Reactor system and method for manufacturing and / or processing particles

Abstract

The present invention relates to a reactor system (1) and method for manufacturing and / or processing particles (P) in a vibrating process gas stream.

Description

Technical Field

[0001] This invention relates to a reactor system for manufacturing and / or processing particles in a vibrating process gas flow. The reactor system includes reactor units having a pre-process gas supply unit and a post-process gas outlet unit. Each reactor unit has at least one reactor, comprising a reaction chamber for manufacturing and / or processing particles and a feeding device for introducing raw materials into the reaction chamber. Process gas flowing through the reactor unit along the direction of the process gas outlet unit can be supplied to the reactor unit via the process gas supply unit. The reactor system includes a pulsation device suitable for generating pulsations of the process gas, wherein the pulsation device can apply a pulsation frequency and a pulsation pressure amplitude to the process gas. The reactor system, which has a static process gas pressure that is particularly adjustable, is configured as an acoustic resonator having an inherent resonant frequency that defines a corresponding resonant state. The process gas can form a resonant gas column in the reactor system, such that the resonator can be excited by the pulsation frequency and / or pulsation pressure amplitude of the pulsation generated by the pulsation device. In the resonant state, the pulsation can be amplified into a resonant vibration of the process gas with a resonant frequency and a resonant pressure amplitude. The process gas supply unit and the process gas outlet unit each include a pressure loss generating device that generates pressure loss, wherein the pressure loss generating device is configured such that one of the resonant states can be selectively adjusted.

[0002] Furthermore, the present invention relates to a method for manufacturing and / or processing particles in a vibrating process gas flow, comprising a reactor system having reactor units, each reactor unit having a pre-process gas supply unit and a post-process gas outlet unit, each reactor unit having at least one reactor, each reactor including a reaction chamber for manufacturing and / or processing particles and a feeding device for introducing raw materials into the reaction chamber, wherein process gas flowing through the reactor unit in the direction of the process gas outlet unit is supplied to the reactor unit via the process gas supply unit, and the reactor system includes a pulsation device suitable for generating pulsations of the process gas, wherein the process gas is subjected to pulsations by means of the pulsation device. The reactor system, which has a particularly adjustable static process gas pressure, is configured as an acoustic resonator with an inherent resonant frequency that defines a corresponding resonant state. The process gas in the reactor system forms a resonant gas column, thereby exciting the resonator through the pulsating frequency and / or pulsating pressure amplitude generated by the pulsating device, and amplifying the pulsation into a resonant vibration of the process gas with a resonant frequency and resonant pressure amplitude in the resonant state. The process gas supply unit and the process gas outlet unit each include a pressure loss generating device that generates pressure loss, wherein the pressure loss generating device is configured such that one of the resonant states can be selectively adjusted. Background Technology

[0003] Reactor systems and methods for producing and / or processing particles, preferably fine particles with an average particle size of 1 nm to 5 mm, especially nano-sized or nanocrystalline particles, in vibrating process gas streams are known from the prior art.

[0004] A reactor system constructed as an acoustic resonator is known, in which the vibration or pulsation of a process gas is used to generate resonance. This resonance, in particular, affects acoustic properties, material properties (e.g., in multiphase systems), and thermal properties (e.g., influencing heat transfer) by means of mechanical forces and / or residence time variations in the process gas, and can be advantageously applied for various purposes. Such acoustic resonators are, for example, cavity resonators, especially Helmholtz resonators, which have inherent resonant frequencies that define the resonant state. Here, resonant vibrations can be generated in different ways and are affected in terms of their resonant frequency and resonant pressure amplitude.

[0005] For the quality of resonant vibrations in a reactor system, the type of resonant vibration generated, the geometry of the reactor system that can utilize the resonant vibrations, the adjustability of the resonant frequency and / or resonant pressure amplitude in the reactor system, the material properties of the process gas (which are especially determined by the temperature and static pressure of the process gas), and the reaction on the reactor system itself play important roles.

[0006] German patent application DE 10 2015 005 224 A1 discloses a method for precisely adjusting or readjusting the vibration amplitude of static pressure and / or hot gas velocity in a vibrating furnace apparatus (Schwingfeueranlage) with or without thermal material processing / material synthesis, the apparatus having at least one burner by means of which vibrating (pulsating) flames are generated, and the apparatus having at least one combustion chamber (resonator) into which the flame is directed. Typically, the amplitude (vibration intensity) of the pulsating hot gas flow caused by self-excited, feedback combustion instability in a vibrating furnace or pulsating reactor cannot be selectively and independently adjusted, and therefore cannot be adapted to the selected reactor throughput (in the case of material processing / material synthesis: e.g., reactant feed rate or product rate) without simultaneously, but undesirably, changing other process parameters (processing temperature, residence time, or processing time) and the resulting material characteristics. Nevertheless, to achieve this, it is proposed to connect a vibrating volume utilizing the flow of air, fuel, or a fuel-air mixture upstream of the burner outlet into the burner's supply line. Preferably, its size is infinitely adjustable. This allows for variation of the vibration amplitude.

