EP4514526A1 - Dispositif et procédé de fabrication de particules solides - Google Patents

Dispositif et procédé de fabrication de particules solides

Info

Publication number
EP4514526A1
EP4514526A1 EP23719789.2A EP23719789A EP4514526A1 EP 4514526 A1 EP4514526 A1 EP 4514526A1 EP 23719789 A EP23719789 A EP 23719789A EP 4514526 A1 EP4514526 A1 EP 4514526A1
Authority
EP
European Patent Office
Prior art keywords
reactor
solid particles
suspension
filtration apparatus
liquid
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP23719789.2A
Other languages
German (de)
English (en)
Inventor
Andreas Mueller
Volker Mathes
Denis Huertgen
Christoph ARIAANS
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
HTE GmbH the High Throughput Experimentation Co
Original Assignee
HTE GmbH the High Throughput Experimentation Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from DE202022102465.0U external-priority patent/DE202022102465U1/de
Application filed by HTE GmbH the High Throughput Experimentation Co filed Critical HTE GmbH the High Throughput Experimentation Co
Publication of EP4514526A1 publication Critical patent/EP4514526A1/fr
Pending legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B01J19/0066—Stirrers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
    • B01J2/06—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops in a liquid medium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/02—Feed or outlet devices; Feed or outlet control devices for feeding measured, i.e. prescribed quantities of reagents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/005—Separating solid material from the gas/liquid stream
    • B01J8/006—Separating solid material from the gas/liquid stream by filtration

Definitions

  • the invention relates to a device for producing solid particles from liquid starting substances with at least storage containers for the liquid starting substances, a reactor in which a suspension containing solid particles is formed by reaction of the liquid starting substances and at least one filtration apparatus for separating the solid particles from the suspension.
  • the invention further relates to a method for producing solid particles from liquid starting substances in such a device.
  • Solid particles are made from different materials and with different particle sizes and, if necessary, formed into flat or solid bodies after further processing steps and used.
  • Typical applications of such bodies made from solid particles in chemical process engineering are catalysts for heterogeneous catalysis, solid electrolytes (solid oxide ceramics) for fuel cells or electrolyzers, functionalized filter materials, electrically active catalyst materials for electrochemistry or for energy storage or pigment particle synthesis .
  • the solid particles are produced using different processes. Common processes for producing solid particles from solutions include precipitation reactions, spray drying or crystallization.
  • Solids differ in density from the density of the solution, which is a property used to separate them from the solution after producing the solids in the solution. Solids with a lower density than the solution will float and can be separated from the solution by flotation, solids with a greater density can be separated by sedimentation, filtration or by centrifugation. Solids with a higher density can be forced to flotation by gassing due to bubble adhesion, although this can also be an undesirable effect, for example if bubbles form during the reaction. In the latter case, bubble separation is required before solid separation.
  • toxic solutions containing heavy metals are often processed into toxic solids containing heavy metals.
  • solids cannot simply be cleaned off by rinsing, especially after sedimentation or by drying on walls, for example in empty pipes or menisci above dry inner container walls.
  • deposits must be removed by operating personnel wearing protective equipment. This approach is very resource-consuming and time-consuming both in production and in testing technology. After each new batch or each new test, the system must be completely freed from buildup so that the subsequent batch or test does not suffer from any contamination caused by the predecessor.
  • Standard laboratory isolation devices such as gloveboxes are poorly suited for continuous production processes due to the lock procedure and limited access to the devices. Complete clean rooms hinder system operation due to the necessary full protective suit.
  • Catalyst materials or storage materials that are made from toxic solutions containing heavy metals are, for example, also powdery oxidic materials, the production of which is of great economic and technical importance.
  • the development and optimization of the technical process conditions is of great interest, as the development and improvement of high-performance materials is seen as a solution to numerous current challenges in order to find new technologies that can help conserve resources better than with existing technologies .
  • WO-A 2015/040005 discloses the production of electrode materials based on mixed metal oxides that contain nickel, cobalt, manganese and also lithium. In addition, the materials also contain lithium and iron phosphate along with a divalent metal.
  • the starting components are first combined in a precipitation reactor. The resulting suspension is then fed into a spray dryer, in which the solid is separated from the suspension.
  • Processes for producing transition metal mixed oxides are known from WO-A 2014/180743 and WO-A 2016/071219, each of which initially uses spherical particles as a precursor of transition metal hydroxides, in which at least one aqueous solution of an alkali metal (hydrogen) carbonate or alkali metal hydroxide, and at least two aqueous solutions of transition metal salts are fed to a reactor in which mixed transition metal carbonates, transition metal hydroxides or transition metal carbonate hydroxides are precipitated and the precipitated particles are then separated.
