimated from a gas mixture flow comprises a housing wall, an inlet in the housing wall for supplying the gas mixture flow to the sublimator, an outlet in the housing wall for removing the treated gas mixture flow from the sublimator, a sublimation zone having temperature-controllable flow channel walls, the temperature of which is controllable so that during a loading process, the at least one gas component to be sublimated sublimes at the flow channel wall, and during a subsequent melting process, the at least one gas component sublimated during the loading process melts at the flow channel wall, a gas inlet distributor space between the inlet and the sublimation zone, and a gas outlet space between the outlet and the sublimation zone.

[0012] According to the present invention, at least one first baffle arranged in the gas inlet distributor space for uniformly distributing the gas mixture flow through the channels originating from the channel walls in the sublimation zone has a geometric center of gravity whose distance from the geometric center of gravity of the inlet area is in the range of 0.2 x D to 10.0 x D, preferably in the range of 0.5 x D to 3.0 x D, where D corresponds to the equivalent diameter of a circle with an area equal to the inlet area, and the distance is measured along the normal vector of the inlet area.

[0013] In a preferred embodiment, the maximum possible distance between the geometric center of gravity of the first baffle and the geometric center of gravity of the inlet region is 0.7 × L, preferably 0.5 × L, particularly preferably 0.3 × L, where L corresponds to the length of the longitudinal axis of the gas inlet distributor space, and the distance is measured along the normal vector of the inlet region.

[0014] As a result, both the aforementioned range of 0.2 × D to 10.0 × D and the range of 0.5 × D to 3.0 × D specified above as preferred are limited to a maximum possible value of 0.3 × L if the distance from the geometric center of gravity of the first baffle to the geometric center of gravity of the inlet region is greater than 0.3 × L, where D corresponds to the equivalent diameter of a circle with an area equal to the inlet region, L corresponds to the length of the longitudinal axis of the gas inlet distributor space, and the distance is measured along the normal vector of the inlet region.

[0015] During the loading process, the first baffle or additional baffles in the gas inlet distributor space distribute the incoming gas mixture flow more uniformly through the individual channels in the sublimation zone, resulting in more uniform sublimation on the channel walls. The more uniform flow through the channels and the more uniform sublimation on the channel walls avoid excessive gas mixture flow velocities, some of which far exceed twice the average velocity of the gas mixture flow through the sublimation zone. Furthermore, the interaction between the channel walls and the gas mixture flow is enhanced.

[0016] Sublimation of at least one gas component to be sublimated results in coating of the surface of the channel walls, resulting in a corresponding increase in pressure drop across each channel during the loading process. A more uniform flow through the channels and more uniform sublimation on the channel walls has the effect of reducing the increase in pressure drop across each channel. Therefore, even during the loading process, the pressure drop between the inlet and outlet of the sublimator of the present invention is reduced, resulting in the sublimator being regenerated at much longer intervals. Furthermore, the sublimator of the present invention can sublimate more of the at least one gas component to be sublimated on its channel walls for the same pressure drop between the inlet and outlet of the sublimator compared to a sublimator without a baffle. Consequently, a sublimator of the present invention with at least one first baffle achieves a greater loading capacity for the same pressure drop.

[0017] In this specification, the expression "gas mixture flow" is generally understood to mean a flowing gas mixture. The gas mixture may also be a gas-vapor mixture. In principle, the gas mixture may contain liquid droplets or solid particles, provided that this does not result in damage or blockage of the sublimator.

[0018] In this specification, the expression "gas component to be sublimated" is generally understood to mean a gas component that sublimes mainly on the channel walls in the sublimation zone, said channel walls having a temperature lower than the sublimation temperature during the loading process. In thermodynamics, sublimation refers to the process of directly converting a substance from the gaseous state to the solid state of matter. The sublimation temperature indicates the maximum temperature at a given pressure at which a gas component changes into the solid state of matter.

[0019] In this specification, the expression "fluid conduit" is understood to mean a traversable conduit through which a coolant or heat transfer medium can flow. The fluid conduit may be arranged outside the housing wall and / or inside the sublimator. If one or more fluid conduits are arranged outside, heat is transferred between the fluid conduit and the housing wall, so that the temperature of the gas mixture flow in contact with the inside of the housing wall can be controlled. Furthermore, it is also possible here to control the temperature of the channel wall when the channel wall is thermally coupled to the inside of the housing wall. If one or more fluid conduits are arranged inside the sublimator, heat is generally transferred mainly between the fluid conduit and the channel wall, so that the temperature of the channel wall can be controlled.

[0020] In this specification, the expression "housing wall" is generally understood to mean the outer boundary of the sublimator. The housing wall is typically also referred to in the literature as a shell. The housing wall has sufficient technical integrity. Typically, the outside of the housing wall is at least partially heated by an external heating element. The external heating element typically takes the form of one or more fluid conduits, typically attached directly to the outside of the housing wall. In this case, during operation of the sublimator, a coolant or heat transfer medium is typically conveyed through the fluid conduits so that the gas mixture flow and / or the temperature of the channel walls can be correspondingly controlled. One or more inlet and outlet regions arise from respective cutouts in the housing wall.

[0021] In this document, the expression "sublimation zone with temperature-controllable channel walls" is generally understood to mean a zone in which, during the loading process, at least one gas component to be sublimated sublimes on the channel walls, while the remainder of the gas mixture flow, also called treated gas mixture flow, leaves the sublimation zone and thus reaches the gas outlet space. In a melting process downstream of the loading process, the channel walls of the sublimation zone are heated in order to melt the gas components sublimated on the channel walls and direct them out of the sublimator.

[0022] The temperature-controllable flow channel walls of the sublimation zone can be defined, for example, by the outer wall of a fin tube, a fin tube bundle, a tube bundle, a lamella body, a honeycomb body, several pipes, a bundle of several pipes, or a plate body. Lamella body, plate body, or honeycomb body is understood to mean the interior containing the corresponding lamella, plate, or honeycomb. When a lamella body is used, the cavities present between the individual lamellae form the flow channels. Correspondingly, the flow channel walls are defined by the lamella surfaces. When the flow channel walls are defined by fin tubes, each adjacent fin forms a cavity that functions as a flow channel through which a fluid, e.g., a gas mixture, can flow. Typically, a bundle of fin tubes is arranged in the sublimation zone, so that, for example, adjacent fin tubes can form additional flow channels, or individual fin tubes combined with corresponding adjacent fin tubes can form a continuous flow channel.

[0023] The flow paths may all have the same channel diameter, in that the fins of one or more fin tubes are spaced equally apart. Preferably, however, the flow paths have different channel diameters, in that the fins of one or more fin tubes are spaced at different intervals. For more uniform flow through the flow paths, it may be advantageous if the channel diameter at the inlet of each flow path is larger than the channel diameter at the outlet of each flow path. Furthermore, at least one gas component to be sublimated will more uniformly sublimate on the flow path wall over the length of each flow path. The tubular shape of the one or more fin tubes may be circular, elliptical, or rectangular.

[0024] Furthermore, the entrance area of ​​the sublimation zone is defined by a theoretical separation plane between the gas inlet distributor space and the sublimation zone, and the surface of each flow channel wall lying within the separation plane is also assigned to the entrance area of ​​the sublimation zone for simplicity.

[0025] The exit area of ​​the sublimation zone is defined by the theoretical separation plane between the gas outlet distributor space and the sublimation zone, and the surface of each channel wall lying within the separation plane is also assigned to the exit area of ​​the sublimation zone for simplicity.

[0026] The ratio of the entrance area of ​​the sublimation zone to the distance between the entrance area and the exit area of ​​the sublimation zone is preferably 5 [m 2 / m], and the ratio is 2 The calculation is performed using measurements of the entrance area in meters [m] and the distance between the entrance and exit areas of the sublimation zone in meters [m].

[0027] By adjusting the ratio to the preferred range, significant excessive sublimation on the channel walls in the area of ​​the entrance region of the sublimation zone is avoided, since increased sublimation on the channel walls would significantly reduce the minimum free gas passage area of ​​the channel in question within very short loading times, which would rapidly increase the pressure drop across the channel in question at the beginning of the loading process and ultimately block the channel in question after a very short loading time if sublimation on the channel walls in question were to take place essentially only in the area of ​​the entrance region of the sublimation zone.

[0028] The more inlet area is available, the less extent to which increased sublimation on the channel walls in the area of ​​the inlet area of ​​the sublimation zone can result in appreciably large pressure drops or even blockages.

[0029] In order to be able to design the sublimator in a cost-effective and space-saving manner, the ratio of the entrance area of ​​the sublimation zone to the distance between the entrance area and the exit area of ​​the sublimation zone is preferably less than 100 [m 2 / m] and the ratio is square meters [m 2 The calculation is performed using measurements made at the entrance area in meters [m], the entrance area in meters [m], and the distance between the entrance and exit areas of the sublimation zone in meters [m].

[0030] To control the temperature of the flow channel walls of the sublimation zone, for example, one or more traversable fluid conduits disposed within the sublimation zone can have a heat transfer medium or coolant flowing therethrough, thereby correspondingly controlling the temperature of the walls of the fluid conduits. Heat transfer between the flow channel walls and the traversable fluid conduits results in corresponding temperature control of the flow channel walls. Additionally or alternatively, temperature control can be achieved by one or more external traversable fluid conduits disposed outside the housing wall. In this case, heat transfer between the flow channel walls of the sublimation zone and the external traversable fluid conduits results in corresponding temperature control of the flow channel walls of the sublimation zone, with heat transfer naturally occurring via the intervening housing wall.

[0031] During the loading process, when a coolant flows through the inner or outer fluid conduit, the walls of the channel are cooled by heat conduction between the channel walls and the fluid conduit, so that at least one gas component to be sublimated can sublimate on the channel walls. During the melting process, when a heat transfer medium flows through the inner or outer fluid conduit, the walls of the channel are heated by heat conduction between the channel walls and the fluid conduit, so that the gas component that has sublimated on the channel walls can melt. The heat transfer medium or coolant used can, for example, be in each case a different or the same heat transfer oil, for example Diphyl DT.

[0032] As used herein, the term "sublimation on the channel walls" is generally understood to mean a deposition process in which at least one sublimation target gas component present in a gas mixture flow cools to such an extent that it sublimes and deposits on the channel walls. Accordingly, the sublimated gas component adheres to the channel walls in the solid state of matter.

[0033] According to given thermodynamic conditions, the term "sublimated" can also be understood herein as meaning that a phase change in at least a part of the gas mixture flow first occurs in the sublimation zone from the gaseous state of the object to the liquid state, and only thereafter from the liquid state to the solid state of the object. Correspondingly, the channel walls of the sublimation zone are at least partially wetted by the liquid formed by the phase change. As a result of the cooled channel walls, the phase change from the liquid state to the solid state of the object occurs at the channel walls within a very short time. In summary, also in this case, the gas component to be sublimated sublimes at the channel walls of the sublimation zone and correspondingly adheres to the channel walls in the solid state of the object.