[0007] German patent application DE 10 2015 006 238 A1 discloses a method and apparatus for the thermal treatment or conversion of materials, particularly large granular materials, in a pulsating hot gas flow, wherein the frequency and amplitude of the velocity or static pressure vibrations of the hot gas flow in a vertically arranged reaction chamber can be adjusted independently of each other. The raw material particles introduced at the upper end of the vertically arranged reaction chamber, due to their shape, mass, and density, cannot be pneumatically transported by the hot gas flow when adjusting the average flow velocity, but instead descend against the flow direction. During this descent time of approximately 1 to 10 seconds, the material is heat-treated into the desired product, which is then removed from the reactor at the lower end of the reaction tube by means of a gate system.

[0008] German patent application DE 10 2016 002 566 A1 discloses a method and apparatus for heat-treating raw materials. The apparatus includes a combustion chamber in which a periodically unstable vibrating flame burns to generate a pulsating exhaust gas flow that passes through a reaction chamber connected to the combustion chamber. To achieve efficient processing of the raw materials, an insert with a reduced cross-sectional area relative to the reaction chamber, through which the exhaust gas flow passes, is proposed. This insert has a length shorter than the total length of the reaction chamber. In particular, the length of the insert and the geometry of the combustion chamber can be varied, allowing the apparatus to have two resonators that can coordinate with each other.

[0009] German patent application DE 10 2018 211 650 A1 relates to an apparatus for producing particles, particularly fine particles, especially nanoscale or nanocrystalline particles, from at least one raw material. The apparatus includes at least one burner and a combustion chamber coupled to the burner for generating a pulsating flow of hot gas, a reaction chamber section subsequently positioned within the combustion chamber, and at least one pressure assembly for adjusting resonant characteristics and thus the sound pressure within the combustion chamber and / or the reaction chamber section.

[0010] The technical solutions known from the prior art all have the following drawbacks: the resonant frequency and / or resonant pressure amplitude of the resonant vibration of the process gas can only be varied by adapting the geometry of the reactor system, which is constructed as an acoustic resonator, and thus the volume of the process gas in the resonant gas column constructed in the reactor system. Summary of the Invention

[0011] Therefore, the object of the present invention is to provide a reactor system and method for manufacturing and / or processing particles in a vibrating or pulsating process gas flow, which achieves adjustment of the resonant frequency and / or resonant pressure amplitude of the resonant vibration of the process gas independently of the geometry of the reactor system configured as an acoustic resonator and thus the volume of the process gas in the resonant gas column configured in the reactor system.

[0012] This objective is achieved in reactor systems of the type mentioned at the beginning by configuring the pulsation device such that the pulsation frequency and / or pulsation pressure amplitude are matched with one of the inherent resonant frequencies of the resonator, thereby achieving a selected resonant state. By such targeted matching of the pulsation frequency and / or pulsation pressure amplitude by the pulsation device, the system capable of vibrating the resonator can be excited, and thus the heat transfer and mass transfer characteristics of the preferred hot process gas in the reactor system can be improved.

[0013] The additional pressure loss caused by the pressure loss generating device, based on the acoustic characteristics of the resonators in the vibration system, corresponds to the resonant pressure amplitude of the resonant vibration of the process gas excited by the pulsation device. The pressure loss generating device geometrically restricts the vibration system of the reactor system under operating conditions, both in terms of the volume of the process gas in the constructed, resonant gas column. Thus, while keeping the vibration system of the reactor system geometrically constant and the volume of the process gas in the constructed, resonant gas column constant within the reactor system, pulsation can be applied to the process gas using the pulsation device, thereby exciting the vibration system in the reactor system and amplifying the resonant vibration of the process gas with its resonant frequency and resonant pressure amplitude.

[0014] Therefore, the essence of a pressure loss generating device lies in: geometrically restricting the reactor system, allowing process gas flow through the reactor system, while simultaneously preventing resonant vibrations from propagating beyond the pressure loss generating device, thereby constructing a defined, vibratory system within the reactor system. The more restricted the vibratory system, the more efficient the generation and propagation of resonant vibrations within it. This is achieved through a defined, vibratory system where the excitation and propagation of resonant vibrations can be continuously, and especially periodically, generated and adjusted with reasonable technology and energy consumption in terms of their resonant frequency and / or resonant pressure amplitude.