  • WO-A 2014/180743 and WO-A 2016/071219 each of which initially uses spherical particles as a precursor of transition metal hydroxides, in which at least one aqueous solution of an alkali metal (hydrogen) carbonate or alkali metal hydroxide, and at least two aqueous solutions of transition metal salts are fed to a reactor in which mixed transition metal carbonates, transition metal hydroxides or transition metal carbonate hydroxides are precipit
  • a process for producing cobalt carbonate is known from CN-A 101376529, a process for producing hexaaluminate by a sol-gel process from EP-A 1 390 298 or a process for producing lithium carbonate from CN-A 106276988.
  • a device for producing solid particles from liquid starting substances comprising: at least two storage containers for the liquid starting substances, at least one reactor in which a suspension containing solid particles is formed by reaction of the liquid starting substances or solids are deposited on seeding surfaces or seeding bodies and when forming a suspension, at least one filtration apparatus for separating the solid particles from the suspension, the storage containers each being connected to the reactor via fluid connections and pumps being accommodated in the fluid connections with which liquid can be conveyed from the respective storage container into the reactor and the Reactor is connected to the filtration apparatus in such a way that the suspension formed in the reactor can flow into the filtration apparatus and all system components of the device are positioned in a closed housing.
  • particle growth depends essentially on the number of particles already formed, it can be useful to accelerate particle formation by introducing particles into at least one of the storage containers as so-called seeding (nucleating agent) on which the solid that forms can grow.
  • seeding particles can consist of the growing solid or another solid, which can then also be viewed as a carrier material for the growing material.
  • This storage container should have devices to prevent sedimentation of the particles.
  • components can also be inserted into the reactor as seeding surfaces or seeding bodies, so that a desired growth of layer sequences is created on them.
  • Bodies can have the size of conventional bulk bodies, for example a mean hydraulic diameter of 0.5 to 10 mm. If the bodies are to be removed as filter cakes, the size is limited to one that still allows hydraulic conveyance in pipelines.
  • seeding areas or seeding bodies can, for example, have sizes that are common on a laboratory scale and are used in electrolysis cells or fuel cells for laboratory studies. Typical areas for such laboratory applications are, for example, 1 cm 2 to 100 cm 2 .
  • the device according to the invention can also be used in industrial production.
  • the seeding areas or surfaces of the seeding bodies can usually have a size of up to 1 m 2 , preferably up to 0.5 m 2 . However, the areas can be even larger for use in even larger stacks.
  • seeding areas or seeding bodies must be removed directly from the reactor. Common reactors can be equipped with baffles near the inner wall of the reactor.
  • the growth can be supported electrochemically by applying a potential to the sheet connected as a cathode in a conductive electrolyte, similar to that in electroplating.
  • the layer thickness can be estimated using Faraday's law and is proportional to the current strength.
  • growth begins at crystal nuclei on the surface. Particles can also be treated in this way. Suitable geometries for seeding surfaces or seeding bodies on whose surface the crystal nuclei grow correspond, for example, to the geometry of Berty reactors.
  • the storage containers can preferably each be filled via an inlet, each inlet having a suitable interface on the housing to which a storage container with the starting substance for the corresponding storage container can be connected.
  • the storage containers are preferably connected to a vacuum pump, so that liquid starting substance can be sucked into the storage container via the inlet connected to the storage container by applying a negative pressure. Since the storage container is located within the closed housing, possible contact with the starting substances is prevented. By applying a negative pressure, it is also not necessary to use a pump in the supply line through which the starting substances are conveyed and which must be opened at least for maintenance purposes, whereby contact with the starting substances conveyed by the pump cannot be prevented.
  • gravimetric dosing is preferred, with the storage containers hanging on weighing cells.
  • the mass decrease in the storage container is recorded.
  • removal from the storage container is stopped.
  • continuous removal is also possible, in which case the decrease in mass of the storage container is continuously recorded and the delivery rate of the pump into the reactor is controlled via the decrease in mass of the storage container.
  • the storage containers are preferably dimensioned so large that a desired batch of the product can be produced with the starting substances presented in the storage containers and no starting substances have to be refilled during production.
  • the liquid starting substances react to form the solid particles, so that a suspension containing the solid particles is created.
  • the reaction can be carried out in just one reactor or in several reactors. If several reactors are used, they can be connected in parallel so that the reaction takes place in several reactors at the same time or alternatively as a reactor cascade so that the reaction starts in a first reactor and the reaction mixture generated is transferred to a further reactor in which the reaction continues. This is repeated until the reaction mixture has been introduced into the last reactor.
  • the use of a reactor cascade also enables, for example, a targeted addition of the starting substances if, for example, it is desired to supply different starting substances one after the other. A different starting substance or a different mixture of starting substances can be added to each reactor.