[0034] In this specification, the expression "gas inlet distributor space" is generally understood to mean the space within the sublimator bounded by the sublimator housing wall, the sublimator inlet region, and the sublimation zone. During the loading process, the gas mixture flow flows through the gas inlet distributor space, and the gas mixture flow can enter through the sublimator inlet. The gas inlet distributor space is bounded by the sublimation zone with temperature-controllable channel walls, and the gas mixture flow can generally only exit the gas inlet distributor space through said sublimation zone.

[0035] In this document, the expression "gas outlet space" is generally understood to mean a space through which the gas mixture stream can be supplied from the adjacent sublimation zone, which space typically also has an outlet through which the treated gas mixture stream can exit the sublimator.

[0036] There is also generally a further outlet port equipped with an outlet valve, which may be, for example, a hermetically closed lid. During the melting process, the outlet valve is in an open state, which means that the produced melt can flow out of the sublimator. During the loading process, the outlet valve is in a closed state, which means that the fluid cannot flow out of the outlet port. Typically, this further outlet port is at the lowest point of the gas outlet space so that the melt can flow to the further outlet port as a result of gravity.

[0037] In this specification, the expression "discontinuously operating sublimator" is generally understood to mean a sublimator that generally operates discontinuously in two or three different process cycles. The first process cycle is a loading process in which at least one gas component to be sublimated sublimes on the channel walls of the sublimation zone. During the loading process, the channel walls are cooled. The second process cycle is a melting process in which the sublimated gas component is melted and removed from the sublimator by heating the channel walls of the sublimation zone.

[0038] The third process cycle is an optional re-cooling process in which the channel walls of the sublimation zone are cooled after the sublimated gas components are removed from the sublimator. Instead of a re-cooling process, channel wall cooling may also be performed only at the beginning of the loading process.

[0039] In this specification, the expression "distance along the longitudinal axis of the channel wall" is generally understood to mean that in a first calculation step, the distance between two points in three-dimensional space is ascertained so that a connection vector between the two points is calculated by forming the difference between the two points. Subsequently, in a second calculation step, a scalar product is formed using the already calculated connection vector and a vector extending parallel to the longitudinal axis of the channel wall, the magnitude of which is normalized to a value of 1. The magnitude of the scalar product thus calculated constitutes the distance along the longitudinal axis of the channel wall between the two points.

[0040] In this specification, the expression "distance along the normal vector" is generally understood to mean that in a first calculation step, the distance between two points in three-dimensional space is ascertained so that a connection vector between the two points is calculated by forming the difference between the two points. Subsequently, in a second calculation step, a scalar product is formed using the connection vector already calculated and the normal vector. The magnitude of the scalar product thus calculated constitutes the distance along the normal vector between the two points.

[0041] Thus, in an exemplary case, the distance between the geometric center of gravity of the baffle and the geometric center of gravity of the inlet region along the normal vector of the inlet region is ascertained in the following manner: In a first calculation step, a connection vector between the geometric center of gravity of the baffle and the geometric center of gravity of the inlet region is calculated by forming the difference between the two points. Subsequently, in a second calculation step, a scalar product is formed using the already calculated connection vector and the normal vector of the inlet region. The magnitude of the scalar product thus calculated constitutes the distance between the geometric center of gravity of the baffle and the geometric center of gravity of the inlet region along the normal vector of the inlet region.

[0042] If the normal vector of the inlet region does not essentially correspond to the main flow direction of the gas mixture flow entering the sublimator occurring during the loading process, a distance along the main flow direction is preferred.

[0043] In this specification, the expression "loading process" is generally understood to mean a process cycle during operation of the sublimator, in which the sublimator is operated until a predetermined loading of one or more sublimated gas components on the channel walls of the sublimation zone is achieved. Loading here should be considered to mean the deposited mass of one or more sublimated gas components on the channel walls.

[0044] As used herein, the term "loading capacity" is generally understood to mean the total mass of sublimed gas components that sublimes on the channel walls during the loading process before the pressure drop between the inlet and outlet of the sublimator exceeds a predetermined value and / or before a predetermined duration of loading time is achieved.

[0045] In this specification, the term "melting process" is generally understood to mean the process cycle during operation of the sublimator, in which the sublimator reaches its loading capacity, and the sublimated gas components subsequently melt as a result of heating of the channel walls and can exit the sublimator, for example, through an outlet port at the base of the sublimator. Generally, during the melting process, the gas mixture flow into the sublimator is stopped. Typically, the melting process is also referred to as a regeneration process.

[0046] In this specification, the term "re-cooling process" is generally understood to mean an optional process cycle during the operation of the sublimator, in which the channel walls of the sublimation zone are cooled after the sublimated gas components have been removed from the sublimator. A re-cooling process, typically combined with an upstream melting process, is also called a regeneration process.

[0047] In this specification, the term "baffle" is generally understood to mean a component that deflects the gas mixture flow entering from the inlet and distributes it in the gas inlet distributor space so that during the loading process, the gas mixture flows with a very uniform distribution through the flow path of the sublimation zone. In this context, the deflection of the gas mixture flow has the effect of, for example, a localized significant change in the magnitude and direction of the flow rate of the gas mixture flow.

[0048] In this document, the expression "surface area" is generally understood to mean the area facing the fluid and therefore subject to flow pressure in the direction of the surface.

[0049] In this specification, the expression "surface area of ​​the baffle projected onto the plane of the inlet region" is generally understood to mean the area that lies on the plane of the inlet region through the projection of the surface area of ​​the baffle. The inlet region is therefore a part of the plane. Furthermore, the projection is perpendicular to the plane of the inlet region.

[0050] In this specification, the expression "free gas passage area between the baffle and the sublimation zone" is generally understood to mean the area between the baffle and the sublimation zone through which fluid can flow unimpeded. In this context, the free gas passage area extends across the entire width of the sublimator, and the free gas passage area is bounded by the area between the baffle and the sublimation zone, and this boundary extends across the entire width of the free gas passage area.

[0051] In this specification, the expression "essentially rectangular design" is generally understood to mean a rectangular design that may also have rounded corners. Furthermore, the interior angle of each corner of the rectangle may vary by up to 10° from the ideal interior angle of 90°, provided that the sum of the interior angles of all corners is indeed 360°. Furthermore, the expression "essentially rectangular design" may also be understood to mean a regular or irregular polygon, in which case the corners of the polygon may also be rounded. Furthermore, the expression "essentially rectangular design" may also be understood to mean an oval or a rectangle with an arch disposed therein.

[0052] In this specification, the term "static mixer" is generally understood to mean a mixer having multiple elements at a specific angle to each other, for example, 90°, for example, multiple impingement plates. In principle, the mixer may comprise flat and / or curved elements. For example, a static mixer may consist of one or more crossbeam elements.

[0053] In a preferred configuration of the sublimator of the present invention, the sublimation zone is located between the gas inlet distributor space and the gas outlet space, such that the gas inlet distributor space is separated from the gas outlet space by the sublimation zone. The gas mixture may flow only through the flow path of the sublimation zone from the gas inlet distributor space to the gas outlet space, or in the case of counterflow, from the gas outlet space to the gas inlet distributor space.

[0054] This offers the advantage that there can be no bypass from the gas inlet distributor space to the gas outlet space, which would always ensure that the gas mixture flows through the sublimator during the loading process, but would require a controllable valve in the bypass, which itself could become blocked by at least one gas component to be sublimated during the loading process.

[0055] In a preferred configuration of the sublimator of the present invention, in the case of multiple baffles, the distance between the geometric centers of gravity of adjacent baffles is in the range of 0.01 × L to 0.5 × L, preferably in the range of 0.05 × L to 0.33 × L, where L corresponds to the length of the longitudinal axis of the gas inlet distributor space, and this distance is measured along the normal vector of the inlet area. This has the advantage that, in the case of multiple baffles, the gas mixture can flow more uniformly through the flow passages of the sublimation zone during the loading process.

[0056] In a further embodiment of the above-described preferred configuration of the sublimator of the present invention, the distance between adjacent baffles is equal, which has the advantage that during the loading process, in the case of multiple baffles, the gas mixture can flow more uniformly through the flow path of the sublimation zone.

[0057] In a preferred configuration of the sublimator of the present invention, the distance between the sublimation zone and the first baffle, or, if there are multiple baffles, each distance between the sublimation zone and each baffle, is at least 0.5 x D.

[0058] This provides the advantage that during the loading process, the gas mixture near each baffle can enter the flow path of the sublimation zone at less excessive velocity.

[0059] In a preferred configuration of the sublimator of the present invention, at least a first baffle has a width in the range of 1×D to a maximum width at which at least one baffle extends to two opposing housing walls of the sublimator, which provides the advantage of allowing a more uniform flow of the gas mixture through the flow passages of the sublimation zone over a wider area, or even over the entire width of the sublimation zone, during the loading process.

[0060] In a preferred configuration of the sublimator of the present invention, the at least first baffle is movable both before and during the loading process. In particular, the at least first baffle may also be tilted and movable. Alternatively, the at least first baffle may also be in a fixed position so that it cannot be moved during the loading process. This provides the advantage that during the loading process, the corresponding baffle can be adapted in terms of its alignment and / or its position depending on the given flow conditions.

[0061] In a preferred configuration of the sublimator of the present invention, at least a first baffle is heated during the loading process so that neither the gas component to be sublimated nor other fluids can sublimate on the baffle. In particular, at least a first baffle may have a double wall through an internal cavity through which a heat transfer medium can flow. This has the advantage that only a small amount, if any, of at least one gas component to be sublimated can sublimate on the corresponding baffle.

[0062] In a preferred configuration of the sublimator of the present invention, the sublimator has a horizontal longitudinal axis oriented perpendicular to the longitudinal axis of the flow path of the sublimation zone, and the gas inlet distributor space is located above the sublimation zone, in this connection the longitudinal axis of the flow path of the sublimation zone is preferably oriented parallel to the gravity vector.

[0063] This provides the advantage that during the loading process, the cooling of the gas mixture flow that takes place in the flow passages of the sublimation zone strengthens the gas mixture flow in the direction of the gas outlet space via the resulting convection effect.

[0064] In a preferred configuration of the sublimator of the present invention, at least the first baffle has a distance between the geometric center of gravity of the baffle and the geometric center of gravity of the inlet region in the range of 0 to 2.0 x D, preferably 0 to 0.5 x D, measured along the longitudinal axis of the flow path of the sublimation zone, with the geometric center of gravity of the first baffle preferably below the geometric center of gravity of the inlet region. This provides the advantage that the baffle can more uniformly distribute the gas mixture through the flow path of the sublimation zone during the loading process.