[0015] According to an advantageous design of the reactor system, the pulsation device is configured as a flameless pulsation device. The pulsation device is preferably configured as a compression module, especially a piston, or as a rotary slider (Drehschieber) or a modified rotary gate (Drehschleuse). The flameless pulsation device is characterized by not being based on a combustion process that applies pulsation to the process gas. In particular, the pulsation is not generated by the pulsating process gas flow caused by the self-excited, feedback combustion instability of a periodically unstable combustion process. Therefore, (compared to combustion process-based pulsation devices) the pulsation frequency and / or pulsation pressure amplitude can be adjusted or adapted, and any, defined, vibratory system can be excited into resonant vibration.

[0016] Furthermore, it is advantageous that the reactor system can be operated or is operable using any process gas or mixture of process gases. The gas used as the process gas is preferably suitable, for example, for reducing operation or as an explosion-proof gas. In a particularly preferred embodiment, the process gas is an inert gas, i.e., the process gas does not participate in the reaction carried out in the reactor for producing and / or processing particles, but is used to provide and transfer heat energy and as a transport gas for the particles. Moreover, it is highly advantageous in the above design that the reactor system is suitable for organic and / or combustible raw materials in addition to "classical" inorganic raw materials.

[0017] Furthermore, no fuel gas is required when operating the reactor system, thus allowing for the production and / or processing of particles with minimal pollution, up to and including pollution-free production and / or processing. According to preferred methods, it is possible to produce high-purity particles by minimizing or avoiding pollution during the production and / or processing of particles, preferably nanoparticles, and particularly preferably nanocrystalline metal oxide particles. Moreover, due to the possibility of not requiring fuel gas, a simplified equipment and safety scheme is sufficient for the reactor system, as flame monitoring is, for example, unnecessary. It is possible that this adaptation to the manufacturing and / or processing processes makes the reactor system suitable for manufacturing processes in the pharmaceutical and food industries.

[0018] According to an advantageous extension of the reactor system, the reactor system includes a heating device for heating the process gas. The heating device is preferably configured as a convection heater, an electro-gas heater, a plasma heater, a microwave heater, an induction heater, a radiant heater, or a gas heater (e.g., a burner).

[0019] The heating device can be arranged upstream or downstream of the pulsating device. An upstream arrangement is preferred because the heating device in such an arrangement does not dampen the resonant pressure amplitude in the reactor system. Furthermore, the heating device is suitable for heating the process gas to temperatures from 100°C to 3000°C, preferably from 240°C to 2200°C, particularly preferably from 240°C to 1800°C, very particularly preferably from 650°C to 1800°C, and most preferably from 700°C to 1500°C. This very wide temperature range of 100°C to 3000°C allows for effective and unique adaptation to particle manufacturing and / or processing processes. Compared to reactor systems based on combustion processes according to the prior art, the significantly lower process temperatures can be very economical, i.e., without the need for an additional air supply.

[0020] According to an additional advantageous design of the reactor system, the pressure loss generating device is immutably arranged in its respective position within the process gas supply unit and the process gas outlet unit during operation. Advantageously, by means of the immutable arrangement of the pressure loss generating device during operation, a vibratory system is obtained within the reactor system, having precisely defined geometry and therefore a resonant gas column constructed within the reactor system with a defined process gas volume. Due to the constrained vibration system, resonant vibrations can be effectively generated and propagated within the vibration system.

[0021] The pulsation device is preferably configured as a pressure loss generating device. By configuring the pulsation device as a pressure loss generating device, equipment components are saved, and thus investment costs are reduced.

[0022] According to another advantageous extension of the reactor system, a process gas volume flow regulator is arranged upstream of at least one reactor. The process gas volume flow regulator is preferably arranged downstream of the pulsation device. The process gas volume flow regulator is hereby constructed, in particular, as a sliding valve, regulating valve, regulating cock, or adjustable irisbleed valve. Regulating fittings with high regulation accuracy are suitable as process gas volume flow regulators. Suitably, the process gas volume flow regulator has a regulation accuracy of less than or equal to 3%, preferably less than or equal to 2%, particularly preferably less than or equal to 1%, and most preferably less than or equal to 0.5%. High regulation accuracy of the process gas volume flow is necessary to minimize or avoid feedback to the process gas volume flow caused by resonant vibrations. Especially when using a process gas flow distribution device, high regulation accuracy of the process gas volume flow is necessary to ensure stable operation of the system, whether vibrating or vibrating during operation.