  • a stirred tank is used as the reactor.
  • the reactor is particularly preferably a continuous stirred tank reactor (CSTR). If several reactors are used as a reactor cascade, it is preferred if all reactors used in the reactor cascade are continuous stirred tank reactors. By using the stirred tank, the suspension formed in the reactor can be stirred continuously, the movement of the suspension preventing solid particles from precipitating and a deposit from forming on the reactor wall.
  • CSTR continuous stirred tank reactor
  • liquid is withdrawn from the reactor during the reaction, as described, for example, in WO-A 2014/180743.
  • the suspension is introduced into a filtration apparatus in which the solid particles collect as filter cakes on a filter and the liquid in the suspension is drawn off through the filter.
  • the filtration apparatus has a filter basket in which the solid particles collect as filter cake and which can be removed from the closed housing.
  • the filter basket can be removed either manually via a lock in the closed housing or automatically.
  • the filter basket in the form of a drawer, which is sealed in the housing during operation and can be pulled out of the housing for removal.
  • the filter cake containing the solid particles can then be sent for further processing, for example drying.
  • the filter cake and filter basket are sent for further processing and a new, clean filter basket is inserted into the filtration apparatus.
  • the filter cake can then be removed from the filter basket and the filter basket cleaned so that it can then be reinserted.
  • a sample changer that holds the filter basket.
  • the sample changer contains empty filter baskets, so that an empty filter basket can be inserted into the filtration apparatus immediately after a filter basket containing the solid particles has been removed. This can then be repeated until all empty filter baskets have been used and the sample changer only contains full filter baskets.
  • the filter baskets containing the solid particles or the entire sample changer can then be removed from the housing, for example via a lock, and the sample changer can be equipped with empty filter baskets.
  • a sample changer it can alternatively be designed in such a way that it includes a removal area outside the housing, so that the filter baskets filled with solid particles are automatically transported through a suitable lock into the removal area located outside the housing.
  • the filled filter baskets can be removed and replaced with empty filter baskets, which are then transported into the housing via the same lock or another lock.
  • a suitable sample changer includes, for example, a carousel that holds the filter baskets. In this case, either the entire carousel can be positioned in the housing, in which case the carousel is removed when it is equipped with filter baskets filled with solid particles, then the filled filter baskets are removed and replaced by empty filter baskets and the carousel is then reinserted becomes.
  • the carousel in such a way that it includes a removal area outside the housing, so that the filter baskets filled with solid particles can be transported out of the housing through a lock and removed from the carousel, empty filter baskets outside the Housing can be placed on the carousel and these can be moved back into the housing through a second lock so that they can then be used later in the filtration apparatus.
  • the filter basket is preferably constructed in such a way that the bottom of the filter basket forms the filter and the side walls of the filter basket are impermeable.
  • a sintered frit is particularly preferably used as a filter.
  • the filter basket has a lid which opens automatically when the filter basket is inserted into the filtration apparatus and closes automatically when the filter basket is removed from the automatic filtration machine .
  • the pressure difference required for filtration is preferably generated by connecting the filtration apparatus to a vacuum pump.
  • the vacuum pump is connected to the suction side of the filter basket so that the suspension is sucked towards the filter basket and the filtrate is sucked through the filter basket. It is particularly preferred here if both for generating the pressure difference for the filtration and for sucking in the output Only a vacuum pump is used to transfer substances from the storage containers to the storage containers.
  • the vacuum pump is connected to the storage containers and the filtration apparatus, for example via a multi-way valve, and depending on the desired process, i.e. carrying out the filtration or supplying starting substance, the multi-way valve is switched accordingly.
  • the filter cake can be removed directly from the filtration apparatus or can be rinsed with a rinsing liquid before removal in order to remove any remaining reactants, which can lead to an undesirable after-reaction, or other liquid contaminants on the solid.
  • a stirring element is preferably included in the filtration apparatus.
  • the stirring element preferably has an inclined blade stirrer which is positioned in the filter basket.
  • stirrer blades of the inclined blade stirrer are only a very small distance from the bottom of the filter basket or even come into contact with the bottom of the filter basket.
  • the distance between the stirrer blades and the inclined blade stirrer is preferably in the range of 0 to 10 mm, more preferably in the range of 0.5 to 5 mm and in particular in the range of 1 to 2 mm.
  • the stirrer preferably has a further stirring element, for example in the form of an anchor stirrer, which is arranged above the inclined blade stirrer.
