Device for treating, rinsing device for rinsing, drying device for drying and system for treating particulate solids, as well as methods for treating, rinsing and / or drying such solids

DE102022131061B4Active Publication Date: 2025-02-06PACE TEC GMBH
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Patent Information

Application Number
DE102022131061
Authority / Receiving Office
DE · DE
Patent Type
Patents
Current Assignee / Owner
Filing Date
2022-11-23
Publication Date
2025-02-06
Estimated Expiration
2042-11-23

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Abstract

Device (10) for treating particulate solids (12), the device (10) comprising: - at least one reactor (26) into which the particulate solids (12) can be introduced, the reactor (26) having a first grid (28) and a second grid (30) which define a reaction chamber (33) and retain the particulate solids (12) introduced into the reaction chamber (33) in the reaction chamber (33), and - at least one closable or sealed receiving chamber (22) into which the reactor (26) can be introduced, - a feed line (44) for supplying a process fluid into the receiving chamber (22), - at least one conveying unit (42) for conveying the process fluid and a reaction mixture of the process fluid and the particulate solids (12) through the receiving chamber (22), the receiving chamber (22) being configured such that the The process fluid and the reaction mixture with the pumping unit (42) activated the first grid (28),the reaction chamber (33) and the second grid (30) flow through when the reactor (26) is placed in the receiving chamber (22), characterized in that the device (10) has an ultrasonic device (62) for coupling ultrasound into the reaction chamber (33).
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Description