[0023] According to an additional advantageous design of the reactor system, a process gas flow distribution device is arranged upstream of at least one reactor, such that each reactor in the reactor unit is equipped with at least one process gas inlet line. Each process gas inlet line preferably has a process gas volume flow regulating device. The process gas flow distribution device is particularly preferably arranged downstream of the pulsation device. Each process gas inlet line is specifically constructed such that each process gas line has a pressure loss between the process gas flow distribution device and the reactor inlet, wherein the pressure loss in each process gas line is substantially the same. For this purpose, the process gas inlet lines also suitably have the same process gas inlet line length and / or the same process gas inlet line inner diameter and / or other identical internal components. The above measures are used to adjust the uniform distribution of the process gas flow in the process gas inlet lines.

[0024] According to an additional advantageous extension of the reactor system or method, the process gas supply unit and the process gas outlet unit have process gas pressure regulating devices, thereby allowing adjustment or regulation of the static process gas pressure in the reactor system. Particularly advantageously, the reactor system can operate under different, arbitrary static process gas pressures. By adapting the static process gas pressure, the acoustic characteristics of the reactor system can be influenced, allowing the reactor system to be adapted, for example, to feeds of different raw materials with varying resonant pressure amplitudes of damped resonant vibrations. This, in turn, allows for an additional influence on the resonant pressure amplitude independently of process temperature, and influences, preferably enhances, the effect on particle manufacturing or processing. The static process gas pressure can be adjusted within a low-pressure range or an over-pressure range relative to the environment. An increase in static process gas pressure generally leads to an increase in the resonant pressure amplitude. The resonator characteristics are significant depending on the change in static process gas pressure.

[0025] Furthermore, the process gas discharge device preferably has multiple process gas discharge lines, each of which has a pressure loss generating device. Thus, the vibratory nature of the reactor system is advantageously limited in its geometry.

[0026] According to an additional advantageous design of the reactor system, the process gas exit device has a process gas cooling section and / or separation device, particularly a cyclone separator and / or filter, and / or a process gas delivery device. The process gas cooling section is used to stop the proceeding reaction and / or adapt the process gas flow to the maximum permissible temperature of the subsequent separation device, particularly the filter, for example, by using a quencher that rapidly stops the proceeding reaction at a specific location and thus at a specific point in time. The separation device (which may have a filtration device including multiple filters, for example to increase the separation surface) is used to separate particles from the process gas.

[0027] In methods of the type described above, this objective is thus achieved by adapting the pulsation frequency and / or pulsation pressure amplitude of the pulsation to one of the inherent resonant frequencies of the resonator using a pulsation device, in order to achieve the selected resonant state. Preferably, periodic pulsation is applied to the process gas. Particularly preferably, the pulsation frequency, or an integer multiple thereof, is adjusted near the resonant frequency of the resonator, thereby exciting the resonator and causing resonant vibration in the vibrating system. By applying periodic pulsation to the process gas, wherein the pulsation frequency, or an integer multiple thereof, is selectively adjusted near the resonant frequency of the resonator, an enhancement of the resonant vibration of the process gas with a resonant frequency and resonant pressure amplitude is achieved. "Near" here means that the pulsation frequency or an integer multiple thereof has a frequency within +5% of the resonant frequency.

[0028] Therefore, instead of adapting the reactor system, constructed as a resonator, to a pulsation with a pulsating frequency and / or pulsating pressure amplitude as is common in the prior art, the pulsation is adapted to a resonator of a vibrating system to achieve the selected resonance state of the acoustic resonator. The resonator characteristics can be changed independently of the process temperature by altering the static process gas pressure. Advantageously, by adapting the pulsation, the same reactor system can now be used to manufacture and / or process different particles.

[0029] According to an advantageous design of this method, the process gas flows through the reactor system with a residence time of 0.1 s to 25 s. Due to the longer residence time in the reactor system and therefore in the reactor, the raw materials are exposed to the process gas temperature for a longer period, thereby enabling particle manufacturing and / or processing to be completed without requiring post-heating treatment of the particles.

[0030] Furthermore, a pulsation frequency of 1 Hz to 2000 Hz, preferably between 1 Hz and 500 Hz, and particularly preferably between 40 Hz and 160 Hz, is applied to the process gas via a pulsation device. Advantageously, this achieves very high turbulence in the gas flowing through the reactor system, as a wide frequency range can be adjusted, thereby producing very small particles down to the nanometer scale, which can be precisely matched to the particles to be treated and manufactured. By increasing turbulence, mass and heat transfer between the process gas and at least one raw material to be heat-treated is significantly improved in the reactor system.