  • the stirrer is set in motion so that the filter cake swirls up and the solid particles come into contact with the rinsing liquid. After a predetermined rinsing time, a pressure difference is generated again, in particular by applying a negative pressure on the filtrate side, and the rinsing liquid is thus sucked out through the filter. A new filter cake is formed from the cleaned solid particles, which can then be removed as a product from the filtration apparatus. If a single rinse cycle is not sufficient, it is possible to carry out additional rinse cycles before the filter cake is removed from the filtration apparatus.
  • the filter cake contains the product and must be regularly removed from the filtration apparatus, it is necessary to regularly interrupt the filtration for the removal of the filter cake and, if the filter cake is rinsed before removal, also for rinsing.
  • a buffer container is arranged between the at least one reactor and the filtration apparatus, so that the suspension is first passed from the reactor into the buffer container and from the buffer container into the filtration apparatus. If a reaction is carried out in which a post-reaction is required or the particles are removed before separation The suspension still needs to age, the buffer container can also be used to carry out these processes.
  • the buffer container includes a stirrer with which the suspension can be kept in motion.
  • the stirrer used is particularly preferably an axially conveying stirrer, for example an inclined blade stirrer.
  • the at least one reactor, the buffer container and the filtration apparatus are arranged one above the other in such a way that the suspension Gravity-driven can flow from the reactor into the buffer container and further from the buffer container into the filtration apparatus and so no pumps are needed to convey the suspension.
  • the at least one reactor possibly the buffer container and the filtration apparatus, includes rinsing nozzles with which drying occurs on interior walls can be prevented.
  • the rinsing nozzles can be used to spray a rinsing liquid onto the inner walls, which can be used to wash away any buildup.
  • the use of rinsing nozzles also allows the walls of the apparatus to be kept moist during operation, for example by spraying solvent, which is also contained in the starting substances, against the walls. In this way, it is possible to prevent deposits from forming on the walls of the apparatus at the liquid meniscus at the liquid interface.
  • the rinsing liquid is sprayed against the walls under pressure from the rinsing nozzles.
  • the rinsing nozzles are axially movable and can thus be moved from top to bottom and back within the apparatus to be cleaned.
  • rotating nozzles are used as rinsing nozzles. The entire rinsing process is preferably fully automated. carried out automatically, so that it is not necessary to employ operating personnel directly at the devices.
  • vortex nozzles are arranged at the outlet of the at least one reactor and optionally the buffer container, with which a shear force can be introduced into the suspension.
  • the use of the vortex nozzles allows solid particles to sink downwards in the container, so that the suspension is thickened in the area of the drain, which is preferably arranged at the bottom of the container, but the particles are kept in motion by the vortices generated, so that they move do not accumulate on the floor or walls of the respective apparatus.
  • a rinsing liquid In addition to spraying the walls with a rinsing liquid, it is also possible to flood the containers with a rinsing liquid and to move it in the containers, for example by stirring or using the vortex nozzles. The flushing liquid is then withdrawn through the filtration apparatus and can be analyzed to determine cleaning progress. Removing the rinsing liquid through the filtration apparatus offers the further advantage that the rinsed solid is collected as a filter cake in the filter basket and, provided it is not contaminated and meets the required specifications, can also still be recovered as a product. On the other hand, even if the cleaned solid can no longer be used, the rinsing liquid can be used for another rinsing cycle.
  • sensors are included with which the cleaning can be monitored.
  • Suitable sensors for monitoring cleaning include measuring the conductivity of the draining filtrate or the use of cameras with which images of the cleaned surfaces are recorded and which are evaluated using suitable image capture or, alternatively, are monitored by operating personnel.
  • flushing nozzles and vortex nozzles in conjunction with the sensors to monitor cleaning, it is possible to operate the system over a longer period of time and also to carry out several different reactions without having to open the housing, so that the operating personnel are not exposed to the im Substances used or produced in the process are avoided.
  • the process control in the device for producing solid particles is intensified. This can be done in particular by making targeted use of the sedimentation in the containers, for example the reactor or the buffer container, by adjusting the shear rate through active flow movement, for example through stirring or the use of vortex nozzles, so that solid sedimentation without particle movement is prevented but loose sedimentation with particle movement is possible.
  • differential velocities can be generated between the solution and the solid particles, which keep the solid particles in suspension, whereby the residence time of the solid particles can be set separately from the residence time of the solution in which the solid particles move.
  • the structure of the solid particles can be specifically influenced and the solids content in the solution and thus the process yield can be increased. Layer sequences on the solid particles are also possible by metering the different starting substances in sections.
  • the particle size and the particle size distribution which can be characterized, for example, by a size distribution sum curve, can be set in a feedback loop.
  • the solid particles are measured, for example, directly in the reactor with a probe or in a flow cell in a reactor circulation or at a point after the reactor, and the starting substances, the pH value, the temperature and / or the stirrer speed are adjusted accordingly.