The present invention relates to an apparatus for treating particulate solids. The invention further relates to a rinsing device for rinsing and to a drying device for drying such solids. The invention also relates to a method for treating, rinsing and / or drying such solids. The invention further relates to a system for treating particulate solids.In the context of the following description, the term "particulate solids" could be understood to mean, for example, a single-grade bed in which the particles consist for the most part of the same component, or a particulate mixture in which a plurality of components are contained in a particle.One application of the present invention is the recycling or purification of chemically separable mixtures of materials which are present as particulate solids. Components of such particulate solids can be elementary semiconductors such as silicon or compound semiconductors such as gallium arsenide. In particular during recycling, these components are frequently present in conjunction with other components, for example metals, which are typically used as carrier material. In other applications, the semiconductors serve as a support material for metals. The corresponding separation process is often relatively difficult. In many cases, apparatuses and processes with which recycling and purification can be carried out economically on an industrial scale are lacking.Information regarding the technical field to which the present invention relates can be found in DD 265 699 A1, DD 281 353 A5, DE 101 26 665 A1 and DE 60 2004 000 055 T2.It is therefore an object of an embodiment of the present invention to propose a device for treating, a flushing device for flushing and a drying device for drying particulate solids, with which it is possible to propose a remedy for the above-mentioned disadvantages and with which the processes mentioned can be carried out economically acceptable and technically controllable with such particulate solids. Furthermore, an embodiment of the present invention is based on the object of providing an economically viable and technically controllable method for treating, flushing and / or drying such particulate solids.This object is achieved by the features specified in claims 1, 9, 12, 14, 15 and 20. Advantageous embodiments are the subject matter of the dependent claims.An embodiment of the invention relates to an apparatus for treating particulate solids, the apparatus comprising:at least one reactor into which the particulate solids can be introduced, wherein the reactoro is a first grating; anda second grid which delimits a reaction space and retains the particulate solids introduced into the reaction space in the reaction space, andat least one closable or closed receiving space into which the reactor can be introduced,a supply line for supplying a process fluid into the receiving space,at least one conveying unit for conveying the process fluid and a reaction mixture of the process fluid and the particulate solids through the receiving space, wherein the receiving space is configured such that the process fluid and the reaction mixture flow through the first grid, the reaction space and the second grid when the conveying unit is activated, when the reactor is introduced into the receiving space.In the context of the present description, a reaction mixture could be understood to mean a mixture which arises during or after the action of the process fluid on the particulate solids. The process fluid could in this case in particular be an alkali solution, an acid and / or water or comprise these substances. It should be emphasized at this point that the present invention could also be applicable to other reaction mixtures.An essential point of the device according to the invention is that the reaction takes place in a transportable reactor. The particulate solids can be introduced into the reactor at any location. The reactor can then be transported to the apparatus and introduced there into the receiving space. The particulate solids are then treated with the process fluid, wherein the reactor is arranged in the receiving space in such a way that the process fluid and / or the reaction mixture flow through the reactor in a forced manner. As a result, depending on the process control, a type of fluidized bed is produced, as a result of which the material transport between the particulate solids and the process fluid is promoted. Due to the action of the process fluid on the particulate solids, metals, for example, are at least partially separated from the carrier material and at least briefly dissolve, while the carrier material remains in the solid state. As a result, a substantial separation of the metal from the carrier material can be achieved without an increased energy consumption being necessary. In particular, it is not necessary to refill the particulate solids during the treatment.According to the invention, the apparatus has an ultrasonic device for coupling ultrasonics into the reaction space.According to a further embodiment, the receiving space can comprise a receiving section into which the reactor can be introduced while forming an intermediate space between the reactor and the receiving section which is closed at least in the radial direction. The provision of a receiving section makes it possible to position the reactor within the receiving section such that virtually all the process fluid and the entire water must flow through the reactor. In other words, due to the provision of the receiving portion, the reactor is integrated into the flow path of the process fluid and / or the reaction mixture through the receiving space. In this respect, the process fluid is used very effectively for treating the particulate solids.In a further developed embodiment, a reservoir container for holding the process fluid can be arranged in the receiving space. The receiver ensures that an additional volume is created where the process fluid and the reaction mixture can be stored. In particular, it is possible to change the ratio between water and the process fluid. In addition, the volume can be used to collect the reaction mixture in the receiver container during the removal or introduction of the reactor from or into the receiving space. A certain residence time can be set there, for example in order to change the temperature of the reaction mixture, as a result of which precipitation processes can be triggered and controlled. As a result, for example, the dissolved metal and / or other constituents such as valuable substances, for example noble metals, can be separated from the reaction mixture.In a further developed embodiment, at least one filter unit for filtering the reaction mixture can be arranged in the receiving space. The reaction mixture must flow through the filter unit when it flows through the receiving space. For example, in the recycling mentioned at the beginning, not only can a mixture of the support material and metal be present, but also other substances can be present in this mixture, which can be removed from the reaction mixture by means of the filter unit, for example when a precipitation or crystallization process is carried out in the receiver vessel. The purity of the carrier material and of the metal after completion of the recycling process is thereby increased.In a further embodiment, the filter unit may beat least one screen insert arranged in the reactor and having a mesh width of from 0.5 mm to 5 mm and in particular from 1 mm to 2 mm, and / orat least one prefilter arranged in the receiver vessel and having a pore size of 50 μm to 500 μm and in particular of 80 μm and 120 μm and / orat least one fine filter arranged between the receiver and the reactor and having a pore size of 1 μm to 50 μm and in particular of 15 μm to 25 μm.The arrangement of the screen insert, the prefilter and the fine filter follows the flow direction of the reaction mixture within the receiving space. As mentioned at the