[0031] According to an additional advantageous extension, a pulsating pressure amplitude of 0.1 mbar to 350 mbar, preferably 1 mbar to 200 mbar, entirely and particularly preferably 3 mbar to 50 mbar, and most preferably 10 mbar to 40 mbar is applied to the process gas via a pulsating device. By applying pressure pulsations with defined amplitudes, optimal adjustment of the process conditions required for the particles to be manufactured and / or processed can be achieved.

[0032] In a particularly preferred configuration of this method, a pulsation frequency of 40 Hz to 160 Hz and a pulsation pressure amplitude of 10 mbar to 40 mbar are applied to the process gas via a pulsation device. These conditions surprisingly prove to be an optimal combination of pulsation frequency and pulsation amplitude, resulting in excellent mass and heat transfer between the process gas and the particles to be heat-treated in the reactor system.

[0033] Furthermore, the pressure loss generating device remains unchanged in its corresponding position during operation. Advantageously, the geometry of the reactor system and the volume of the process gas in the resonant gas column constructed within the reactor system do not change during operation, allowing the pulsation to be optimally adapted to the method performed with a specific raw material. Another advantage is that, after the method ends, the pressure loss generating device can be changed in its corresponding position, and thus the reactor system can be adapted to other methods to be performed.

[0034] Furthermore, the reactor system used in the method is a reactor system according to the present invention. Attached Figure Description

[0035] The invention will now be explained in more detail with reference to the accompanying drawings. Wherein:

[0036] Figure 1 A schematic diagram of a first embodiment of a preferred reactor system is shown.

[0037] Figure 2 A schematic diagram of a second embodiment of a preferred reactor system is shown.

[0038] Figure 3 A schematic diagram of a third embodiment of a preferred reactor system is shown.

[0039] Figure 4 A schematic diagram of a fourth embodiment of a preferred reactor system is shown.

[0040] Figure 5 A schematic diagram of a fifth embodiment of a preferred reactor system is shown, and

[0041] Figure 6 The diagram shows the resonant pressure amplitude versus resonant frequency at three different locations in the reactor system. Detailed Implementation

[0042] Unless otherwise stated, the following description refers to all embodiments shown in the figures of reactor system 1, which is used to manufacture and / or process particles P in a vibrating process gas stream.

[0043] The reactor system 1 has a reactor unit 2, a process gas supply unit 3 connected upstream of the reactor unit, and a process gas outlet unit 4 connected downstream of the reactor unit.

[0044] The reactor system 1 includes a process gas delivery device 5 and a heating device 6. The process gas PG flowing through the reactor system 1 enters the reactor system 1 via the process gas supply unit 3 and is delivered through the reactor system 1 via the process gas delivery device 5.

[0045] The process gas delivery device 5 is constructed, for example, particularly as a radial flow ventilator, blower, or compressor. The process gas delivery device 5 can be arranged, particularly in the process gas supply unit 3, the process gas outlet unit 4, or alternatively, both in the process gas supply unit 3 and the process gas outlet unit 4. Figure 1 , Figure 2 and Figure 4 In this embodiment, the arrangement of the process gas delivery device 5 within the process gas supply unit 3 is shown. Figure 5 In the process gas export unit 4, there is a process gas delivery device 5. Figure 3 An embodiment with two process gas delivery devices 5 is shown, which are arranged both in the process gas supply unit 3 and the process gas outlet unit 4. The arrangement of the process gas delivery devices 5 is adapted to the conditions to be adjusted in the reactor system 1, particularly the conditions to be adjusted in terms of the shape, quality, and density of the raw materials.

[0046] The heating device 6 can be arranged upstream of or downstream of the pulsating device 7. The arrangement upstream of the pulsating device 7 (e.g., in...) Figure 1 , Figure 2 , Figure 3 and Figure 5 The arrangement shown in the embodiment is preferred because the heating device 6 in such an arrangement does not dampen the resonant pressure amplitude in the reactor system 1. The arrangement downstream of the pulsating device 7... Figure 2 The embodiment shown is disclosed. The arrangement of the heating device 6 determines whether the heating device 6 is associated with the reactor unit 2 or the process gas supply unit 3. The heating device 6 arranged upstream of the pulsating device 7 is associated with the process gas supply unit 3, and the heating device 6 arranged downstream of the pulsating device 7 is associated with the reactor unit 2.

[0047] The heating device 6 is preferably configured as a convection gas heater, an electro-gas heater, a plasma heating device, a microwave heating device, an induction heating device, or a radiation heater. More preferably, the heating device 6 is configured as a burner with a flame.

[0048] The process gas PG flowing through reactor system 1 is heated to the manufacturing temperature and / or processing temperature by heating device 6. The temperature used for manufacturing or heat treating at least one raw material is preferably between 100°C and 3000°C, more preferably between 240°C and 2200°C, particularly preferably between 240°C and 1800°C, very particularly preferably between 650°C and 1800°C, and most preferably between 700°C and 1500°C.