  • the torque on the stirrer drive is measured. This provides an indication of the stirring energy introduced, which must not be exceeded.
  • a valve can also be provided at the outlet of the buffer container, with which either the connection to the filtration apparatus or the connection to a sample vessel can be opened.
  • a sample changer is used for sampling.
  • This is preferably constructed as described above for the sample changer for the filter baskets.
  • the sample changer is particularly preferably a carousel, which can either be completely removed from the housing after all sample vessels have been filled or which in particular includes a removal area outside the housing, so that filled sample vessels are transported with the carousel out of the housing through a first lock and empty Sample containers can be transported back into the housing through another lock, so that regular sampling is possible without opening the housing and more samples can be taken than the carousel has spaces for sample containers.
  • valve for sampling it can preferably always be switched so that the outlet from the reactor or the buffer container can be closed. Even if no sampling is provided, a valve or a tap is preferably included with which the outlet from the reactor and the buffer container can be closed.
  • a flushing nozzle with which the valve or the tap can be flushed.
  • the rinsing is carried out every time the reactor or the buffer container is completely emptied in order to avoid that the rinsing solution used for rinsing gets into the suspension. If the liquid phase of the suspension can be used as the rinsing solution, it is also possible, if necessary, to rinse if the reactor or the buffer container are not completely emptied, since in this case no unwanted components can get into the suspension.
  • sampling is designed in such a way that the sample containers are automatically closed after the sample has been taken and can then be removed from the housing for analysis via a suitable lock.
  • the device according to the invention and the method according to the invention are preferably used for the production of catalyst materials or electrode materials. These often use acids or alkalis as starting substances and the solid particles produced are often toxic.
  • the storage containers, the reactor and connecting lines are made of a material that is chemically inert to the liquid starting substances and substances formed in the production of the solid particles, or are coated with such a material.
  • the storage containers, the at least one reactor and the buffer container are preferably made of glass.
  • the containers are also possible to make the containers from a plastic that is inert to the starting substances or to make them from steel or stainless steel and coat them with a coating made from a material that is inert to the starting substances, for example a suitable plastic or enamel.
  • the connecting lines are preferably pipes or hoses made of a plastic that is inert to the starting substances used, for example made of polytetrafluoroethylene (PTFE), polyether ether ketone (PEEK), polypropylene (PP), polyethylene (PE) or mixtures thereof and particularly preferably made of PTFE.
  • PTFE polytetrafluoroethylene
  • PEEK polyether ether ketone
  • PP polypropylene
  • PE polyethylene
  • Pumps that are used to convey the starting substances or also to convey the suspension containing the solid particles or intermediate products are preferably peristaltic pumps or diaphragm pumps, whereby the hoses of the peristaltic pump or the membrane of the diaphragm pump are also made of polymers that are inert to the starting materials used. The same polymers can be used here as described above for the connecting lines.
  • Figure 1 is a schematic representation of a device according to the invention for producing solid particles
  • Figure 2 shows a buffer container as used in the device for producing solid particles
  • Figure 3 shows a filtration apparatus as used in the device for producing solid particles
  • Figure 4 shows a stirrer used in the filtration apparatus.
  • a device 1 for producing solid particles from liquid starting substances comprises several storage containers 3.1, 3.2, in which the liquid starting substances are placed, with a starting substance being kept in each storage container 3.1, 3.2, so that the number of storage containers 3.1, 3.2 depends on the number of depends on liquid starting substances.
  • the storage containers 3.1, 3.2 can each be connected via a connecting line 5.1, 5.2 to a storage container 7.1, 7.2, in which the respective starting substance is stored.
  • a negative pressure is applied to the storage containers 3.1, 3.2, through which the respective starting substance is conveyed from the storage container 7.1, 7.2 into the storage container 3.1, 3.2.
  • they are connected to a vacuum pump 9.
  • a valve 11 is provided, which can be switched so that the negative pressure is only applied to the storage container 3.1, 3.2 that is to be filled. If several storage containers 3.1, 3.2 are to be filled, this is preferably done one after the other, so that only one storage container 3.1, 3.2 is filled at a time. This allows a vacuum pump 9 with a lower delivery rate to be used. In addition, more precise filling of the storage containers 3.1, 3.2 is possible in this way.
  • the connecting lines 5.1, 5.2 each open into the upper area, preferably above the maximum specified filling level, into the storage container 3.1, 3.2.
  • the starting substances are fed into a reactor 13 from the storage containers 3.1, 3.2.
  • the liquid starting substances react to form solid particles, so that a suspension is formed in the reactor 13.
  • each storage container 3.1, 3.2 is suspended from a weighing cell 15.1, 15.2.