[0065] In a preferred configuration of the sublimator of the present invention, in the case of multiple baffles, each individual baffle downstream of the first baffle has a distance between its geometric center of gravity and the geometric center of gravity of the baffle immediately adjacent to it in the direction of the inlet, measured along the longitudinal axis of the flow path of the sublimation zone, in the range of 0 to 1.0 x D, preferably 0 to 0.5 x D. This has the advantage that during the loading process, the gas mixture can flow more uniformly through the flow path of the sublimation zone.

[0066] In a preferred configuration of the sublimator of the present invention, in the case of multiple baffles, baffles at a greater distance from the inlet region are positioned at a higher level than baffles at a shorter distance from the inlet region, the distance from the inlet region being measured along the normal vector of the inlet region.

[0067] This provides the advantage that the gas mixture can flow more uniformly through the flow passages of the sublimation zone during the loading process.

[0068] In a further configuration of the sublimator of the present invention, the geometric center of gravity of at least the first baffle is offset laterally in a horizontal plane from the geometric center of gravity of the inlet region. In this regard, for example, the height of the geometric center of gravity of the first baffle and the height of the geometric center of gravity of the inlet region may be the same.

[0069] This provides the advantage that, if a corresponding asymmetric gas flow exists in the gas inlet distributor space, the gas mixture can flow more uniformly through the flow passages of the sublimation zone during the loading process.

[0070] In a preferred configuration of the sublimator of the present invention, in the case of multiple baffles, the geometric center of the baffle furthest from the inlet region has a distance between its geometric center of gravity and the geometric center of gravity of the inlet region 9 in the range of 0 to 2.0 x D, preferably 0 to 1.0 x D, measured along the longitudinal axis of the flow path of the sublimation zone.

[0071] This provides the advantage that the gas mixture can flow more uniformly through the flow passages of the sublimation zone during the loading process.

[0072] In the above embodiments, when three or more baffles are present, the baffles are preferably arranged such that the respective distances between two adjacent baffles are equal, this distance being measured along the normal vector of the inlet region.

[0073] This provides the advantage that the gas mixture can flow more uniformly through the flow passages of the sublimation zone during the loading process.

[0074] In a preferred configuration of the sublimator of the present invention, the free gas passage area between the sublimation zone and the first baffle, or in the case of multiple baffles, between the sublimation zone and each baffle, is greater than 0.75, preferably greater than 1.0, relative to the inlet area. This has the advantage that during the loading process, the gas mixture near each baffle can enter the flow path of the sublimation zone without excessive velocity.

[0075] In a preferred configuration of the sublimator of the present invention, the surface area of ​​the first baffle, or, in the case of multiple baffles, the surface area of ​​each baffle, projected perpendicularly onto the plane of the inlet region, is greater than 1. This has the advantage that during the loading process, the gas mixture can flow more uniformly through the flow passages of the sublimation zone.

[0076] In a preferred configuration of the sublimator of the present invention, at least the first baffle has a ratio of its longest side to its shortest side in the range of 1 to 100, preferably in the range of 1 to 10. This has the advantage that during the loading process the gas mixture can flow more uniformly through the flow passages of the sublimation zone.

[0077] In a preferred configuration of the sublimator of the present invention, the first baffle, or in the case of multiple baffles, each baffle, is a static mixer or impingement plate, preferably having an essentially rectangular design, which has the advantage that the gas mixture can flow more uniformly through the flow passages of the sublimation zone during the loading process.

[0078] In a preferred configuration of the sublimator of the present invention, at least the first baffle takes the form of a static mixer composed of a plurality of crossbeam elements, each individual crossbeam element having two elements, and the at least first baffle is composed of at least two elements, preferably 4 to 16 elements, more preferably 6 elements, with adjacent elements disposed at an interior angle toward the inlet region relative to each other in the range of 60 to 120 degrees, preferably 85 to 95 degrees, more preferably 89 to 91 degrees. For example, the interior angle toward the inlet region may be 90 degrees.

[0079] Preferably, the above-mentioned interior angles between the respective elements may be varied before or during the loading process.

[0080] This provides the advantage that the gas mixture can flow more uniformly through the flow passages of the sublimation zone during the loading process.

[0081] In a preferred configuration of the sublimator of the present invention, at least the first baffle has a geometrically averaged normal vector over its surface facing the inlet, and the included angle formed by the geometrically averaged normal vector and the normal vector of the inlet region in the direction of exiting the sublimator is in the range of -60 degrees to 60 degrees, preferably in the range of -45 degrees to 45 degrees, and more preferably in the range of -15 degrees to 15 degrees.

[0082] In the particular case where the corresponding baffle is a static mixer, the static mixer may be composed of multiple cross beam elements. The geometrically averaged normal vector in this case corresponds to the angle bisector of the cross beam elements pointing towards the inlet region. Preferably, the aforementioned interior angle may be changed before or during the loading process. This has the advantage that the gas mixture can flow more uniformly through the flow path of the sublimation zone during the loading process.

[0083] In a preferred configuration of the sublimator of the present invention, the channel walls are defined by the outer walls of the tube bundles, fin tubes, fin tube bundles, lamellae, honeycomb and / or plate bodies, which provides the advantage that during the loading process, at least one gas component to be sublimated is efficiently sublimated on the channel walls of the sublimation zone, minimizing the pressure drop across the sublimation zone during the loading process.

[0084] In a preferred configuration of the sublimator of the present invention, the sublimator has a circular inlet area with a length of 7.240 m, a width of 2.850 m, a height of 4.560 m, and a diameter of 0.79 m. The sublimator is equipped with four static mixers as baffles. Each static mixer is composed of three crossbeam elements, each having two elements, and adjacent elements are arranged at an internal angle of 90 degrees facing the inlet area. Each crossbeam element has a length of 1.130 m, a width of 0.20 m, and a thickness of 0.005 m. The configuration of the individual elements therefore gives each static mixer a total width of 1.200 m. Each static mixer has a geometrically averaged normal vector across its surface facing the inlet. In this case, each geometrically averaged normal vector corresponds to the angle bisector of the crossbeam element facing the inlet area. Each static mixer has an interior angle formed by the geometrically averaged normal vector and the normal vector of the inlet region in the direction of exit from the sublimator. For all static mixers, the interior angle is 0 degrees. The geometric center of gravity of the first baffle is 1.36 m from the geometric center of gravity of the inlet region, measured along the normal vector of the inlet region.

[0085] The distance between the geometric centroids of adjacent baffles is 1.4 m, measured along the normal vector of the inlet region. Each of the baffles has a distance of 0.284 m between the sublimation zone and the respective baffle. The distance between the geometric centroid of each baffle and the geometric centroid of the inlet region is 0.000 m, measured along the longitudinal axis of the flow path of the sublimation zone.

[0086] The present invention further provides a method of operating the sublimator of the present invention.

[0087] In the method for operating the sublimator of the present invention, during the loading process, a gas mixture flow containing at least one gas component to be sublimated flows into the inlet at a mass flow rate of at least 0.01 kg / s at a temperature ranging from above the sublimation temperature of the at least one gas component to be sublimated at a given pressure to 300°C above the sublimation temperature at the given pressure, and at an absolute pressure ranging from 0.1 bar to 10.00 bar, preferably from 0.5 bar to 1.5 bar, and more preferably from 1.05 bar to 1.10 bar. The channel walls of the sublimation zone are cooled to a temperature ranging from 150°C below the sublimation temperature at the given pressure to 1°C below the sublimation temperature at the given pressure. The at least one gas component to be sublimated in the gas mixture flow is at least partially sublimated in the sublimator. Preferably, the at least one gas component to be sublimated is sublimated in a range of 10% to 100% by weight based on the at least one gas component to be sublimated in the gas mixture flow entering at the inlet. More preferably, the at least one component to be sublimated is sublimated in a range of 50% to 100% by weight based on the at least one gas component to be sublimated in the gas mixture flow entering at the inlet. When multiple gas components to be sublimated are present in the gas mixture flow, the above specified ranges relate to each gas component to be sublimated.

[0088] This provides the advantage that during the loading process, at least one gas component to be sublimated is efficiently sublimated on the channel walls of the sublimation zone, minimizing the pressure drop across the sublimation zone during the loading process. Additionally, the gas mixture also flows more uniformly through the channels of the sublimation zone.

[0089] In a preferred configuration of the method for operating the sublimator of the present invention, the pressure drop between the inlet and outlet of the sublimator during the loading process is 80 mbar or less, preferably 40 mbar or less, and more preferably 20 mbar or less. This has the advantage that the pressure drop is not too large when the loading process is operated at maximum loading. If the pressure drop becomes too large, the mass flow rate of the gas mixture flow at the inlet may decrease. In this case, an auxiliary pump may be used to achieve the desired mass flow rate of the gas mixture flow at the inlet. However, this carries the risk that the pump may become blocked by at least one gas component to be sublimated during operation and therefore have to be stopped.

[0090] In a preferred configuration of the method of the present invention for operating the sublimator of the present invention, the pressure drop during the loading process caused by the first baffle, or in the case of multiple baffles, by all the baffles present, is less than 0.1, preferably less than 0.01, relative to the pressure drop occurring between the inlet and outlet of the sublimator. This has the advantage that the baffles do not significantly contribute to the pressure drop occurring between the inlet and outlet of the sublimator. Therefore, the pressure drop across the baffles is small and can be neglected.

[0091] In a preferred configuration of the method of the invention for operating the sublimator of the invention, after achieving a predetermined loading of at least one sublimated gas component onto the walls of the channels of the sublimator or after achieving a predetermined loading time, a melting process is carried out, which comprises the following steps: - stopping the flow of the gas mixture into the sublimator; heating the channel walls of the sublimation zone to a temperature in the range from the sublimation temperature of at least one gas component to be sublimated at a given pressure to a temperature 300° C. higher than the sublimation temperature at the given pressure; melting at least one sublimated gas component in a sublimator to obtain a melt; and Removing the melt from the sublimator, preferably via an outlet port in the housing wall of the gas outlet space.

[0092] This has the advantage that the melting process proceeds efficiently, for example, sublimated gas components do not have to be scraped off the channel walls of the sublimation zone.

[0093] In a preferred configuration of the method for operating the sublimator of the present invention, after the melt has been removed from the sublimator, a re-cooling process is carried out in which the walls of the channels of the sublimation zone are cooled to a temperature ranging from 150° C. below the sublimation temperature at a given pressure to 1° C. below the sublimation temperature at a given pressure. This provides the advantage that the channels of the sublimation zone are already at the temperature required for sublimation before the loading process. Thus, at the start of the loading process, at least one gas component to be sublimated is efficiently removed from the gas mixture stream.