[0049] The process gas PG flowing through the reactor system 1 is subjected to pulsation with a pulsation frequency and pulsation pressure amplitude by means of pulsation device 7. The pulsation preferably has a pulsation pressure amplitude of 0.1 mbar to 350 mbar, particularly preferably 1 mbar to 200 mbar, very particularly preferably 3 mbar to 50 mbar, and most preferably 10 mbar to 40 mbar.

[0050] The pulsation frequency of the process gas PG can be adjusted independently of the pulsation pressure amplitude. The pulsation frequency of the process gas PG flowing through the reactor system 1 in a pulsating manner due to the pulsation device 7 can also be adjusted, preferably within a frequency range of 1Hz to 2000Hz, more preferably 1Hz to 500Hz, and particularly preferably 40Hz to 160Hz.

[0051] The pulsation device 7 is configured as a flameless pulsation device 7. The pulsation device 7 is suitably configured as a compression module, especially a piston, or as a rotating slider or a modified rotary gate.

[0052] Reactor 9, which has a reaction chamber 8 and is associated with reactor unit 2, is located downstream of process gas supply unit 3. In the reaction chamber 8 of reactor 9, raw materials are introduced into the pulsating process gas PG flowing through reactor system 1 and reactor 9 via feed device 10.

[0053] The feeding device 10 is preferably configured to introduce liquid or solid into the reaction chamber 8 of the reactor 9.

[0054] Liquid or liquid feedstock (precursor) may preferably be introduced into reaction chamber 8 as a solution, suspension, melt, emulsion, or as a pure liquid. The introduction of liquid feedstock or liquid is preferably continuous. To introduce liquid into reaction chamber 8 of reactor 9 in reactor unit 2, a feed device 10 is preferably used, such as a jet nozzle, supply pipe, or dropper, which may be configured as a single-material or multi-material nozzle, pressure nozzle, atomizer (aerosol), or ultrasonic nozzle.

[0055] In contrast, in order to introduce solids (e.g., powders, particles, etc.) into reactor 9, preferably reactor 9's reaction chamber 8, it is preferable to use a feeding device 10 such as a double valve, a star wheel brake, a timing brake, or a syringe.

[0056] The introduction of raw materials in liquid or solid form can be carried out along the flow direction of the process gas PG flowing through reactor system 1 or against that flow direction. Figure 1 and Figures 3 to 5 In the implementation method described, the raw material is fed along the flow direction of the process gas. Figure 2 In the embodiment shown, the raw material is fed against the flow direction of the process gas.

[0057] Preferably, the raw material is introduced into reactor system 1, and more preferably into reaction chamber 8 of reactor 9, when using a carrier gas. The decision of whether the raw material is introduced into reactor system 1 along or against the flow direction of the process gas depends primarily on the shape, mass, and density of the raw material at the adjusted average flow velocity of the process gas PG. Therefore, there is also the possibility of heat-treating raw materials that cannot be transported in reactor system 1 by process gas PG.

[0058] The raw materials are heat-treated in the processing zone of reactor 9, preferably in reaction chamber 8, to construct the particles P to be manufactured, preferably inorganic or organic nanoparticles, and particularly preferably nanocrystalline metal oxide particles. The area in which the raw materials are heat-treated is defined as the processing zone.

[0059] The process gas exit unit 4, located after reactor unit 2, includes a separation device 11. The separation device 11, particularly a filter, preferably a hot gas filter, entirely and especially preferably a hose filter, a metal filter or glass fiber filter, a cyclone separator, or a scrubber, separates the heat-treated particles P from the pulsating flow of hot process gas through reactor system 1. The particles P separated from the process gas flow are exited from the separation device 11 for further processing. If necessary, the heat-treated particles P in reactor system 1 may undergo further post-processing steps, such as suspension, grinding, or calcination. Unloaded process gas PG is discharged into the environment.

[0060] The residence time of the raw materials introduced into reactor system 1, especially into reaction chamber 8 of reactor 9, is between 0.1 s and 25 s. A circulating operation mode for the process gas PG is possible. If necessary, partial recirculation of the process gas PG is also possible.

[0061] Furthermore, the reactor system 1 with static process gas pressure is configured as an acoustic resonator 12, which has a natural resonant frequency that defines the resonant state. The process gas PG can be configured into a resonant gas column within the reactor system 1, such that the resonator 12 can be excited by the pulsating frequency and / or pulsating pressure amplitude generated by the pulsating device 7, and in the resonant state, the pulsation can be amplified into resonant vibration of the process gas PG with a resonant frequency and resonant pressure amplitude.