beginning, the particulate solids are held in the reaction space by the first grid and by the second grid. After the action of the process fluid on the particulate solids, there is usually a decrease in the average particle size, which may result in a greater portion of the mixture being able to traverse the first grid and the second grid, although the process being performed has not yet been fully performed. The sieve insert prevents such relatively large particles from being able to leave the reaction space, so that they can be treated further in the reactor and the desired residence time can be achieved. The prefilter can be used to collect precipitated substances such as metal hydroxide or washed-out particles such as the support material or further components obtained in the receiver vessel and remove them from the reaction mixture. The same applies to the fine filter which is arranged downstream of the prefilter. The fine filter can be arranged in the region into which a pipeline passes from the storage container into the receiving section. Fine particles which have formed in this pipeline or which are so small that they could pass through the prefilter can then also be filtered.A further embodiment may be characterized in that the device comprises at least one coolant line for supplying a coolant into the receiving space. Water can be used in particular as coolant. The reaction between the particulate solids and the process fluid can be strongly exothermic, so that very high temperatures can be formed within a very short time and the reaction can hardly be controlled any longer. The progress of this reaction can be seen only with great difficulty, especially for the following reason: the materials provided for recycling are usually supplied in the shredded state, as a result of which the mixture is present in the form of particles. However, the particle size distribution of the particulate solids is very different, so that the particles can have very different specific surfaces from batch to batch. If the particulate solids to be treated at the moment have a comparatively high specific surface area, the corresponding mass transfer between the process fluid and the particulate solids is particularly intensive, so that the reaction proceeds very vigorously and can no longer be controlled. In this case, the reaction can be slowed down and, in particular, stopped with the coolant, so that the generation of very high temperatures, which could damage the reactor, for example, can be prevented. Supplying a coolant to slow down or stop a chemical reaction is also referred to as "quenching.".In a further embodiment, it can be expedient for the ultrasonic device to have a number of ultrasonic vibrators which are arranged on the receiving section. The arrangement of ultrasonic oscillators on the receiving section makes it possible to couple the ultrasonic waves into the reaction space as directly as possible and without major losses.According to a further embodiment, the reactor can have a number of apertures corresponding to the number of ultrasonic oscillators, which apertures are arranged such that they are aligned with the ultrasonic oscillators when the reactor is introduced into the receiving section. In this embodiment, the ultrasound can enter the reaction space without the wall of the reactor causing attenuation of the ultrasound. As mentioned, the receiving space can have a receiving section into which the reactor can be introduced while forming an intermediate space closed in the radial direction. The volume of this intermediate space can be kept small. Although a certain proportion of the reaction mixture can pass through the apertures into this intermediate space, since this proportion is very small, this can be accepted. In addition, the presence of the reaction mixture in the intermediate space promotes the transmission of the ultrasound into the reaction space, since no air layer attenuating the ultrasound is present.One embodiment of the invention relates to a flushing device for flushing particulate solids, wherein the flushing device comprises:at least one reactor into which the particulate solids can be introduced, wherein the reactoro is a first grating; anda second grid which delimits a reaction space and retains the particulate solids introduced into the reaction space in the reaction space, andat least one closable or closed receiving space into which the reactor can be introduced,a flushing fluid supply line for supplying a flushing fluid into the receiving space,at least one flushing fluid conveying unit for conveying the flushing fluid through the receiving space, wherein the receiving space is configured such that the flushing fluid flows through the first grid, the reaction space and the second grid when the flushing fluid conveying unit is activated when the reactor is introduced into the receiving space.It should be mentioned at this point that the flushing device can be used both for flushing the particulate solids and for flushing the reaction mixture. In the first case, the flushing serves to free the particulate solids from contaminants which have formed, for example, during shredding of the starting material before the particulate solids are treated with the process fluid. In the second case, the flushing serves to remove residues of the process fluid used from the particulate solids, for example in order to subsequently feed the particulate solids to a treatment with another process fluid.The essential structure of the flushing device is the same as the structure of the device with which the particulate solids are treated. In particular, in this case as well, a type of fluidized bed is produced when the flushing fluid flows through the reactor, whereby the flushing can be carried out particularly effectively and thoroughly.According to the invention, it is provided that the receiving space comprises a receiving section into which the reactor can be introduced while forming an intermediate space between the reactor and the receiving section which is closed at least in the radial direction. Moreover, it is provided according to the invention that a seal is arranged in the receiving section, which seal interacts with the reactor in the region of the first grid. The provision of a receiving section makes it possible to position the reactor within the receiving section in such a way that virtually all the flushing fluid has to flow through the reactor. In other words, due to the provision of the accommodation portion, the reactor is integrated into the flow path of the scavenging fluid through the accommodation space. In this respect, the flushing fluid is used very effectively for flushing the particulate solids.A more advanced embodiment can specify that a rinsing fluid storage container for holding the rinsing fluid is arranged in the receiving space. In the rinsing fluid receiver, for example, the rinsing fluid can be heated to a certain temperature, if this is desired. Furthermore, if this is not yet excessively contaminated, already used flushing fluid can be temporarily stored while the reactor is removed from the receiving section and another reactor with another charge of the particulate solids to be flushed is inserted therein. The flushing fluid can then be reused.According to a further development, the device can have at least one flushing fluid discharge line for discharging the flushing fluid from the receiving space. If the flushing fluid is so heavily contaminated that it can no longer be used, it can be discharged from the flushing device via the flushing fluid discharge line.One embodiment of the invention relates to a drying device for drying particulate solids, wherein the drying device comprises:at least one reactor into which the particulate solids can be introduced, wherein the reactor◯ a first grating, and◯ has a second grid which delimits a reaction space and retains the particulate solids introduced into the reaction space in the reaction space, andat