[0094] In a preferred configuration of the inventive method for operating the inventive sublimator, the at least one gas component to be sublimated comprises, in its mass fraction, mainly, and preferably exclusively, phthalic anhydride.

[0095] In a preferred configuration of the inventive method for operating the inventive sublimator, the concentration of at least one gas component to be sublimated in the gas mixture flow at the inlet is in the range of 0.001% to 50% by weight, preferably in the range of 0.1% to 10% by weight.

[0096] This provides the advantage that at least one gas component to be sublimated is efficiently removed from the gas mixture stream.

[0097] The invention will be discussed in more detail below with reference to the drawings, which should be considered as schematic representations and which do not constitute limitations of the invention, for example with respect to specific dimensions or design variations. [Brief explanation of the drawings]

[0098] [Figure 1] 1 is a longitudinal cross-sectional view of a first exemplary embodiment of a sublimator of the present invention; FIG. [Figure 2] 2 is a cross-sectional view of a first exemplary embodiment of the sublimator of the present invention according to FIG. 1; [Figure 3] 2 is a cross-sectional view of a first exemplary embodiment of the sublimator of the present invention according to FIG. 1, showing not only the inlet area but also the surface area and free gas passage area of ​​the baffle projected onto a plane. [Figure 4] FIG. 2 is a longitudinal cross-sectional view of a second exemplary embodiment of a sublimator of the present invention. [Figure 5] FIG. 10 is a longitudinal cross-sectional view of a third exemplary embodiment of a sublimator of the present invention. [Figure 6] FIG. 1 is a diagram of a first exemplary embodiment of a baffle of the present invention having a rectangular flat design. [Figure 7] FIG. 10 is a diagram of a second exemplary embodiment of a baffle of the present invention having a rectangular curved design. [Figure 8] FIG. 10 is a diagram of a third exemplary embodiment of a baffle of the present invention having a rectangular curved design, the design having holes. [Figure 9] FIG. 10 is a diagram of a fourth exemplary embodiment of the baffles of the present invention, wherein at least a first baffle is a static mixer. [Figure 10] FIG. 10 is a perspective view of a fourth exemplary embodiment of the sublimator of the present invention, with four static mixers as each baffle. [Figure 11] 1 is a perspective view of a first comparative example of a sublimator without baffles, showing the velocity of the gas mixture flow in the direction of the longitudinal axis of the flow passage in the indicated region at the beginning of the loading process, the region shown here being at the top of the sublimation zone. [Figure 12] 10 is a perspective view of a fifth exemplary embodiment of the sublimator of the present invention having a static mixer as a baffle of the present invention, showing the velocity of the gas mixture flow in the direction of the longitudinal axis of the flow passage in the indicated region at the beginning of the loading process, the region shown here being at the top of the sublimation zone. [Figure 13]12 is a vector plot of the velocity of the gas mixture flow at the beginning of the loading process in the sublimator without baffles according to FIG. 11, showing the vector plot at a cross section of the longitudinal sublimator section. [Figure 14] 13 is a vector plot of the velocity of the gas mixture flow at the beginning of the loading process in the fifth exemplary embodiment of the sublimator of the present invention having a static mixer as a baffle of the present invention according to FIG. 12, showing the vector plot in the cross section of the longitudinal sublimator section. [Figure 15] 10 is a perspective view of a sixth exemplary embodiment of the sublimator of the present invention having a static mixer as a baffle of the present invention, showing the velocity of the gas mixture flow in the direction of the longitudinal axis of the flow passage in the indicated region at the beginning of the loading process, the region shown here being at the top of the sublimation zone. [Figure 16] 10 is a perspective view of a seventh exemplary embodiment of the sublimator of the present invention having a static mixer as a baffle of the present invention, showing the velocity of the gas mixture flow in the direction of the longitudinal axis of the flow passage in the indicated region at the beginning of the loading process, the region shown here being at the top of the sublimation zone. [Figure 17] 10 is a perspective view of an eighth exemplary embodiment of the sublimator of the present invention having a static mixer as a baffle of the present invention, showing the velocity of the gas mixture flow in the direction of the longitudinal axis of the flow passage in the indicated region at the beginning of the loading process, the region shown here being at the top of the sublimation zone. [Figure 18] 10 is a perspective view of a ninth exemplary embodiment of the sublimator of the present invention having a static mixer as a baffle of the present invention, showing the velocity of the gas mixture flow in the direction of the longitudinal axis of the flow passage in the indicated region at the beginning of the loading process, the region shown here being at the top of the sublimation zone. [Figure 19] 1 is a perspective view of a second comparative example of a sublimator without baffles, showing the velocity of the gas mixture flow in the direction of the longitudinal axis of the flow passage in the indicated region at the beginning of the loading process, the region shown here being at the top of the sublimation zone. DETAILED DESCRIPTION OF THE INVENTION

[0099] FIG. 1 shows a longitudinal cross-section of a first exemplary embodiment of a sublimator 1 of the present invention having a length L, with the gravity vector g indicated by the arrow at the bottom right of FIG. 1 and the xy coordinate system indicated by the arrow at the bottom left of FIG. 1.

[0100] The sublimator 1 has a horizontal longitudinal axis perpendicular to the longitudinal axis of the flow path of the sublimator zone 4. The sublimator 1 has an inlet 2 with an inlet port 10, through which a gas mixture flow containing at least one gas component to be sublimated enters the gas inlet distributor space 3 of the sublimator 1 during the loading process. For this purpose, an inlet region 9 is provided correspondingly in the housing wall 7, which serves as the outer boundary of the sublimator 1. The sublimator zone 4, with its temperature-controllable flow path wall, separates the gas inlet distributor space 3 from the gas outlet space 5. The sublimator zone 4 is connected to the gas inlet distributor space 3 so that the gas mixture flow can flow from the gas inlet distributor space 3 to the sublimator zone 4 during the loading process. Furthermore, the sublimator zone 4 is connected to the gas outlet space 5 so that the gas mixture flow can flow from the sublimator zone 4 to the gas outlet space 5 during the loading process. An outlet 6 is arranged in the gas outlet space 5 so that the gas mixture flow can exit the sublimator 1 during the loading process. For this purpose, an outlet area 12 is provided corresponding to the housing wall 7 and outlet ports 11 are arranged around the outlet area 12 .

[0101] The sublimation zone 4 is preferably 1 m 3 ~100m 3 The volume is in the range of

[0102] In order to make the gas mixture flow more uniformly through the channels during the loading process, baffles 8 are arranged in the gas inlet distributor space 3. In this regard, the gas mixture should flow through the maximum part of the total area of ​​all channel walls of the sublimation zone 4 so that the gas mixture flows in the direction from the gas inlet distributor space 3 to the gas outlet space 5.

[0103] This provides the maximum area for sublimation.

[0104] To prevent rapid blockage of individual channels, the maximum flow velocity through the channels in the sublimation zone 4 should be as close as possible to the average velocity through the channels. Furthermore, reverse flow of the treated gas mixture from the gas outlet space 5 towards the gas inlet distributor space 3 should also be avoided as much as possible, so that a large pressure drop across the sublimation zone 4 can be avoided.

[0105] The baffle of the present invention in this example is an impingement plate. The geometric center of gravity of the baffle 8 is a distance A from the geometric center of gravity of the inlet region 9. T is in the range of 0.5 × D to 3.0 × D, where D corresponds to the equivalent diameter of a circle with an area equal to the inlet area 9, and the distance A T is the normal vector n of the inlet region 9 E It is measured along the

[0106] Furthermore, there is also a further outlet port 17 equipped with an outflow valve, which may be, for example, a hermetically closed lid. During the loading process, the outflow valve is in a closed state, which means that the gas mixture cannot flow out of the further outlet port 17. However, during the melting process, the outflow valve is in an open state, which means that the produced melt can flow out of the sublimator. Typically, this further outlet port 17 is at the lowest point of the gas outlet space so that the melt can flow to the further outlet port 17 as a result of gravity.

[0107] Figure 2 shows a cross-sectional view of a first exemplary embodiment of the sublimator 1 of the present invention according to Figure 1, the sublimator 1 having a height H and a width B. Figure 2 shows the zy coordinate system at the bottom left. In the cross-sectional view, the housing wall 7, the gas inlet distributor space 3, the sublimation zone 4, the gas outlet space 5, the outlet region 12, and the inlet region 9 with a diameter D are shown. In this context, the rectangular boundary frame 20 of the baffle 8 is shown with a dotted line. The rectangular boundary frame is defined by the dimensions of the baffle 8 projected perpendicularly onto the plane of the inlet region.

[0108] Figure 3 shows further details regarding Figure 2. In Figure 3, the rectangular boundary frame 20 of the inlet region 9 and the baffle 8 is again shown in dotted lines on the left side. In the center of the drawing, the surface area 13 of the baffle 8 projected onto the plane of the inlet region 9 is shown in the background, and the inlet region 9 is shown in the foreground. On the right side of the drawing, the free gas passage area 14 between the boundary frame 20 of the baffle 8 and the sublimation zone 4 is shown.

[0109] FIG. 4 shows a second exemplary embodiment of the sublimator 1 of the present invention, in which, compared to the first embodiment of the sublimator 1 of the present invention, an additional impingement plate as a second baffle 18 and an additional impingement plate as a third baffle 19 are arranged in the gas inlet distributor space 3.

[0110] where A T1 is the distance between the geometric center of gravity of the second baffle 18 and the geometric center of gravity of the first baffle 8, and A T2 is the distance between the geometric center of gravity of the third baffle 19 and the geometric center of gravity of the second baffle 18, and these distances are respectively determined by the normal vector n E It is measured along the

[0111] A S2 is the distance between the second baffle and the sublimation zone 4, and A S3 is the distance between the third baffle and sublimation zone 4, each of these distances being measured along the longitudinal axis of the flow path of sublimation zone 4.

[0112] 5 shows a third exemplary embodiment of the sublimator 1 of the present invention, in which, compared to the second embodiment of the sublimator 1 of the present invention, the second baffle 18 and the third baffle 19 are arranged at different heights. In this regard, the rectangular boundary frame 20 of the baffle 8 is shown by a dashed line, the geometric centers of gravity of the individual baffles 8, 18, 19 are shown by circles, and the connecting lines between the geometric centers of gravity of the individual baffles 8, 18, 19 are shown by dotted lines. The horizontal longitudinal axis of the sublimator 1 is shown by a dashed line and passes through the geometric center of gravity of the inlet region 9.