  • the load cells 15.1, 15.2 allow gravimetric metering of the liquid starting substances into the reactor 13.
  • the individual starting substances can be introduced into the reactor 13 in an individually controlled manner.
  • the control is preferably carried out automatically using a suitable control device, for example control software running on a computer 17.
  • the reactor preferably has a mixing device, for example a stirrer 19.
  • the reactor 13 is a continuous stirred tank reactor (CSTR) or a reactor cascade made up of several reactors connected in series, with each reactor in the reactor cascade preferably being a CSTR in this case too.
  • CSTR continuous stirred tank reactor
  • the suspension produced in the reactor is continuously withdrawn via an outlet line 21 and passed into a buffer container 23.
  • the suspension is then fed from the buffer container 23 to a filtration apparatus 25, in which the solid particles are separated from the suspension.
  • the buffer container 23 also serves in particular as a buffer for the continuously supplied suspension, which is then removed in batches from the buffer container 23 and fed to the filtration apparatus 25.
  • the buffer container 23 can also be used to give the solid particles sufficient time for a subsequent reaction, for example if the reaction is slow and the residence time in the reactor 13 is not sufficient to achieve complete conversion of the starting substances.
  • the buffer container 23 comprises a stirrer 27 with which the suspension is stirred and the solid particles are kept moving in the liquid phase.
  • a sample line 29 branches off from the drain line 21. Samples can be taken via the sample line 29 and fed to an analysis unit 31. It is particularly preferred if the sample line 29 is connected to the drain line 21 with a valve, the valve closing the sample line 29 and opening the drain line during normal operation and closing the drain line 21 and opening the sample line 29 to take a sample. In this valve position, a sample is taken and then the valve is switched again so that the drain line 21 is opened and the sample line 29 is closed. The system then switches again briefly to take another sample.
  • the individual samples taken via the sample line 29 are preferably each introduced into a sample vessel 33, with a new sample vessel 33 being used for each sample.
  • the sample vessels 33 are located, for example, on a carousel 35, which rotates one step further after a sample has been removed and positions the next, empty sample vessel 33 under the sample line 29.
  • the samples contained in the sample vessels 33 can either be evaluated automatically or the holder with the filled sample vessels 33 is removed and replaced with a new holder with sample vessels 33 as soon as all sample vessels 33 are filled.
  • the analysis of the samples contained in the sample vessels 33 can also be carried out on a separate analysis unit.
  • the solid particles are separated from the suspension in the filtration apparatus 25.
  • a pressure difference is applied by connecting the filtrate side to a vacuum pump 37.
  • the device 1 comprises only one vacuum pump, whereby the one vacuum pump is used both to generate the pressure difference for filtration and to generate the negative pressure in the storage containers 3.1, 3.2.
  • the filtrate side of the filtration apparatus 25 is not connected to a separate vacuum pump 37 as shown here, but to the vacuum pump 9 via the valve 11. The valve 11 can then be switched in such a way that either a negative pressure is applied to one of the storage containers 3.1, 3.2 or on the filtrate side of the filtration apparatus 25.
  • the liquid phase of the suspension is sucked through a filter in the filtration apparatus 25, so that the solid particles collect as filter cakes on the filter and the liquid phase can be removed as a filtrate.
  • the filter is designed as the bottom of a filter basket and the filter basket can be removed from the filtration apparatus together with the filter cake.
  • the filter cake can be washed before removal from the filtration apparatus.
  • the filter cake is mixed with a rinsing liquid, which can be removed again as a filtrate after the rinsing process.
  • the filtration apparatus preferably also has a stirrer 39.
  • the rinsing liquid is preferably held in a storage container 40, as shown here.
  • all components of the device 1 except for the storage containers 7.1, 7.2 and the computer 17 are arranged inside a closed housing 41.
  • the housing 41 In order to access the components arranged in the housing 41 if necessary, for example if replacement or maintenance is required, the housing 41 preferably has an access that can be closed gas-tight and liquid-tight.
  • the gases removed from the process via the vacuum pumps 9, 37 and possibly other exhaust gases generated in the process can preferably be removed via an exhaust gas outlet 43 on the housing 41, the exhaust gas outlet 43 being connected to an exhaust gas cleaning system in order to prevent gaseous hazardous substances from being released are withdrawn from the housing 41 and can reach the environment.
  • these containers preferably each have at least one flushing nozzle, which is arranged above the maximum liquid level and through which a rinsing liquid can be sprayed onto the walls of the containers in order to form a liquid film on them and thus prevent solid particles from being deposited at the interface of the liquid in the respective container.