least one closable or closed receiving space into which the reactor can be introduced,at least one suction unit for conveying a drying fluid through the receiving space, wherein the receiving space is configured such that the drying fluid flows through the first grid, the reaction space and the second grid when the suction unit is activated, when the reactor is introduced into the receiving space.The drying device serves in particular to dry the particulate solids. As mentioned, the particulate solids are treated with the usually liquid process fluid, so that the particulate solids are moist after the treatment. For subsequent storage and transport, however, it is desirable in many ways for the particulate solids to be dried, which can be accomplished with the drying apparatus. In particular, in this case as well, a type of fluidized bed is produced when the drying fluid flows through the reactor, whereby the drying can be carried out particularly effectively and thoroughly. The use of heated air is suitable as the drying fluid, which can be sucked and heated from the surroundings of the drying device, for example, by means of the suction unit designed as a side duct compressor.In a further development, the receiving space can comprise a receiving section into which the reactor can be introduced while forming an intermediate space between the reactor and the receiving section which is closed at least in the radial direction. The provision of a receiving section makes it possible to position the reactor within the receiving section in such a way that virtually all the drying fluid must flow through the reactor. In other words, due to the provision of the accommodation portion, the reactor is integrated into the flow path of the drying fluid through the accommodation space. In this respect, the drying fluid is used very effectively for drying the particulate solids.One embodiment of the invention relates to a system for treating particulate solids comprisinga first device for treating particulate solids according to one of the aforementioned embodiments,a second device for treating particulate solids according to one of the aforementioned embodiments,a first flushing device for flushing the particulate solids according to one of the embodiments discussed above,a third device for treating particulate solids according to one of the aforementioned embodiments,a second flushing device for flushing the particulate solids according to one of the embodiments discussed above,a drying device for drying the particulate solids according to one of the embodiments described above, anda transport device for transporting the reactor within the system.In this system, the particulate solids can be treated in different ways. The system according to this implementation comprises a total of six stations, wherein the particulate solids are transported from one station to the next by means of a transport device. The particulate solids always remain in the reactor, so that the reactor also has the function of a carrier with respect to the particulate solids. It is not necessary to replenish the particulate solids, thus simplifying and accelerating the treatment. The provision of a total of six stations has proven to be optimum for a multiplicity of treatment processes for particulate solids, in particular if the reactions can proceed strongly exothermically. In this case, a total of three apparatuses for treating the particulate solids, two rinsing apparatuses for rinsing the particulate solids and a drying apparatus for drying the particulate solids are provided.An implementation of the present invention relates to a method for treating particulate solids with an apparatus according to the embodiments explained above, comprising the following steps:introducing the particulate solids to be treated into the reaction space,introducing the reactor into the receiving space,supplying a process fluid into the receiving space, andconveying the process fluid and a reaction mixture of the process fluid and the particulate solids through the receiving space in such a way that the process fluid and the reaction mixture flow through the first grid, the reaction space and the second grid when the conveying unit is activated.The technical effects and advantages that can be achieved with the method according to the invention correspond to those discussed for the correspondingly configured device for treating particulate solids. In summary, it should be pointed out that a type of fluidized bed is produced when flowing through the reactor, as a result of which the treatment of the particulate solids can be carried out particularly effectively and thoroughly.According to the invention, the method comprises the following step:coupling ultrasound into the reaction space by means of the ultrasound device.For the separation of some materials from the carrier material, it may be necessary to couple ultrasound into the process fluid, whereby the separation result and in particular the purity level achieved at the end of the recycling process can be increased.In another implementation, the method may include the steps of:determining the temperature of the reaction mixture in the receiving space by means of a temperature determination unit, andsupplying a coolant into the receiving space by means of the coolant line if the determined temperature exceeds a limit value.Water can be used in particular as coolant. As mentioned, the reaction between the particulate solids and the process fluid can be highly exothermic, so that very high temperatures can be formed within a very short time and the reaction can no longer be controllable. However, it is already possible to estimate, on the basis of the temperature profile, whether or not the reaction is in controlled trajectories. If the temperature curve indicates that the reaction could no longer be controllable, the coolant can be supplied in good time and the reaction can be delayed or stopped. Damage to the reactor can thereby be avoided.According to a further implementation, the method can have the following steps:supplying a flushing fluid into the receiving space by means of a flushing fluid conveying line, andconveying the flushing fluid through the receiving space by means of a flushing fluid conveying unit in such a way that the flushing fluid flows through the first grid, the reaction space and the second grid when the flushing fluid conveying unit is activated.As mentioned, the flushing device can be used both for flushing the particulate solids and for flushing the reaction mixture. In particular, in this case as well, a type of fluidized bed is produced when the flushing fluid flows through the reactor, whereby the flushing can be carried out particularly effectively and thoroughly.In a further implementation, it may be advantageous for the method to have the following steps:conveying a drying fluid through the receiving space by means of a suction unit, wherein the receiving space is configured such that the drying fluid flows through the first grid, the reaction space and the second grid when the suction unit is activated.As mentioned, the particulate solids are often treated with a liquid process fluid such that the particulate solids are moist after treatment. For subsequent storage and transport, however, it is desirable in many ways for the particulate solids to be dried, which can be accomplished with the drying apparatus. In particular, in this case as well, a type of fluidized bed is produced when the drying fluid flows through the reactor, whereby the drying can be carried out particularly effectively and thoroughly. The use of heated air is suitable as the drying fluid, which can be sucked and heated from the surroundings of the drying device, for example, by means of the suction unit designed as a side duct compressor.In a further development of the implementation, the first grid can be arranged below the second grid during the intended use of the device and the drying