[0113] where A T、max is the distance between the geometric center of gravity of the furthest removed baffle 19 and the geometric center of gravity of the inlet region 9, and the distance A T、max is the normal vector n of the inlet region 9 E It is measured along the

[0114] A H1 is the distance between the geometric center of gravity of the first baffle 8 and the geometric center of gravity of the inlet region 9, and A H2 is the distance between the geometric center of gravity of the second baffle 18 and the geometric center of gravity of the first baffle 8, and A H3 is the distance between the geometric center of gravity of the second baffle 18 and the geometric center of gravity of the third baffle 19, and A H、max is the maximum distance A from the entrance area 9 T、max and the geometric center of gravity of the inlet region 9, and the individual distances A H、max , A H1 , A H2 , A H3 are each measured along the longitudinal axis of the flow channel in sublimation zone 4.

[0115] Figure 6 shows a first exemplary embodiment of a baffle 8 of the invention, with an impingement plate 15 in the form of a rectangular flat design. On the left side of the figure, the height of the baffle is S H and the length of the baffle is S L In the center of the figure, the geometrically averaged normal vector n of the surface of the baffle 8 facing the inlet 2 is A , and the normal vector n of the inlet region 9 facing in the negative direction E Furthermore, an angle α1 is presented, which is the angle of the negative normal vector n E and the geometrically averaged normal vector n A In this context, the geometrically averaged normal vector n A is determined by the geometric mean of the normal vectors of its surface facing the inlet 2. On the right side of the figure, the inlet 2, the inlet region 9 and the inlet port 10 are shown.

[0116] Figure 7 shows a second exemplary embodiment of a baffle 8 of the invention with an impingement plate 15 in the form of a rectangular curved or flat design. On the left side of the figure, the height of the baffle is S H The length of the baffle 8 is S L On the right side of the figure, a flat embodiment of the baffle 8 and two exemplary embodiments with possible curvatures in the baffle 8 are shown.

[0117] Figure 8 shows a third exemplary embodiment of a baffle 8 of the present invention, with an impingement plate 15 in the form of a rectangular curved or flat design, the baffle 8 having circular holes through which the material can flow. On the left side of the figure, the height of the baffle is shown as S H The length of the baffle 8 is S L On the right side of the figure, a flat embodiment of the baffle 8 and two exemplary embodiments with possible curvatures of the baffle 8 are shown. In principle, all hole shapes can be used, for example circular, elliptical or angular hole shapes.

[0118] In particular, the impingement plate may have multiple holes through which the material can flow. All of the holes through which the material can flow may have a circular or elliptical shape. A mixture of circular and elliptical holes is also possible.

[0119] FIG. 9 shows a fourth exemplary embodiment of a baffle 8 of the present invention, which is a static mixer. On the left side of the figure, black rectangles with arrows inside them indicate a specific orientation of each element 16 of the mixer, and white rectangles with arrows inside them indicate another specific orientation of each element 16 of the mixer. In the center of the figure, a cross section of the mixer is shown, revealing two adjacent elements 16 of the mixer. The black elements 16 correspond to the black rectangles on the left side of the figure, and the white elements 16 correspond to the white rectangles on the left side of the figure. Furthermore, the geometrically averaged normal vector n of the surface of the baffle 8 facing the inlet 2 is A , and the normal vector n of the inlet region 9 facing in the negative direction EFurthermore, two angles α1 and α2 are presented, where the angle α1 is the angle between the normal vector n of the inlet region 9 in the direction of exiting the sublimator 1. E and the geometrically averaged normal vector n A and angle α2 denotes the interior angle between two adjacent elements 16 facing towards the inlet region 9. On the right side of the figure, the inlet 2, the inlet region 9 and the inlet port 10 are shown.

[0120] FIG. 10 shows a perspective view of a fourth exemplary embodiment of the sublimator 1 of the present invention, in which the sublimator 1 has a length L of 7.240 m, a width B of 2.850 m, a height H of 4.560 m, and a circular inlet area 9 with a diameter of 0.79 m, and is equipped with four static mixers 8, 18, 19, 21 as baffles.

[0121] 9, in FIG. 10, each static mixer 8, 18, 19, 21 is constructed from three cross beam elements, each individual cross beam element having two elements 16, with adjacent elements 16 arranged at an interior angle α2 facing the inlet region 9 of 90 degrees. Each element 16 of the cross beam has a length of 1.130 m, a width of 0.20 m, and a thickness of 0.005 m. The configuration of the individual elements 16 therefore gives each static mixer 8, 18, 19, 21 an overall width of 1.200 m. Each static mixer 8, 18, 19, 21 is oriented along a normal vector n geometrically averaged over its surface facing the inlet region 9. A Each of the geometrically averaged normal vectors in this case corresponds to the angle bisector of the cross beam element pointing towards the inlet region. Each static mixer 8, 18, 19, 21 has a geometrically averaged normal vector n A and the normal vector n of the inlet region 9 in the direction of exiting the sublimator 1. E 10, the geometric center of gravity of the first baffle 8 is at a distance A of 1.36 m from the geometric center of gravity of the inlet region 9. T at a distance A Tis the normal vector n of the inlet region 9 E It is measured along the

[0122] According to FIG. 4, in FIG. 10, the distances A between the geometric centers of gravity of adjacent baffles (8, 18), (18, 19), and (19, 21) are T1 , A T2 , A T3 is 1.4m, and the distance A T1 , A T2 , A T3 is the normal vector n of the inlet region 9 E 4, in FIG. 10, the baffles 8, 18, 19, 21 present are each measured along the distance A between the sublimation zone 4 and the respective baffle 8, 18, 19, 21. S1 , A S2 , A S3 , A S4 5, the distance A between the geometric center of gravity of each baffle 8, 18, 19, 21 and the geometric center of gravity of the inlet region 9 is 0.284 m. H1 , A H2 , A H3 , A H4 is 0.000m, and the distance A H1 , A H2 , A H3 , A H4 is measured along the longitudinal axis of the flow channel in the sublimation zone 4.

[0123] Example The example sublimator loading process described below is modeled using a numerical flow mechanics simulation, often referred to as "Computational fluid dynamics" (CFD).

[0124] For this purpose, the ANSYS Fluent software is used, which can be found on the web page https: / / www.ansys.com / de-de / products / fluids / ansys-fluent (retrieved 25 August 2022). ANSYS Fluent is a wide-ranging simulation software package used for modelling, simulating and optimising flow-related processes, plants and components in industry.

[0125] The simulations in the following examples are based on steady-state simulations using the RANS turbulence model. Standard settings of the Fluent Solver, version 22.1, are used here.

[0126] Example 1 A thermodynamic simulation of an inventive embodiment of a method for operating an inventive sublimator 1 according to FIG. 1 was carried out in Fluent.

[0127] The length L of the sublimator 1 is 7.24 m, the width B of the sublimator 1 is 2.85 m, the height H of the sublimator 1 is 4.56 m, the diameter D of the circular inlet area 9 is 0.79 m, the diameter of the circular outlet area 12 is 0.79 m, and the internal volume of the gas inlet distributor space is 23.8 m 3 The internal volume of the gas outlet space is 24.9 m 3 is.

[0128] The ratio of the entrance area of ​​the sublimation zone 4 to the distance between the entrance area and the exit area of ​​the sublimation zone 4 is 13.1 [m 2 / m].

[0129] Sublimation Zone 4 is 32.58m 3 The surface area of ​​all the channel walls in the sublimation zone 4 is 5000 m 2 Therefore, 5000m 2 of cooling area is available for the loading process and 5000m 2 is available for the melting process.

[0130] However, for the purposes of computational power, the fin tubes are simplified in the simulation so that the porous zone models a four-fin tube bundle. Thus, the pressure drop across the flow path in sublimation zone 4 is efficiently calculated. The porous zone is described in detail in Chapter 6.2.3 of the ANSYS Fluent User's Guide, February 17, 2016, available from ANSYS, Inc. at its website, https: / / www.ansys.com / . Furthermore, such a porous zone is also shown on page 44 of the website "Computational Fluid Dynamics (CFD) of Chemical Processes - Google Books" (retrieved September 5, 2022).

[0131] In this regard, the flow directions of the gas mixture stream within the flow passage that may vary from the longitudinal axis of the flow passage are at least primarily aligned by the corresponding pressure drop so that these flow directions also point in the direction of the longitudinal axis of the flow passage.

[0132] The baffle 8 of the present invention is designed in the following embodiment.

[0133] The baffle 8 of the present invention is constructed from three cross beam elements, each having two elements 16, with adjacent elements 16 being arranged at an interior angle α2 facing the inlet region 9 of 90 degrees relative to each other. Each element 16 of the cross beam has a length of 0.710 m, a width of 0.200 m, and a thickness of 0.005 m. The configuration of the individual elements 16 therefore provides the static mixer with an overall width of 1.200 m.

[0134] The baffle 8 is geometrically averaged over its surface facing the inlet 2 by a normal vector n A The geometrically averaged normal vector in this case corresponds to the angle bisector of the cross beam element pointing towards the inlet region.

[0135] Geometrically averaged normal vector n A and the normal vector n of the inlet region 9 in the direction of exiting the sublimator 1. E The resulting interior angle α1 is 0 degrees.

[0136] The geometric center of gravity of the baffle 8 is 1.050 m from the geometric center of gravity of the inlet area 9. T at a distance A T is the normal vector n of the inlet region 9 E It is measured along the

[0137] The resulting distance A between the baffle 8 and the sublimation zone 4 S1 is 0.460 m, and the distance A between the geometric center of gravity of the inlet region 9 and the geometric center of gravity of the baffle 8 H1 is 0.000m, and distance A H1 is measured along the longitudinal axis of the flow channel in the sublimation zone 4.

[0138] The simulation gives the following results: A gas mixture stream is fed to the sublimator 1 via the inlet 2 at a mass flow rate of 150 t / h, an absolute pressure of 1.086 bar and a temperature of 178°C. The mass flow rate of the gas mixture stream here contains PA as the gas component to be sublimated in a concentration of 8 wt%. Under these thermodynamic conditions, the density of the gas mixture stream is 4.4 kg / m 3 and the kinematic viscosity of the gas mixture flow is 2.5 × 10 -5 Pa x s. The housing wall is at a temperature of 178°C.

[0139] The pressure drop caused by the baffle 8 is of the order of magnitude of 1 mbar. The pressure drop between the inlet 2 and the outlet 6 of the sublimator 1 is 17 mbar.

[0140] The uniformity achieved in the distribution of the gas mixture flow through the flow channel is evaluated using the following results described from the flow simulation:

[0141] Sublimation Zone 4 is 9.8m 2is contacted from the gas inlet distributor space 3 over a surface area of ​​1000 nm, which surface area corresponds to the top surface of the sublimation zone 4 according to Figure 12. In the remaining part of the surface area, a counterflow occurs. The maximum velocity of the gas mixture flow through the sublimation zone 4 is 7.6 m / s, and the average velocity of the gas mixture flow through the sublimation zone 4 is 0.46 m / s.