  • flushing nozzle which is arranged above the maximum liquid level and through which a rinsing liquid can be sprayed onto the walls of the containers in order to form a liquid film on them and thus prevent solid particles from being deposited at the interface of the liquid in the respective container.
  • vortex nozzles are also included, with which the liquid in the containers can be kept moving in order to avoid deposits.
  • the system components can be cleaned automatically; for this purpose, for example, liquid can be sprayed under pressure onto the inner walls of the containers via the rinsing nozzles in order to remove possible deposits.
  • liquid can be sprayed under pressure onto the inner walls of the containers via the rinsing nozzles in order to remove possible deposits.
  • the same rinsing liquid can be used to clean the system components as for cleaning the filter cake, this is preferably also taken from the storage container 40, which is connected not only to the filter apparatus but also to the reactor 13.
  • Figure 2 shows a buffer container 23 as it can be used in the device shown in Figure 1.
  • the suspension is introduced from the reactor 13 into the buffer container 23 via an inlet 43.
  • the suspension is kept in motion with the stirrer 27 in order to prevent solid particles from precipitating out of the suspension and forming an undesirable deposit on the inner walls 45 of the buffer container 23.
  • Any suitable stirrer can be used for this purpose, with the stirrer particularly preferably being an axially conveying stirrer.
  • Axial-acting inclined blade stirrers are particularly suitable.
  • a rinsing line 49 preferably opens at the outlet 47, through which rinsing liquid can be introduced into the buffer container 23 from below in order to be able to rinse it after a batch has been completed.
  • a sample line can also branch off from the outlet 47. Samples can be taken via the sample line in order to analyze the suspension removed from the buffer container 23 before it is fed to the filtration apparatus 25.
  • Figure 3 shows a filtration apparatus 25 such as can be used in the device 1 according to the invention for the production of solids.
  • the filtration apparatus 25 is filled with the suspension to be separated via an inlet line 51.
  • the inlet line 51 is generally the line that is connected to the outlet 47 of the buffer container 23, so that the suspension can be passed from the buffer container 23 into the filtration apparatus 25.
  • the filtration apparatus 25 can be operated continuously or batchwise, with batch operation being preferred.
  • the filtration apparatus 25 is filled with the suspension and a negative pressure is applied on the filtrate side, i.e. below a filter 53.
  • the filtrate side is connected to the vacuum pump 37.
  • a pressure difference is created, through which the liquid phase of the suspension is drawn through the filter 53.
  • Those contained in the suspension Solid particles collect on the filter 53 and form a filter cake.
  • the liquid phase is removed from the filtration apparatus as a filtrate via an outlet 55 and can be sent for processing if sensible processing of the filtrate is possible.
  • the filtrate can also be disposed of appropriately.
  • a moist filter cake which still contains residues of the liquid phase, remains on the filter 53. Since the liquid phase can still contain starting substances and in particular starting materials, it is necessary to rinse the solid particles remaining as filter cake in order to remove the residues of the liquid phase.
  • the outlet 55 is closed with a valve 57 after all of the filtrate has been withdrawn.
  • a rinsing liquid is then introduced into the filtration apparatus 25 via a rinsing line 59. With the help of the stirrer, the filter cake formed on the filter 53 is whirled up again so that all solid particles come into contact with the rinsing liquid and the remaining liquid phase of the suspension can be washed off.
  • the stirring is stopped again and the valve 57 is switched so that negative pressure can be applied to the filtrate side again.
  • the rinsing liquid is removed as a filtrate and the rinsed solid particles remain on the filter 53 as a cleaned filter cake. If it is not possible to rinse the entire liquid phase of the suspension from the solid particles in one rinse, the rinse process can be repeated once or several times.
  • the rinsing liquid is analyzed for residues of the starting substances after the end of a rinsing cycle.
  • a probe is preferably placed at the outlet 55 of the rinsing liquid from the filtration apparatus 25, with which the rinsing liquid can be analyzed for residues.
  • Suitable probes are, for example, probes for measuring conductivity in the rinsing liquid. A low conductivity is then an indication of a low load of metal salts.
  • the filter 53 is a bottom of a filter basket 58, which can be removed together with the filter cake formed on the filter 53.
  • the walls of the filter basket 58 are preferably impermeable and only the bottom of the filter basket 58 acts as a filter 53.
  • the filtration is repeated until the filter cake has reached a desired height.
  • continuous filtration suspension is added until the filter cake has reached the desired height.
  • batch filtration after the liquid phase of a batch has been drawn off, suspension is fed in again, the liquid phase is drawn off and this is repeated until the filter cake reaches the desired height height has reached. If the filter cake is to be rinsed, it is preferably only rinsed when the filter cake is filtered, even with batch filtration has reached the desired height, otherwise the already cleaned solid particles from the previous filtrations will be contaminated again with the liquid phase.