fluid can flow through the reaction space from the second grid to the first grid. In this embodiment, the drying fluid flows through the reactor along the direction of action of gravity. The energy which must be applied for the flow is significantly lower than in the case where the drying fluid would flow through the reactor counter to the direction of action of gravity. In addition, the particulate solids in this configuration are flowed through more uniformly than if the particulate solids are flowed through counter to the direction of action. If the particulate solids are flowed through counter to the direction of action, flow channels can be formed through which the drying fluid flows in an increased manner, while other regions of the particulate solids are not flowed through or are flowed through to a lesser extent.One embodiment of the invention relates to a method for treating particulate solids with a system according to the embodiment described above, comprising the following steps:introducing the reactor into the receiving space of the first apparatus for treating particulate solids by means of the transport device, and treating the particulate solids with the first apparatus,removing the reactor from the receiving space of the first device, introducing the reactor into the receiving space of the second device for treating particulate solids by means of the transport device, and treating the particulate solids with the second device,removing the reactor from the receiving space of the second device, introducing the reactor into the receiving space of the first flushing device for flushing the particulate solids by means of the transport device, and flushing the treated solids by means of the first flushing device,removing the reactor from the receiving space of the first flushing device, introducing the reactor into the receiving space of the third device for treating particulate solids by means of the transport device, and treating the particulate solids with the third device, wherein ultrasound is coupled into the reaction space,removing the reactor from the receiving space of the third device, introducing the reactor into the receiving space of the second flushing device for flushing the particulate solids by means of the transport device, and flushing the treated solids by means of the second flushing device,removing the reactor from the receiving space of the second flushing device, introducing the reactor into the receiving space of the drying device for drying the particulate solids by means of the transport device and drying the treated solids by means of the drying device, andremoving the reactor from the receiving space of the drying device by means of the transport device.The above-mentioned sequence of the various steps to which the particulate solids are subjected represents the preferred sequence, it not being excluded that other sequences may also be targeted. It should be mentioned in particular that the particulate solids are first treated twice in succession with the process fluid and the water. As mentioned, for example, the reaction between the metal and the process fluid and the water may be very violent. As likewise mentioned, a decisive factor here is the specific surface area of the particulate solids, which can deviate significantly from batch to batch. In the first apparatus, the process fluid is contacted with the particulate solids at a comparatively low temperature, whereby the probability of a violent and uncontrollable reaction occurring is low. As a result of the treatment of the particulate solids in the first device, the specific surface area is reduced because, inter alia, sections of the particulate solids protruding outward in a star shape are removed. During the subsequent treatment in the second device, the temperature of the process fluid in particular can consequently be increased, which is desirable for a rapid and extensive reaction. However, since, as mentioned, the specific surface area is reduced in the first device, the probability of a violent and uncontrollable reaction occurring is significantly reduced.For transferring the particulate solids from the first device to the second device, the transport device grasps the reactor, removes it from the receiving space of the first device and inserts it into the receiving space of the second device. The particulate solids remain in the reactor without the particulate solids having to be transferred. The procedure is accordingly followed when transferring between the remaining stations of the system. After the particulate solids have been treated in the second apparatus, they are transferred to the first rinsing apparatus for rinsing in the manner explained above. After rinsing has taken place, the particulate solids are transferred into the third device, where, in addition to the treatment with the process fluid, an ultrasonic treatment is also carried out, which serves, for example, for separating valuable materials from the carrier material. The particulate solids are then transferred to the second flushing device, so that residues of the reaction mixture which have formed in the third device are removed from the particulate solids. Finally, the particulate solids are dried in the drying device.Exemplary embodiments of the invention are explained in more detail below with reference to the attached drawings. They show FIG. 1 shows an embodiment of an apparatus for treating particulate solids, FIG. 2 shows an embodiment of a flushing device for flushing particulate solids, FIG. 3 shows an embodiment of a drying device for drying particulate solids, and FIG. 4 shows a representation of a system for treating particulate solids, in each case on the basis of principal representations.FIG. 1 shows a device 10 for treating particulate solids 12 on the basis of a basic sectional illustration. The particulate solids 12 which are to be treated with the apparatus 10 can have, for example, a carrier material and metal, but can also comprise further components, of which, in particular, valuable materials are to be mentioned. However, it is also possible to treat particulate solids having a completely different composition.The device 10 is bounded by a device wall 14 which encloses an interior 16. The interior 16 is accessible through an opening 18 which can be selectively opened or closed by a cover 20. In the interior 16, the device 10 forms a receiving space 22, which can be closed by the mentioned cover 20 and forms a receiving section 24, the precise function of which will be discussed in more detail later.The apparatus 10 comprises a reactor 26 into which the particulate solids 12 can be introduced. The reactor 26 has a first grid 28 and a second grid 30, which together with a reactor wall 32 delimit a reaction space 33. The grids 28, 30 are dimensioned such that they permit the flow through the reaction space 33, which will be discussed in more detail below, but at the same time retain the particulate solids 12 in the reaction space 33. The second grid 30 is detachably fastened to the reactor wall 32, wherein the fastening means used for this purpose, such as clamps or screws, are not shown.The reactor also has one or more side openings 36, the function of which will likewise be discussed in more detail later.The reactor 26 can be introduced into the receiving section 24 already mentioned, for which purpose a transport device 34, not shown here (see FIG. 4 in this regard), can be used. For this purpose, the cover 20, with which both the interior 16 and the receiving space 22 can be closed, is opened.Furthermore, a storage container 38 is arranged in the interior 16 of the apparatus 10, which storage container is likewise to be understood as a part of the receiving space 22. Moreover, the receiving section 24 is connected to the storage container 38 by pipelines 40, which likewise form part of the receiving space 22. Furthermore, a conveying unit 42 is provided, which communicates with one of the pipelines 