[0142] The surface area of ​​the sublimation zone 4 is shown in FIG. 12, which shows the velocity of the gas mixture flow in the direction of the longitudinal axis of the channel at the start of the loading process, the surface area being at the top of the sublimation zone 4.

[0143] Sublimation on the channel walls of the sublimation zone 4 occurs at the beginning of the loading process mainly in the area opposite the inlet region 9. Later, during the loading process, the sublimation sites move towards the inlet region 9.

[0144] Velocities with velocity vectors oriented in the direction of the main flow direction of the gas mixture flow through the flow passage of the sublimation zone 4 are shown in black if the magnitude of the velocity is 10 m / s or greater. Velocities with velocity vectors oriented in the direction opposite to the main flow direction of the gas mixture flow through the flow passage of the sublimation zone 4 are shown in white if the magnitude of the velocity is greater than 0 m / s.

[0145] As is clear from a comparison of Figures 11 and 12, in the case of the sublimator 1 of the present invention, the gas mixture flows through a larger area of ​​the sublimation zone 4 in the direction of the gas outlet space 5. Furthermore, the effect of the baffle 8 of the present invention is that the rear area of ​​the gas inlet distributor space 3 in the main flow direction exhibits a velocity direction across the entire width B of the sublimator 1 oriented in the direction of the gas outlet space 5. This avoids high velocities in the channels of the sublimation zone 4 and accordingly reduces the pressure drop across the sublimation zone 4. High flows through individual channels can lead to their rapid blockage. In extreme cases, the effect can even be such that sublimation only partially occurs at the channel walls due to the high velocity of the gas mixture flow. The baffle 8 reduces the excessive velocities and backflows caused by them in adjacent channels, thereby avoiding or at least partially avoiding the aforementioned effects.

[0146] A vector plot of the velocity vectors of the gas mixture flow at the beginning of the loading process in the sublimator 1 of the present invention is shown in Figure 14, which shows a vector plot at a cross section of a longitudinal sublimation section, where the length of the vector is constant and therefore independent of the magnitude of the velocity.

[0147] It can be seen that in the area essentially to the left of the sublimation zone 4, indicated by the rectangular box, the gas mixture flows through the sublimation zone 4 in the direction of the gas outlet space 5. The diagonal dashed line within the sublimation zone 4 indicates the switch point where the velocity direction through the flow passages of the sublimation zone 4 switches to the opposite direction. The greater the drop within the dashed line, the less the gas mixture flows through the flow passages of the sublimation zone 4 in the direction of the gas outlet space 5. In the area to the right of the diagonal dashed line, the gas mixture flows from the gas outlet space 5 through the flow passages of the sublimation zone 4 in the direction of the gas inlet distributor space 3.

[0148] 13 and 14, in the case of the sublimator 1 of the present invention, the gas mixture flows through a larger area of ​​the sublimation zone 4 in the direction of the gas outlet space 5. This reduces the higher velocities in the flow path of the sublimation zone 4, resulting in a correspondingly smaller pressure drop across the sublimation zone 4 during the loading process. Furthermore, backflow from the gas outlet space 5 to the gas inlet distributor space 3 is also reduced.

[0149] Excessive flow through the individual channels can also lead to their rapid blockage. In extreme cases, the effect can even be that the gas mixture flow velocity is so high that only partial sublimation occurs on the channel walls. The baffle 8 reduces the excessive velocity, so that the aforementioned effect can be avoided, or at least partially avoided.

[0150] Example 2 A thermodynamic simulation of an embodiment of the method of operating the sublimator 1 of the invention according to Figure 1 was carried out in Fluent. The only difference between this Example 2 and Example 1 is the spacing A of the baffles 8. T In this second embodiment, the interval A T is equal to 0.395.

[0151] The surface area of ​​the sublimation zone 4 is shown in FIG. 15, which shows the velocity of the gas mixture flow in the direction of the longitudinal axis of the channel at the start of the loading process, the surface area being at the top of the sublimation zone 4.

[0152] Sublimation on the channel walls of the sublimation zone 4 occurs at the beginning of the loading process mainly in the area opposite the inlet region 9. Later, during the loading process, the sublimation sites move towards the inlet region 9.

[0153] Velocities with velocity vectors oriented in the direction of the main flow direction of the gas mixture flow through the flow passage of the sublimation zone 4 are shown in black if the magnitude of the velocity is 10 m / s or greater. Velocities with velocity vectors oriented in the direction opposite to the main flow direction of the gas mixture flow through the flow passage of the sublimation zone 4 are shown in white if the magnitude of the velocity is greater than 0 m / s.

[0154] As is clear from a comparison of Figures 11 and 15, in the case of the sublimator 1 of the present invention, the gas mixture flows through a larger area of ​​the sublimation zone 4 in the direction of the gas outlet space 5. Furthermore, the effect of the baffle 8 of the present invention is that the rear area of ​​the gas inlet distributor space 3 in the main flow direction exhibits a velocity direction across the entire width B of the sublimator 1 oriented in the direction of the gas outlet space 5. This avoids high velocities in the channels of the sublimation zone 4 and accordingly reduces the pressure drop across the sublimation zone 4. High flows through individual channels can lead to their rapid blockage. In extreme cases, the effect can even be such that sublimation only partially occurs at the channel walls due to the high velocity of the gas mixture flow. The baffle 8 reduces the excessive velocities and backflows caused by them in adjacent channels, thereby avoiding or at least partially avoiding the aforementioned effects.

[0155] Example 3 A thermodynamic simulation of an embodiment of the method of operating the sublimator 1 of the invention according to Figure 1 was carried out in Fluent. The only difference between this example 3 and example 1 is the spacing A of the baffles 8. T In this Example 3, Separation A T is equal to 2.37.

[0156] The surface area of ​​the sublimation zone 4 is shown in FIG. 16, which shows the velocity of the gas mixture flow in the direction of the longitudinal axis of the channel at the start of the loading process, the surface area being at the top of the sublimation zone 4.

[0157] Sublimation on the channel walls of the sublimation zone 4 occurs at the beginning of the loading process mainly in the area opposite the inlet region 9. Later, during the loading process, the sublimation sites move towards the inlet region 9.

[0158] Velocities with velocity vectors oriented in the direction of the main flow direction of the gas mixture flow through the flow passage of the sublimation zone 4 are shown in black if the magnitude of the velocity is 10 m / s or greater. Velocities with velocity vectors oriented in the direction opposite to the main flow direction of the gas mixture flow through the flow passage of the sublimation zone 4 are shown in white if the magnitude of the velocity is greater than 0 m / s.

[0159] As is clear from a comparison of Figures 11 and 16, the rear area of ​​the gas inlet distributor space 3 in the main flow direction shows a velocity direction across the entire width B of the sublimator 1, oriented in the direction of the gas outlet space 5. This avoids higher velocities in the channels of the sublimation zone 4 and, accordingly, reduces the pressure drop across the sublimation zone 4. Large flows through individual channels can lead to their rapid blockage. In extreme cases, the effect can even be such that sublimation only partially occurs at the channel walls due to the high velocity of the gas mixture flow. The baffle 8 reduces the excessive velocities and backflows caused by them in adjacent channels, thereby avoiding or at least partially avoiding the aforementioned effects.

[0160] Example 4 A thermodynamic simulation of an embodiment of the method of operating the sublimator 1 of the invention according to Figure 1 was carried out in Fluent. The only difference between this Example 4 and Example 1 is the spacing A of the baffles 8. T In this third embodiment, the interval A T is equal to 5.53.

[0161] The surface area of ​​the sublimation zone 4 is shown in FIG. 17, which shows the velocity of the gas mixture flow in the direction of the longitudinal axis of the channel at the start of the loading process, the surface area being at the top of the sublimation zone 4.

[0162] Sublimation on the channel walls of the sublimation zone 4 occurs at the beginning of the loading process mainly in the area opposite the inlet region 9. Later, during the loading process, the sublimation sites move towards the inlet region 9.

[0163] Velocities with velocity vectors oriented in the direction of the main flow direction of the gas mixture flow through the flow passage of the sublimation zone 4 are shown in black if the magnitude of the velocity is 10 m / s or greater. Velocities with velocity vectors oriented in the direction opposite to the main flow direction of the gas mixture flow through the flow passage of the sublimation zone 4 are shown in white if the magnitude of the velocity is greater than 0 m / s.

[0164] As is clear from a comparison of Figures 11 and 17, the rear area of ​​the gas inlet distributor space 3 in the main flow direction shows a velocity direction across the entire width B of the sublimator 1, oriented toward the gas outlet space 5. This avoids higher velocities in the channels of the sublimation zone 4 and accordingly reduces the pressure drop across the sublimation zone 4. Large flows through individual channels can lead to their rapid blockage. In extreme cases, the effect can even be such that sublimation only partially occurs at the channel walls due to the high velocity of the gas mixture flow. The baffle 8 reduces the excessive velocities and backflows caused by them in adjacent channels, thereby avoiding or at least partially avoiding the aforementioned effects.

[0165] Example 5 A thermodynamic simulation of an embodiment of the present invention of a method for operating the inventive sublimator 1 according to Fig. 1 was carried out in Fluent. The only difference between this example 5 and example 1 is the physical properties and mass flow rate of the gas mixture stream. In this example 5, the gas mixture stream is fed to the sublimator 1 via the inlet 2 at a mass flow rate of 30 t / h, an absolute pressure of 1.086 bar and a temperature of 178°C. The mass flow rate of the gas mixture stream here contains PA as the gas component to be sublimated in a concentration of 3 wt%, so that the gas mixture stream has a molar mass of 29.7 g / mol. Under these thermodynamic conditions, the kinematic viscosity of the gas mixture stream is 2.26 x 10 -5 Pa x s. The housing wall is at a temperature of 178°C.

[0166] The surface area of ​​the sublimation zone 4 is shown in Figure 18, which shows the velocity of the gas mixture flow in the direction of the longitudinal axis of the channel at the start of the loading process, the surface area being at the top of the sublimation zone 4. 2 The surface area of ​​the sublimator 1 is exposed to a flow from the gas inlet distributor space 3 to the gas outlet space 5. In the remaining part of the surface area, a counterflow occurs. The maximum velocity of the gas mixture flow through the sublimation zone 4 is 3.4 m / s, and the average velocity of the gas mixture flow through the sublimation zone 4 is 0.46 m / s. The pressure drop between the inlet 2 and the outlet 6 of the sublimator 1 is 3.3 mbar.

[0167] Sublimation on the channel walls of the sublimation zone 4 occurs at the beginning of the loading process mainly in the area opposite the inlet region 9. Later, during the loading process, the sublimation sites move towards the inlet region 9.