  • a lower fill level sensor 61 is preferably provided, which is arranged in such a way that the desired height of the filter cake can be detected. Furthermore, it is preferred if a second fill level sensor 63 is included, with which the desired fill level of the suspension or the rinsing liquid can be detected when the filtration apparatus 25 is filled with the suspension or the rinsing liquid. With an upper fill level sensor 65, the maximum permissible fill level can be detected in order to prevent the filtration apparatus from being overfilled.
  • the lower level sensor 61 can also be used to set a lower level of the suctioned cleaning liquid. This can prevent the filter cake from drying too early between the cleaning steps.
  • a supply line 67 is provided for a cleaning liquid. This can be used to flood the filtration apparatus for cleaning.
  • the filtration apparatus 67 is preferably filled to the maximum filling level, which is detected by the upper filling level sensor 65.
  • the cleaning liquid is then set in motion in the filtration apparatus with the aid of the stirrer 39 and, if necessary, vortex nozzles (not shown here), so that the contaminants are washed off the walls of the filtration apparatus 25 with the shear forces generated.
  • Solid impurities are then caught in the filter basket and, if it is still a usable product, can be further processed and used as a product. Alternatively, the solid impurities are removed using the filter basket and disposed of.
  • a stirrer 39 is preferably used, as shown in Figure 4.
  • the stirrer 39 preferably has stirrer blades 69 set at an angle to the horizontal at the lower end, so that the lower part of the stirrer 39 is an inclined blade stirrer.
  • the stirrer blades 69 are preferably only a small distance above the filter 53 or even touch the filter 53.
  • the solid particles that are located directly on the filter 53 are scraped off by the filter and can therefore also be washed around and cleaned evenly with the rinsing liquid.
  • there is another stirring element 71 above the stirrer blades 69 forming the inclined blade stirrer which is preferably an anchor stirrer as shown here. This achieves an even mixing of the solid particles with the rinsing liquid.
  • the stirrer is stopped again so that filtration can take place. As soon as the solid particles have been cleaned and the filter basket 58 with the filter cake is to be removed from the filtration apparatus 25, the stirrer is moved upwards if the filter basket 58 is to be removed from the side of the filtration apparatus 25. When removing the filter basket 58 downwards from the filtration apparatus 25, it is not necessary

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)

Abstract

L'invention concerne un dispositif de fabrication de particules solides à partir de substances de départ liquides, le dispositif comprenant : au moins deux contenants de stockage (3.1, 3.2) pour les substances de départ liquides ; au moins un réacteur (13) dans lequel est formée une suspension contenant des particules solides ou des solides sont déposés sur des surfaces d'ensemencement ou des corps d'ensemencement par réaction des substances de départ liquides ; et, si une suspension est formée, au moins un appareil de filtration (25) pour séparer les particules solides de la suspension. Les contenants de stockage (3.1, 3.2) sont chacun reliés au réacteur (13) par l'intermédiaire de liaisons fluidiques, et des pompes sont logées dans les liaisons fluidiques, au moyen desquelles des pompes peuvent être pompées à partir du contenant de stockage pertinent (3.1, 3.2) et dans le réacteur (13), et le réacteur (13) est relié à l'appareil de filtration (25) de telle sorte que la suspension formée dans le réacteur (13) peut s'écouler dans l'appareil de filtration (25). Tous les composants du système (1) sont positionnés dans un boîtier fermé (41). L'invention concerne également un procédé de fabrication de particules solides dans un tel dispositif.
EP23719789.2A 2022-04-29 2023-04-20 Dispositif et procédé de fabrication de particules solides Pending EP4514526A1 (fr)

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EP22170961 2022-04-29
DE202022102465.0U DE202022102465U1 (de) 2022-04-29 2022-05-05 Vorrichtung zur Herstellung von Feststoffpartikeln
PCT/EP2023/060349 WO2023208742A1 (fr) 2022-04-29 2023-04-20 Dispositif et procédé de fabrication de particules solides

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CN118079537B (zh) * 2024-04-19 2024-07-09 厦门紫京科技有限责任公司 一种三元前驱体浓缩机构
CN119793377B (zh) * 2025-03-13 2025-08-08 富祥(山东)新材料有限公司 一种对硝基苄醇制备方法与装置

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WO1997041954A1 (fr) 1996-05-06 1997-11-13 Institute Of Geological & Nuclear Sciences Limited Fabrication et recuperation de sols de silice monodispersee a partir d'une saumure geothermique
DE60223016T2 (de) 2001-05-23 2008-07-17 Ecaps Ab Sinterbeständiges katalysatormaterial und verfahren zu dessen herstellung
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