40.By means of a supply line 44, a process fluid can be guided into the receiving space 22, which can subsequently be conveyed and circulated within the receiving space 22 by means of the conveying unit 42. In the embodiment shown, the supply line 44 comprises a first supply sub-line 46 1, with which, for example, a base solution or an acid can be conveyed as process fluid into the receiver tank 38. In addition, the supply line 44 comprises a second supply sub-line 46 2, with which a second substance such as water can be conveyed into the storage container 38. The pumps and valves necessary for this purpose are not shown. However, it is possible to adjust the concentration as desired with the ratio of the supplied volume of alkali or acid and water.Furthermore, a discharge line 48 is provided, with which the process fluid can be discharged from the receiving space 22. As can be seen from FIG. 1, the receiver 38 is provided with a double jacket 50, which is part of a temperature control device 52, not shown in more detail. With this temperature control device 52, the process fluid can be brought to the desired temperature and held at this temperature.For this purpose, a temperature measuring unit, not shown, may be provided.Furthermore, the device 10 has a coolant line 54, with which a coolant, in particular water, can be introduced into the receiving space 22.As already mentioned, the reactor 26 can be introduced into the receiving section 24, as shown. For this purpose, the reactor 26 is provided with fastening sections 56, with which the reactor 26 can be positioned with respect to the receiving section 24. The receiving section 24 has a shape largely complementary to the shape of the reactor 26, so that an annular intermediate space 58 is formed between the reactor 26 and the receiving section 24 in the radial direction. In the receiving section 24, a seal 60 is arranged, which interacts with the reactor 26 in the region of the first grid 28. The annular interspace 58 is therefore bounded on the one hand by the seal 60 and on the other hand by the fastening section 56 of the reactor 26. In this case, a seal 60, not shown here, can likewise be arranged in the fastening section 56. When the process fluid is circulated within the receiving space 22 when the reactor 26 is introduced into the receiving section 24, the process fluid flows through the reaction space 33, wherein the process fluid penetrates the reaction space 33 through the first grid 28 and leaves the reaction space 33 through the second grid 30. However, the process fluid cannot pass through the seal 60 and therefore cannot pass directly into the interspace 58.In addition, the apparatus 10 is provided with an ultrasonic device 62 which has a number of ultrasonic oscillators 64. The ultrasonic oscillators 64 are arranged on the receiving section 24, wherein a number of apertures 66 corresponding to the number of the ultrasonic oscillators 64 is provided in the reactor wall 32. The ultrasonic resonators 64 are arranged such that when the reactor 26 is introduced into the receiving section 24, the ultrasonic resonators 64 are brought into alignment with the apertures 66 and are aligned therewith. The fastening section 56 can be designed such that the reactor 26 can be introduced into the receiving space 22 only in specific rotational positions, for which purpose a type of bayonet closure can be provided, for example. As a result of the aligned alignment, the ultrasound can pass directly into the reaction space 33 without being significantly attenuated by the reactor wall 32.Furthermore, a filter unit 68 is provided, which in the embodiment shown comprises a screen insert 70 which is arranged in the reactor 26 and has a mesh width of 0.5 to 5 mm. The screen insert 70, which can have a plurality of sections which can be separated from one another, covers the first grid 28, the second grid 30, the side openings 36 and the apertures 66. Furthermore, a fine filter 74 having a pore size of 1 μm to 50 μm is assigned to the filter unit 68, which is positioned in the pipeline 40 leading to the receiving section 24. The use of the terms "mesh size" and "pore size" is intended to identify the different size ranges in which the filter unit 68 operates.The device 10 is further provided with a temperature determination unit 76, with which the temperature of the process fluid can be determined.The apparatus 10 is operated in the following manner: First, the particulate solids 12 are introduced into the reaction space 33, the second grid 30 being removed from the reactor 26 and the lid 20 being open. As can be seen from FIG. 1, the reaction space 33 is filled to approximately 2 / 3, so that a certain free space still remains to the second grid 30. Then, the second mesh 30 is attached to the reactor 26, and the reactor 26 is suspended in the receiving portion 24 using the transport device 34 shown in FIG. 4. The lid 20 is now closed and the desired volume of water and alkali or acid is conveyed into the receiver 38, wherein the receiver 38 is also not completely filled. The conveying unit 42 is activated so that the process fluid, here the alkali or the acid and the water, is conveyed from the storage container 38 to the receiving section 24. The process fluid now enters the reaction space 33 through the first grid 28 and flows through the reaction space 33 thereby forming a type of fluidized bed. As a result, a reaction occurs between the process fluid and the particulate solids 12, and the reaction mixture formed as a result of this reaction then leaves the reaction space 33 through the second grid 30 and the screen insert 70. the treated particulate solids 12 are retained in the reaction space 33 by the second grid 30 and the screen insert 70 and are in particular prevented from entering the intermediate space 58 through the side openings 36 and the apertures 66. As can be seen, the apertures 66 are larger than the holes of the second grid 30. Due to the formation of a fluidized bed, the second grid 30 and / or the screen insert 70 can clog in front of the second grid 30, so that the reaction mixture does not flow through it, or only to a small extent. The apertures 66 are not, however, added or only to a negligible extent, because of their arrangement and configuration.The reaction mixture then passes into the receiver tank 38 where it must pass through the prefilter 72 and is filtered accordingly. The reaction mixture then passes through the fine filter 74 into the reaction space 33 and flows through the particulate solids 12, and the reaction mixture can consequently be conveyed and circulated in circulation through the receiving space 22. The reaction mixture can be circulated in the receiving space 22 until the particulate solids 12 have been treated to the desired extent. The essential reaction takes place between the process fluid and the metal. The temperature of the reaction mixture is determined by means of the temperature determination unit 76. If the temperature of the reaction mixture exceeds a certain threshold value, an uncontrollable course of the reaction between the process fluid and the metal is to be expected. In this case, the refrigerant is fed into the receiving space 22 using the refrigerant pipe 54, and thus the reaction between the process fluid and the metal is stopped, and the feeding unit 42 is also stopped to suppress the formation of the fluidized bed. The relevant batch of particulate solids 12 must be disposed of.However, when the reaction is scheduled, the circulation of the reaction mixture is stopped after the desired time. The ultrasonic device 62 is then activated and ultrasonic waves are coupled into the particulate solids 12. Since the intermediate space 58 is filled with the reaction mixture, the ultrasound can be passed on well. Damping due to an air layer is avoided. Thereafter, the circulation may be reactivated. It is also possible to couple in the ultrasound during the circulation.After the treatment