[0168] Velocities with velocity vectors oriented in the direction of the main flow direction of the gas mixture flow through the flow passage of the sublimation zone 4 are shown in black if the velocity magnitude is 12 m / s or greater. Velocities with velocity vectors oriented in the direction opposite to the main flow direction of the gas mixture flow through the flow passage of the sublimation zone 4 are shown in white if the velocity magnitude is greater than 0 m / s.

[0169] As is evident from a comparison of the two Figures 12 and 18, despite the different physical characteristics and mass flow rates of the gas mixture flow, the baffles 8 achieve a similar effect with respect to the uniformity of the distribution of the gas mixture flow through the flow path of the sublimation zone 4. In both Figures 12 and 18, the loading process occurs primarily on the side opposite the inlet region 9, with flow through a significant area near the inlet region 9 in a direction opposite to the main flow direction.

[0170] As a result, excess velocities and associated backflows in adjacent flow passages are reduced by the baffle 8, even if the gas mixture flows have different physical properties and mass flow rates.

[0171] The baffles 8 have been shown to achieve the effect of better uniformity of distribution through the flow path of the sublimation zone 4 with different physical properties of the gas mixture stream or different mass flow rates of the gas mixture stream.

[0172] Comparative Example 1 Compared to Example 1, there is no baffle 8. All other features of the sublimator 1 and the process parameters for the loading process are the same. Again, the simulation was carried out using Fluent software. The uniformity achieved in the distribution of the gas mixture flow through the individual channels is evaluated using the following results described from the flow simulation:

[0173] Sublimation Zone 4 is 8.6m 2 is contacted from the gas inlet distributor space 3 over a surface area of ​​13.4 m / s, which surface area corresponds to the top surface of the sublimation zone 4. In the remaining part of the surface area, a counterflow occurs. The maximum velocity of the gas mixture flow through the sublimation zone 4 is 13.4 m / s, and the average velocity of the gas mixture flow through the sublimation zone 4 is 0.46 m / s.

[0174] The surface area of ​​the sublimation zone 4 is shown in Figure 11, which shows the velocity of the gas mixture flow at the start of the loading process at the surface area shown in the direction of the longitudinal axis of the flow channel and at the surface area of ​​the top surface of the sublimation zone 4.

[0175] Sublimation on the channel walls of the sublimation zone 4 occurs at the beginning of the loading process mainly in the area opposite the inlet region 9. Later, during the loading process, the sublimation sites move towards the inlet region 9.

[0176] The surface area has a gradient between the central axis and the housing wall 7, the gradient being determined by the non-uniform velocity distribution. Sublimation occurs particularly in the vicinity of the housing wall 7. In the area of ​​the inlet region 9, at the beginning of the loading process, almost no sublimation occurs.

[0177] Velocities with velocity vectors oriented in the direction of the main flow direction of the gas mixture flow through the flow passage of the sublimation zone 4 are shown in black if the magnitude of the velocity is 10 m / s or more. Velocities with velocity vectors oriented in the direction opposite to the main flow direction of the gas mixture flow through the flow passage of the sublimation zone 4 are shown in white if the magnitude of the velocity is greater than 0 m / s. The values ​​in the intermediate region are represented according to the scale according to Figure 11.

[0178] A vector plot of the velocity vectors of the gas mixture flow at the beginning of the loading process in sublimator 1 is shown in Figure 13, which shows a vector plot at a cross section of the longitudinal sublimation section, where the length of the vector is constant and therefore independent of the magnitude of the velocity.

[0179] It can be seen that in the area essentially to the left of the sublimation zone 4, indicated by the rectangular box, the gas mixture flows completely through the sublimation zone 4 in the direction of the gas outlet space 5. The curved dashed line in the sublimation zone 4 indicates the switch point where the velocity direction through the flow passages of the sublimation zone 4 switches to the opposite direction. The greater the drop in the curve, the less the gas mixture flows through the flow passages of the sublimation zone 4 in the direction of the gas outlet space 5. In the area to the right of the curve, the gas mixture flows from the gas outlet space 5 through the flow passages of the sublimation zone 4 in the direction of the gas inlet distributor space 3.

[0180] Comparative Example 2 The only difference between Comparative Example 2 and Comparative Example 1 is the physical properties and mass flow rate of the gas mixture flow. Again, the simulation was performed using Fluent software.

[0181] In this comparative example 2, a gas mixture stream is fed to the sublimator 1 via the inlet 2 at a mass flow rate of 30 t / h, an absolute pressure of 1.086 bar and a temperature of 178°C. The mass flow rate of the gas mixture stream here contains PA as the gas component to be sublimated at a concentration of 3 wt%, so that the gas mixture stream has a molar mass of 29.7 g / mol. Under these thermodynamic conditions, the kinematic viscosity of the gas mixture stream is 2.26 x 10 -5Pa x s. The housing wall is at a temperature of 178°C.

[0182] The uniformity achieved in the distribution of the gas mixture flow through the individual channels is evaluated using the following results described from the flow simulation:

[0183] The sublimation zone 4 is contacted from the gas inlet distributor space 3 over a surface area according to Figure 19, the surface area corresponding to the top surface of the sublimation zone 4. The pressure drop between the inlet 2 and the outlet 6 of the sublimator 1 is 3.2 mbar.

[0184] 8.7m 2 Through this surface area there is a flow from the gas inlet distributor space 3 towards the gas outlet distributor space 5. In the remaining part of the surface area a reverse flow occurs. The maximum velocity of the gas mixture flow through the sublimation zone 4 is 11.2 m / s and the average velocity of the gas mixture flow through the sublimation zone 4 is 0.46 m / s.

[0185] The surface area of ​​the sublimation zone 4 is shown in Figure 19, which shows the velocity of the gas mixture flow at the start of the loading process at the surface area shown in the direction of the longitudinal axis of the flow channel and at the surface area of ​​the top surface of the sublimation zone 4.

[0186] Sublimation on the channel walls of the sublimation zone 4 occurs at the beginning of the loading process mainly in the area opposite the inlet region 9. Later, during the loading process, the sublimation sites move towards the inlet region 9.

[0187] The surface area has a gradient between the central axis and the housing wall 7, the gradient being determined by the non-uniform velocity distribution. Sublimation occurs particularly in the vicinity of the housing wall 7. In the area of ​​the inlet region 9, at the beginning of the loading process, almost no sublimation occurs.

[0188] Velocities with velocity vectors oriented in the direction of the main flow direction of the gas mixture flow through the flow passage of the sublimation zone 4 are shown in black if the magnitude of the velocity is 12 m / s or more. Velocities with velocity vectors oriented in the direction opposite to the main flow direction of the gas mixture flow through the flow passage of the sublimation zone 4 are shown in white if the magnitude of the velocity is greater than 0 m / s. The values ​​in the intermediate zone are represented according to the scale according to Figure 19.

[0189] Conclusion: Example 1 has a surface area that is about 12% greater than the surface area of ​​Comparative Example 1. Additionally, Example 1 has a maximum velocity that is about 44% less than the maximum velocity of Comparative Example 1.

[0190] The larger the contact area, the more channels flow from the gas inlet distributor space towards the gas outlet distributor space. In particular, this utilizes a larger proportion of the available sublimation area represented by the walls of the channels. As a result, the channels walls are subjected to a more uniform loading and the corresponding channels are less rapidly blocked.

[0191] The greater the maximum velocity through the corresponding channel, the more pressure drop occurs during the loading process across the channel.

[0192] In particular, in the zone of maximum velocity, a very low percentage of the available sublimation area is exposed to very high volumetric flow rates. Therefore, there is a significant local increase in sublimation here, such that these channels are quickly blocked and can no longer be utilized for the duration of the loading process. Furthermore, at very high volumetric flow rates, there is an increased risk that at least one gas component to be sublimated cannot be completely separated in this zone.

[0193] Furthermore, the smaller surface area means that the gas mixture flows through only a small area of ​​the sublimation zone 4, and the individual channels of the sublimation zone 4 are covered by sublimation more quickly.

[0194] Additionally, excessive velocities can cause backflow in adjacent channels or enhance existing areas of backflow in adjacent channels, which significantly increases the pressure drop across the sublimation zone 4.

[0195] Examples 2-5 show similar improvements compared to Comparative Example 1. For example, Example 2 has a contact area that is approximately 12% larger than Comparative Example 1. Furthermore, Example 2 has a maximum speed that is approximately 40% lower than the maximum speed of Comparative Example 1.

[0196] Also, Example 3 has a contact area that is about 7% smaller than Comparative Example 1, but Example 3 has a maximum speed that is about 32% lower compared to the maximum speed of Comparative Example 1.

[0197] Furthermore, Example 4 has a contact area that is about 28% smaller than Comparative Example 1, but Example 4 has a maximum velocity that is about 20% lower compared to the maximum velocity of Comparative Example 1.

[0198] Furthermore, Example 5 has a contact area that is about 43% larger than that of Comparative Example 1. Furthermore, Example 5 has a maximum velocity that is about 74% lower than that of Comparative Example 1.

[0199] Finally, we report below the so-called Uniformity Index Mass Weighted, which is described in the Fluent Version 2022R1 manual from page 986 onwards. The manual can be found on the web page https: / / www.ansys.com / de-de / products / fluids / ansys-fluent (retrieved on December 6, 2023).

[0200] A relatively high uniformity index is the objective, since in that case the flow through the channel walls becomes more uniform, so that sublimation occurs more uniformly at the channel walls, and therefore the sublimator can be operated for a longer period in the loading process, thereby increasing the sublimation loading capacity. Furthermore, the risk of local excessive velocities, such that at least one gas component to be sublimated is not completely separated in the sublimation zone and / or the channel in question becomes impassable within a very short loading time, is reduced.

[0201] This uniformity index is based, in the example embodiment, only on the contact area where there is flow in the direction from the entrance region of the sublimation zone to the exit region of the sublimation zone.