[0062] The process gas supply unit 3 and the process gas outlet unit 4 each include a pressure loss generating device 13, wherein the pressure loss generating device 13 is configured such that one of the resonant states of the resonator 12 can be selectively adjusted. The pressure loss generating device 13 geometrically restricts the vibratory or operating system 14 of the reactor system 1 in terms of the process gas volume of the constructed, resonant gas column. The pressure loss generating device 13 thus prevents resonant vibrations from propagating beyond the pressure loss generating device 13. The more restricted the vibratory or operating system 14 is, the more efficient the generation and propagation of resonant vibrations within the system 14.

[0063] The pulsation device 7 is preferably configured as a pressure loss generating device 13. This preferred configuration of the pulsation device 7... Figure 1 , Figure 3 and Figure 5 The implementation method is shown below.

[0064] The pressure loss generating device 13 is variably arranged in its respective position within the reactor system 1, particularly in the process gas supply unit 3 and the process gas outlet unit 4, wherein, during operation, the pressure loss generating device 13 cannot be changed in its previously adjusted position. This ensures that the vibration of the system 14 during operation remains unchanged.

[0065] The pulsation device 7 of reactor system 1 is configured such that the pulsation frequency and / or pulsation pressure amplitude are matched to one of the inherent resonant frequencies of resonator 12, thereby enabling the achievement of a selected resonant state. Particularly preferably, the pulsation frequency, or an integer multiple thereof, is adjusted near the resonant frequency of resonator 12, thereby exciting resonator 12 and resulting in resonant vibration in the vibrating system 14. By applying periodic pulsations to the process gas, particularly by selectively adjusting the pulsation frequency, or an integer multiple thereof, near the resonant frequency of resonator 12, the resonant vibration of the process gas with resonant frequency and resonant pressure amplitude is enhanced. This improves the heat transfer and mass transfer characteristics of the preferably hot process gas in reactor system 1.

[0066] In certain processes, it is advantageous that the static pressure in reactor system 1 can be adjusted or regulated. For this purpose, reactor system 1, especially process gas supply unit 3 and process gas outlet unit 4, has a process gas regulating device 15. Figure 3 The implementation method discloses such a component.

[0067] The pressure loss generating device 13 of the system 14, which restricts vibration or vibration during operation, can be arranged within the process gas conditioning device 15. Therefore, the process gas conditioning device 15 is arranged upstream of the pressure loss generating device 13 in reactor unit 2, and downstream of the pressure loss generating device 13 in reactor unit 2. Without such a process gas conditioning device 15, the static process gas pressure in reactor system 1 corresponds to atmospheric pressure.

[0068] The characteristics of the acoustic resonator 12 can be affected by adapting the static process gas pressure in reactor system 1. Changes in the flow resistance, acoustic phenomena, and material properties of the process gas and the raw materials fed into it can dampen resonant vibrations. The energy consumption for generating resonant vibrations increases accordingly and / or the adjustability of resonant vibrations is affected. In particular, reactor system 1 can thus be adapted to factors affecting the resonant pressure amplitude of damped resonant vibrations.

[0069] Higher static process gas pressures, for example, alter the acoustic characteristics of resonator 12, causing its inherent resonant frequency to shift. For this reason, reactor system 1 can only be excited by applying other pulsating frequencies to the process gas.

[0070] Additionally, the amplitude of the pulsating pressure applied to the process gas by the pulsating device 7, and therefore the amplitude of the resonant pressure in the resonant state, are also enhanced.

[0071] Additionally, reactor system 1 may include, for example... Figure 5 The process gas cooling section 16 shown, particularly the quenching device, is used to stop the reaction in the reactor system 1 at a specific time point and / or to adapt the process gas flow to the maximum permissible temperature of the subsequent separation device 11, particularly the filter. The process gas cooling section 16, preferably the quenching device, is arranged upstream of the separation device 11, which is configured as a filter, in the process gas outlet unit 4.

[0072] To stop the reaction and / or limit the temperature of the process gas stream to the maximum permissible temperature of the subsequent separation unit 11, a cooling gas, preferably air, particularly preferably cold air or compressed air, is mixed with the hot process gas stream that is pulsatingly flowing through the reactor system 1 via the process gas cooling section 16. The air mixed via the process gas cooling section 16 may be pre-filtered or temperature-controlled if necessary. In addition to the air mixture or gas mixture, an evaporative liquid (e.g., a solvent or liquefied gas, but preferably water) may be injected.

[0073] The quenching device arranged in reactor system 1 may have an internal component or may be installed in reactor system 1 without an internal component. Other gases, such as nitrogen (N2), argon (Ar), other inert gases, or rare gases, may also be used as cooling gases.