has been concluded, the reaction mixture is conveyed as far as possible into the receiver tank 38 and the reactor 26 with the transport device 34 is removed from the apparatus 10. The treated particulate solids 12 can then be further processed in the desired manner.Depending on how far the reaction mixture can still be used for the treatment of a further batch, the reaction mixture can remain in the receiving space 22 and in particular in the receiver container 38 and be circulated again as soon as a further reactor 26 with a further batch of the particulate solids 12 to be treated has been inserted into the receiving section 24. However, when the reaction mixture has been consumed to such an extent that it can no longer be used, it can be removed from the receiving space 22 by means of the discharge line 48.FIG. 2 shows a flushing device 78 for flushing particulate solids 12, wherein the basic design of the flushing device 78 corresponds largely to the design of the device 10 shown in FIG. 1 for treating such particulate solids 12. In particular, the reactor 26 is also introduced into the receiving section 24 here. The essential difference is that no process fluid is used, but rather a flushing fluid is used, which is introduced into the receiving space 22 by means of a flushing fluid supply line 79 and is circulated there, for which purpose a flushing fluid delivery unit 80 is used. The flushing fluid can be water in particular. However, since no process fluid is circulated, no corresponding reaction takes place between the process fluid and the particulate solids 12. Consequently, provision of a temperature determination unit 76 and a coolant line 54 can be omitted. In addition, the supply line 44 can be designed such that only the flushing fluid can be introduced into the receiving space 22. The flushing fluid can be removed from the receiving space 22 by means of a flushing fluid discharge line 82. The possibility of supplying an alkali is not required. The provision of an ultrasonic device 62 is also not necessary, but is also not excluded. The flushing device 78 also has the filter unit 68, however. Otherwise, the flushing device 78 is operated in the same way as the device 10 for treating the particulate solids 12. It should also be noted that the flushing fluid can likewise be stored in a flushing fluid storage container 38 and circulated within the receiving space 22.In FIG. 3, a drying device 84 for drying particulate solids 12 is shown. The drying device 84 is also substantially constructed in the same way as the device 10 described in FIG. 1 for treating such particulate solids 12. However, the drying fluid, in particular heated air, is not circulated here. As a result, the drying device 84 also does not have a storage container 38. Instead, air is drawn in from the environment of the drying device 84 by means of a suction unit 86, which can be designed, for example, as a side duct compressor, and in the process is heated to the desired temperature. The heated air is guided to the reactor 26 in such a way that, in contrast to the process fluid and the flushing fluid, it penetrates through the second grid 30 into the reaction space 33, flows through the particulate solids 12 and subsequently leaves the reaction space 33 again through the first grid 28. As mentioned, the drying fluid is not circulated but is discharged directly back to the environment. However, the heated air can also be blown into the reaction space 33 through the first grid 28 in the same direction as the process fluid and the flushing fluid.FIG. 4 shows a system 88 for treating particulate solids 12 on the basis of a basic illustration. The system 88 comprises, as seen from left to right, a first device 10 1 and a second device 10 2 for treating the particulate solids 12, which can be constructed in the same way as that shown in FIG. 1. Further, the system 88 includes a first flushing device 78 1, which may be constructed as that illustrated in FIG. 2. Furthermore, the system 88 comprises a third device 10 3 for treating the particulate solids 12, a second flushing device 78 2 and a drying device 84, wherein the drying device 84 can be constructed in the same way as that shown in FIG. 3.The particulate solids 12 are treated in the following manner: In the first device 10 for treating the particulate solids, the process fluid is brought into contact with the particulate solids 12 at a comparatively low temperature, whereby the probability of a violent and uncontrollable reaction occurring between the alkali and the metal is very low. As a result of the treatment of the particulate solids 12 in the first apparatus 10, the specific surface area of the particulate solids 12 is reduced because, inter alia, sections of the particulate solids protruding outward in a star shape are etched away. During the subsequent treatment in the second device 10, the temperature of the process fluid in particular can consequently be increased, which leads to a rapid and comprehensive reaction between the particulate solids 12 and the process fluid. However, as mentioned, since the specific surface area is reduced in the first device 10, the possibility of a violent and uncontrollable reaction occurring is significantly reduced.In order to transfer the particulate solids 12 from the first apparatus 10 1 to the second apparatus 10 2 the transport device 34 grasps the reactor 26, removes the latter from the receiving space 22 of the first apparatus 10 and inserts it into the receiving space 22 of the second apparatus 10 2. The particulate solids 12 remain in the reactor 26 without the particulate solids 12 having to be transferred. The procedure is accordingly followed during the transfer between the remaining stations of the system 88. After the particulate solids 12 have been treated in 2 in the second apparatus 10, they are transferred to the first flushing apparatus 78 1 for flushing in the manner explained above. After rinsing has taken place, the particulate solids 12 are transferred into the third device 10 3 where, in addition to the treatment with the process fluid, treatment with ultrasound is also carried out. Thereafter, the particulate solids 12 are transferred into the second flushing device 78 2 so that residues of the reaction mixture which have formed in the third device 10 3 are removed from the particulate solids 12. Finally, the particulate solids 12 are dried in the drying device 84.In FIG. 4, a first reactor 26 1, a second reactor 26 2, a third reactor 26 3 and a fourth reactor 26 4 are shown. While the first reactor 26 contains 1 untreated particulate solids 12, the particulate solids 12 of the second reactor 26 are treated in 2 in the first apparatus 10 1 in the process. The particulate solids 12 in the third reactor 26 3 and fourth reactor 26 4 have already passed through the system 88 completely and have been completely processed. As the particulate solids 12 pass through the system 88, they always remain in the reactor 26 which is moved from station to station by the transport device 34 without being replenished.List of reference characters10 Apparatus 10 1- 103 Apparatus 12 Particulate solids 14 Apparatus wall 16 Interior 18 Opening 20 Cover 22 Receiving space 24 Receiving section 26 Reactor 26 1- 264 Reactor 28 First grid 30 Second grid 32 Reactor wall 33 Reaction space 34 Transport device 36 Side opening 38 Storage container 40 Pipeline 42 Transport unit 44 Feed line 46 1 First feed sub-line 46 2 Second feed sub-line 48 Discharge line 50 Double jacket 52 Temperature control unit 54 Coolant line 56 Fastening section 58 Intermediate space 60 Seal 62 Ultrasound device 64 Ultrasound oscillator 66 Aperture 68 Filter unit 70 Screen insert 72 Prefilter 74 Fine filter 76 Temperature determination unit 78 Flushing apparatus 78 1- 78_ner 32_purger 79 rinsing fluid supply line 80 rinsing fluid supply unit 82 rinsing fluid discharge line 83 rinsing fluid storage container 84 drying device 86 suction unit 88 system