[0202] For example, Example 1 has a uniformity index that is about 12% higher than that of Comparative Example 1, Example 2 has a uniformity index that is about 13% higher than that of Comparative Example 1, Example 3 has a uniformity index that is about 15% higher than that of Comparative Example 1, Example 4 has a uniformity index that is about 20% higher than that of Comparative Example 1, and Example 5 has a uniformity index that is about 7% higher than that of Comparative Example 1. [Explanation of symbols]

[0203] 1 coagulator 2 entrance 3 Gas inlet distributor space 4. Sublimation Zone 5 Gas outlet space 6 exit 7 Housing Wall 8 baffles 9 Entrance area 10 inlet port 11 Exit Port 12 Exit area 13 Projected surface area of ​​the baffle in the plane of the inlet area 14 Free gas passage area between the baffle and the sublimation zone 15 Curved or flat impact plates with or without holes 16 Curved or flat elements of mixer with or without quencher 17 Further outlet port with outflow valve 18 Second Baffle 19 Third Baffle 20 Baffle boundary frame 21 Fourth Baffle α1 Negative normal vector n of the entrance region E and the geometrically averaged normal vector n A the angle between α2 is the angle between two adjacent elements of the mixer A H1 is the distance between the geometric center of gravity of the first baffle and the geometric center of gravity of the inlet region, and the distance is determined by the normal vector n E It is measured along the A H2 is the distance between the geometric center of gravity of the second baffle and the geometric center of gravity of the inlet region, and the distance is determined by the normal vector n E It is measured along the A H3 is the distance between the geometric center of gravity of the third baffle and the geometric center of gravity of the inlet region, and the distance is determined by the normal vector n E It is measured along the A H4 is the distance between the geometric center of gravity of the fourth baffle and the geometric center of gravity of the inlet region, and the distance is determined by the normal vector n E It is measured along the A H、max is the distance between the geometric center of gravity of the baffle at the greatest distance from the inlet area and the geometric center of gravity of the inlet area, and distance A H、max is measured along the longitudinal axis of the flow channel in the sublimation zone. A T is the distance between the geometric center of gravity of the first baffle and the geometric center of gravity of the inlet region, and the distance is determined by the normal vector n E It is measured along the A T2 The distance between the geometric center of gravity of the second baffle and the geometric center of gravity of the first baffle. A T3 The distance between the geometric center of gravity of the third baffle and the geometric center of gravity of the second baffle. A T4 The distance between the geometric center of gravity of the fourth baffle and the geometric center of gravity of the third baffle. A T、max The distance between the geometric center of gravity of the inlet region and the baffle furthest from the inlet region. A S1 Distance between the first baffle and the sublimation zone A S2 Distance between the second baffle and the sublimation zone A S3 Distance between the third baffle and the sublimation zone A S4 Distance between the fourth baffle and the sublimation zone B. Width of sublimator B S Baffle width D equivalent diameter g gravity vector H Height of sublimator L Length of sublimator n A Geometrically averaged normal vector of the baffle surface facing the inlet n E Normal vector of the entrance area S L Baffle length S H Baffle height

Claims

1. A discontinuously operating sublimator (1) for removing at least one gas component to be sublimated from a gas mixture flow, comprising: a housing wall (7) as the outer boundary; an inlet (2) in said housing wall (7) for feeding said gas mixture flow into said sublimator (1); an outlet (6) in said housing wall (7) for removing the treated gas mixture stream from said sublimator (1); a sublimation zone (4) having temperature-controllable channel walls, the temperature of which is controllable so that during a loading process, the at least one gas component to be sublimated sublimes on the channel walls, and during a subsequent melting process, the at least one gas component sublimated during the loading process melts on the channel walls; a gas inlet distributor space (3) between the inlet (2) and the sublimation zone (4); a gas outlet space (5) between said outlet (6) and said sublimation zone (4); Equipped with At least a first baffle (8) arranged in the gas inlet distributor space (3) for uniform distribution of the gas mixture flow through the flow passages arising from the flow passage walls in the sublimation zone (4) is located at a distance (A Ｔ ) has a geometric center of gravity lying in the range of 0.2×D to 10.0×D, preferably in the range of 0.5×D to 3.0×D, where D corresponds to the equivalent diameter of a circle having an area equal to that of said inlet region (9), and said distance (A Ｔ ) is the normal vector (n Ｅ ) is measured along Coagulant (1).

2. When there are multiple baffles (8, 18, 19), the respective distances (A) between the geometric centers of gravity of adjacent baffles (8, 18, 19) Ｔ１ , A Ｔ２ ) is in the range of 0.01×L to 0.5×L, preferably in the range of 0.05×L to 0.33×L, where L corresponds to the length of the longitudinal axis of the gas inlet distributor space (3), and the respective distances (A Ｔ１ , A Ｔ２ ) is the normal vector (n Ｅ 2. The sublimator (1) according to claim 1, wherein the distance is measured along the axis of the sublimator.

3. The distance (A) between the sublimation zone (4) and the first baffle (8) Ｓ１ ), or if there are several baffles (8, 18, 19), the respective distances (A) between the sublimation zone (4) and each of the baffles (8, 18, 19) Ｓ１ , A Ｓ２ , A Ｓ３ 3. The sublimator (1) according to claim 1 or 2, wherein the distance D is at least 0.5×D.

4. At least the first baffle (8) has a width (B Ｓ 4. The sublimator (1) according to claim 1, wherein at said maximum width, said at least one baffle (8) extends to said two opposing housing walls (7) of said sublimator (1).

5. 5. The sublimator (1) according to claim 1, wherein the sublimator (1) has a horizontal longitudinal axis oriented perpendicular to the longitudinal axis of the flow path of the sublimation zone (4), and the gas inlet distributor space (3) is arranged above the sublimation zone (4).

6. At least the first baffle (8) has a distance (A) between the geometric center of gravity of the baffle (8) and the geometric center of gravity of the inlet region (9). Ｈ１ ) is in the range of 0 to 2.0 × D, preferably in the range of 0 to 0.5 × D, and Ｈ１ 6. The sublimator (1) according to claim 5, wherein the geometric center of gravity of the first baffle (8) is preferably below the geometric center of gravity of the inlet region (9).

7. In the case of a plurality of baffles (8, 18, 19), each individual baffle (18, 19) downstream of the first baffle (8) has a distance (A) between its geometric center of gravity and the geometric center of gravity of the baffle (8, 18) immediately adjacent to it in the direction of the inlet (2). Ｈ２ , A Ｈ３ ) is in the range of 0 to 1.0 × D, preferably in the range of 0 to 0.5 × D, and the distance (A Ｈ２ , A Ｈ３ 7. The sublimator (1) according to claim 5 or 6, wherein the distance (km) is measured along the longitudinal axis of the flow channel of the sublimation zone (4).

8. In the case of a plurality of baffles (8, 18, 19), the baffles (8, 18, 19) at a greater distance from the inlet region (9) are arranged at a higher level than the baffles at a shorter distance from the inlet region (9), and the distance from the inlet region (9) is determined by the normal vector (n Ｅ 8. The sublimator (1) according to any one of claims 5 to 7, wherein the distance is measured along the axis of the sublimator (1).

9. In the case of multiple baffles (8, 18, 19), the maximum distance (A Ｔ、ｍａｘ The geometric center of gravity of the baffle (19) having a distance (A) between the geometric center of gravity and the geometric center of gravity of the inlet region (9) Ｈ、ｍａｘ ) is in the range of 0 to 2.0 x D, preferably in the range of 0 to 1.0 x D, and in the case of three or more baffles (8, 18, 19), the other baffles (19) are preferably each the distance (A) between two adjacent baffles ((8, 18), (18, 19)). Ｔ１ , A Ｔ２ ) are arranged so that the distance (A Ｔ１ , A Ｔ２ ) is the normal vector (n Ｅ ), and the maximum distance (A Ｈ、ｍａｘ 9. The sublimator (1) according to any one of claims 5 to 8, wherein the distance is measured along the axis of the sublimator (1).

10. 10. The sublimator (1) according to any one of claims 1 to 9, wherein the free gas passage area (14), which is present between the sublimation zone (4) and the first baffle (8), or, in the case of a plurality of baffles (8, 18, 19), between the sublimation zone (4) and each of the baffles (8, 18, 19), is greater than 0.75 relative to the inlet area (9), preferably greater than 1.

0.

11. 11. The sublimator (1) according to any one of claims 1 to 10, wherein the surface area (13) of the first baffle (8), projected perpendicularly onto the plane of the inlet region (9), or, in the case of a plurality of baffles (8, 18, 19), the surface area (13) of each baffle (8, 18, 19), projected perpendicularly onto the plane of the inlet region (9), is greater than 1 relative to the inlet region (9).

12. At least the first baffle (8) has its longest side (S Ｌ ) and its shortest side (S Ｈ 12. The sublimator (1) according to any one of claims 1 to 11, wherein the ratio of 0.1 to 0.2 is in the range of 1 to 100, preferably in the range of 1 to 10.

13. 13. The sublimator (1) according to any one of claims 1 to 12, wherein the first baffle (8), or in the case of a plurality of baffles (8, 18, 19), each baffle (18, 19) is a static mixer or impingement plate (15), preferably an impingement plate (15) having an essentially rectangular design.

14. At least said first baffle (8) is in the form of a static mixer consisting of a plurality of cross beam elements, each individual cross beam element having two elements (16), at least said first baffle (8) being composed of at least two elements (16), preferably 4 to 16 elements (16), more preferably 6 elements (16), and adjacent elements (16) have an interior angle (α ) facing said inlet region (9) relative to each other in the range of 60 degrees to 120 degrees, preferably in the range of 85 degrees to 95 degrees, more preferably in the range of 89 degrees to 91 degrees. ２ 14. The sublimator (1) according to any one of claims 1 to 13, wherein the sublimator (1) is arranged in a

15. At least the first baffle (8) has a normal vector (n Ａ ), and the geometrically averaged normal vector (n Ａ ) and the normal vector (n Ｅ ) and the interior angle (α １ 15. The sublimator (1) according to any one of claims 1 to 14, wherein the angle of the sublimator (1) is in the range of -60 degrees to 60 degrees, preferably in the range of -45 degrees to 45 degrees, more preferably in the range of -15 degrees to 15 degrees.

16. 16. The sublimator (1) according to any one of the preceding claims, wherein the channel walls are defined by the outer walls of tube bundles, fin tubes, fin tube bundles, lamella bodies, honeycomb bodies and / or plate bodies.

17. 17. A method for operating a sublimator (1) according to any one of claims 1 to 16, characterized in that during the process of loading the sublimator (1), the gas mixture flow comprising the at least one gas component to be sublimated flows in at the inlet (2) with a mass flow rate of at least 0.01 kg / s, at a temperature in the range from above the sublimation temperature of the at least one gas component to be sublimated at a given pressure to 300°C above the sublimation temperature at the given pressure, and at an absolute pressure in the range of 0.1 bar to 10.00 bar, preferably in the range of 0.5 bar to 1.5 bar, more preferably in the range of 1.05 bar to 1.10 bar, the channel walls of the sublimation zone (4) are cooled to a temperature ranging from 150°C below the sublimation temperature at the given pressure to 1°C below the sublimation temperature at the given pressure; and the at least one gas component to be sublimated in the gas mixture flow is at least partially sublimated, preferably in the range of 10% to 100% by weight based on the at least one gas component to be sublimated in the gas mixture flow entering at the inlet (2), and more preferably in the range of 50% to 100% by weight based on the at least one gas component to be sublimated in the gas mixture flow entering at the inlet (2); method.

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