Claims

Device (10) for treating particulate solids (12), wherein the device (10) comprises: - at least one reactor (26) into which the particulate solids (12) can be introduced, wherein the reactor (26) ◯ has a first grid (28) and ◯ has a second grid (30), which delimit a reaction space (33) and retain the particulate solids (12) introduced into the reaction space (33) in the reaction space (33), and - at least one closable or closed receiving space (22) into which the reactor (26) can be introduced, - a feed line (44) for feeding a process fluid into the receiving space (22), - at least one feed unit (42) for feeding the process fluid and a reaction mixture of the process fluid and the particulate solids (12) through the receiving space (22), wherein the receiving space (22) is configured such that, the process fluid and the reaction mixture flow through the first grid (28), the reaction space (33) and the second grid (30) when the delivery unit (42) is activated, when the reactor (26) is introduced into the receiving space (22), characterized in that the apparatus (10) has an ultrasonic device (62) for coupling ultrasonics into the reaction space (33).Device (10) according to claim 1, characterised in that the receiving space (22) comprises a receiving section (24), into which the reactor (26) can be introduced, forming an intermediate space (58), which is closed at least in the radial direction, between the reactor (26) and the receiving section (24).Device (10) according to either of Claims 1 and 2, characterized in that a storage container (38) for holding the process fluid is arranged in the receiving space (22).Device (10) according to one of the preceding claims, characterized in that at least one filter unit (68) for filtering the reaction mixture is arranged in the receiving space (22).Device (10) according to Claim 4, characterized in that the filter unit (68) comprises - at least one screen insert (70), which is arranged in the reactor (26) and has a mesh width of from 0.5 mm to 5 mm and in particular from 1 mm to 2 mm, and / or - at least one prefilter (72), which is arranged in the feed container (38) and has a pore size of from 50 μm to 500 μm and in particular of from 80 μm and 120 μm, and / or - at least one fine filter (74), which is arranged between the feed container (38) and the reactor (26) and has a pore size of from 1 μm to 50 μm and in particular of from 15 μm to 25 μm.Device (10) according to one of the preceding claims, characterized in that the device (10) comprises at least one coolant line (54) for supplying a coolant into the receiving space (22).The device (10) according to one of claims 1 and 2, characterized in that the ultrasonic device (62) comprises a number of ultrasonic oscillators (64) which are arranged on the receiving section (24).Device (10) according to claim 7, characterised in that the reactor (26) has a number of apertures (66) corresponding to the number of ultrasonic oscillators (64), which apertures are arranged such that they are aligned with the ultrasonic oscillators (64) when the reactor (26) is introduced into the receiving section (24).Flushing device (78) for flushing particulate solids (12), wherein the flushing device (78) comprises: - at least one reactor (26) into which the particulate solids (12) can be introduced, wherein the reactor (26) ◯ has a first grid (28) and ◯ has a second grid (30), which delimit a reaction space (33) and retain the particulate solids (12) introduced into the reaction space (33) in the reaction space (33), and - at least one closable or closed receiving space (22) into which the reactor (26) can be introduced, - a flushing fluid supply line (79) for supplying a flushing fluid into the receiving space (22), - at least one flushing fluid conveying unit (80) for conveying the flushing fluid through the receiving space (22), wherein the receiving space (22) is designed such that, the flushing fluid, when the flushing fluid delivery unit (80) is activated, flows through the first grid (28), the reaction space (33) and the second grid (30) when the reactor (26) is introduced into the receiving space (22), characterized in that the receiving space (22) comprises a receiving section (24), into which the reactor (26) can be introduced between the reactor (26) and the receiving section (24) forming an intermediate space (58) which is closed at least in the radial direction, wherein a seal (60) is arranged in the receiving section (24), which seal interacts with the reactor (26) in the region of the first grid (28).Flushing device (78) according to claim 9, characterised in that a flushing fluid storage container (83) for holding the flushing fluid is arranged in the receiving space (22).Flushing device (78) according to one of Claims 9 or 10, characterized in that the device (10) has at least one flushing fluid discharge line (82) for discharging the flushing fluid from the receiving space (22).Drying device (84) for drying particulate solids (12), wherein the drying device (84) comprises: - at least one reactor (26) into which the particulate solids (12) can be introduced, wherein the reactor (26) ◯ has a first grid (28) and ◯ has a second grid (30), which delimit a reaction space (33) and retain the particulate solids (12) introduced into the reaction space (33) in the reaction space (33), and - at least one closable or closed receiving space (22) into which the reactor (26) can be introduced, - at least one suction unit (86) for conveying a drying fluid through the receiving space (22), wherein the receiving space (22) is configured such that the drying fluid flows through the first grid (28), the reaction space (33) and the second grid (30) when the suction unit is activated, when the reactor (26) is introduced into the receiving space (22).Drying device (84) according to claim 12, characterised in that the receiving space (22) comprises a receiving section (24), into which the reactor (26) can be introduced, forming an intermediate space (58), which is closed at least in the radial direction, between the reactor (26) and the receiving section (24).System for treating particulate solids (12), comprising - a first device (10 1) for treating particulate solids (12) according to one of Claims 1 to 8, - a second device (10 2) for treating particulate solids (12) according to one of Claims 1 to 8, - a first flushing device (78 1) for flushing the particulate solids (12) according to one of Claims 9 to 11, - a third device (10 3) for treating particulate solids (12) according to one of Claims 1 to 8, - a second flushing device (78 2) for flushing the particulate solids (12) according to one of Claims 9 to 11, - a drying device (84) for drying the particulate solids (12) according to one of claims 12 or 13, and - a transport device (34) for transporting the reactor (26) within the system.Method for treating particulate solids (12) with a device (10) according to one of Claims 1 to 8, comprising the following steps: - introducing the particulate solids (12) to be treated into the reaction space (33), - introducing the reactor (26) into the receiving space (22), - feeding a process fluid into the receiving space (22), - conveying the process fluid and a reaction mixture of the process fluid and the particulate solids (12) through the receiving space (22) in such a way that the process fluid and the reaction mixture flow through the first grid (28), the reaction space (33) and the second grid (30) when the conveying unit (42) is activated, and - coupling ultrasound into the reaction space (33) by means of the ultrasound device (62).Method according to claim 15, comprising the following steps: - determining the temperature of the reaction mixture in the receiving space (22) by means of a temperature determination unit, and - supplying a coolant into the receiving space (22) by means of the coolant line (54) if the determined temperature exceeds a limit value.Method according to one of claims 15 or 16, comprising the following steps: - supplying a flushing fluid into the receiving space (22) by means of a flushing fluid conveying line, and - conveying the flushing fluid through the receiving space (22) by means of a flushing fluid conveying unit (80) in such a way that the flushing fluid flows through the first grid (28), the reaction space (33) and the second grid (30) when the flushing fluid conveying unit (80) is activated.Method according to one of claims 15 or 16, comprising the following steps: - conveying a drying fluid through the receiving space (22) by means of a suction unit, wherein the receiving space (22) is configured such that the drying fluid flows through the first grid (28), the reaction space (33) and the second grid (30) when the suction unit is activated.Method according to claim 18, wherein, in the intended use of the device (10), the first grid (28) is arranged below the second grid (30) and the drying fluid flows through the reaction space (33) from the second grid (30) towards the first grid (28).Method for treating particulate solids (12) with a system according to claim 14, comprising the following steps: - introducing the reactor (26) into the receiving space (22) of the first apparatus (10 1) for treating particulate solids (12) by means of the transport device (34), and treating the particulate solids (12) with the first apparatus (10 1), - removing the reactor (26) from the receiving space (22) of the first apparatus (10 1), introducing the reactor (26) into the receiving space (22) of the second apparatus (10 2) for treating particulate solids (12) by means of the transport device (34), and treating the particulate solids (12) with the second apparatus (10 2), removing the reactor (26) from the receiving space (22) of the second device (10 2), introducing the reactor (26) into the receiving space (22) of the first flushing device (78 1) for flushing the particulate solids (12) by means of the transport device (34) and flushing the treated solids (12) by means of the first flushing device (78 1), - removing the reactor (26) from the receiving space (22) of the first flushing device (78 1), introducing the reactor (26) into the receiving space (22) of the third device (10 3) for treating particulate solids (12) by means of the transport device (34), and treating the particulate solids (12) by means of the third device (10), wherein ultrasound is coupled into the reaction space (33), - removing the reactor (26) from the receiving space (22) of the third device (10 3), introducing the reactor (26) into the receiving space (22) of the second flushing device (78 2) for flushing the particulate solids (12) by means of the transport device (34) and flushing the treated solids (12) by means of the second flushing device (78 2), - removing the reactor (26) from the receiving space (22) of the second flushing device (78 2), introducing the reactor (26) into the receiving space (22) of the drying device (84) for drying the particulate solids (12) by means of the transport device (34) and drying the treated solids (12) by means of the drying device (84), and - removing the reactor (26) from the receiving space (22) of the drying apparatus (84) by means of the transport device (34).

Citation Information

Patent Citations

  • multivalent laboratory reactor with reverse mixing

    DD281353B5

  • REACTOR WITH BACK MIXING FOR TESTING CATALYST FORMINGS

    DD265699A1

  • Automotive fuel cell, for use in gas filter system, comprises cold start-up droplet separator, adsorbent unit and oxidation stage within single housing

    DE10126665A1

  • horizontal reactor, especially for the production of methanol

    DE602004000055T2

  • DD000000265699A1