[0074] In addition, a process gas volume flow regulating device 17 is suitably arranged upstream of at least one reactor 9. Figure 3 , Figure 4 and Figure 5 The embodiment illustrates a process gas volume flow regulating device 17. The process gas volume flow regulating device 17 is preferably arranged downstream of the pulsation device. The process gas volume flow regulating device 17 is particularly constructed as a sliding valve, regulating valve, regulating cock, or adjustable aperture throttle valve. The process gas volume flow regulating device 17 has a regulating accuracy of less than or equal to 3%, preferably less than or equal to 2%, particularly preferably less than or equal to 1%, and most preferably less than or equal to 0.5%. A process gas volume flow regulating device 17 with high regulating accuracy is necessary to minimize or avoid feedback to the process gas volume flow caused by resonant vibration. In particular, when using the process gas flow distribution device 18, high regulating accuracy of the process gas volume flow is necessary to ensure stable operation of the system 14, which is capable of vibration or vibrates during operation.

[0075] If reactor unit 2 is as follows Figure 4The embodiment shown has multiple reactors 9, and a process gas flow distribution device 18 is arranged upstream of the reactors 9, such that each reactor 9 of the reactor unit 2 is associated with at least one process gas input pipeline 19.

[0076] Preferably, the process gas flow distribution device 18 is arranged downstream of the pulsation device 7, and each process gas inlet line 19 has a process gas volume flow regulating device 17. Each process gas inlet line 19 is constructed such that each process gas inlet line 19 has a pressure loss between the process gas flow distribution device 18 and the reactor inlet 20, wherein the pressure loss in each process gas inlet line 19 is substantially the same. This is achieved in particular by the fact that the process gas inlet lines 19 have the same process gas inlet line length and / or the same process gas inlet line inner diameter and / or other identical internal components.

[0077] In addition, the process gas discharge unit 4 has at least one of the multiple process gas discharge lines 21 corresponding to the multiple reactors 9, wherein each process gas discharge line 21 has a pressure loss generating device 13.

[0078] The process gas exhaust lines 21 are collected together and the particles P are separated from the process gas stream via the separation device 11, preferably from the hot process gas stream.

[0079] Figure 6 A graph showing the resonant pressure amplitude versus resonant frequency at three different locations in reactor system 1 at a process gas temperature of 300°C is presented.

[0080] Curves x1 to x3 show the variation of the resonant pressure amplitude in units of mbar at three different locations in reactor system 1, namely immediately after the pulsation device 7 (x1), at reactor inlet 20 (x2), and at reactor outlet 22 (x3).

[0081] Resonant vibration corresponds to enhanced pulsation, such that the pulsation frequency matches the resonant frequency.

[0082] The pulsation pressure amplitude is adjusted to approximately 15 mbar, which can be read from the average pulsation pressure amplitude immediately following the pulsation device 7, wherein the pulsation pressure amplitude varies minimally with different pulsation frequencies in system 14.

[0083] The graph shows that 60Hz is the inherent resonant frequency of resonator 12, because the maximum resonant pressure amplitude of approximately 70mbar occurs at reactor inlet 20.

[0084] At the natural resonant frequency of 60 Hz, a resonant pressure amplitude of approximately 35 mbar can be read at reactor outlet 22. The decrease in the resonant pressure amplitude between reactor inlet 20 and reactor outlet 22 can be explained by the damping of system 14, as feed material and flow resistance damp the resonant pressure amplitude of system 14.

Claims

1. A reactor system (1) for manufacturing and / or processing particles (P) in a vibrating process gas stream, the reactor system comprising a reactor unit (2) having a pre-process gas supply unit (3) and a post-process gas outlet unit (4), the reactor unit having at least one reactor (9), the reactor comprising a reaction chamber (8) for manufacturing and / or processing particles and a feed device (10) for introducing raw materials into the reaction chamber (8), wherein, The process gas (PG) flowing through the reactor unit (2) along the direction of the process gas outlet unit (4) can be supplied to the reactor unit (2) via the process gas supply unit (3), and the reactor system (1) includes a pulsation device (7) suitable for generating pulsations of the process gas (PG), wherein the process gas (PG) can be subjected to pulsations having a pulsation frequency and a pulsation pressure amplitude by means of the pulsation device (7), characterized in that the reactor system (1) having an adjustable static process gas pressure is configured as an acoustic resonator (12), the resonator having an inherent resonant frequency that correspondingly defines the resonant state, and the process gas (PG) can form a resonant gas column in the reactor system (1), such that the resonator (12) can be excited by the pulsation frequency and / or pulsation pressure amplitude of the pulsations generated by the pulsation device (7), and Furthermore, in the resonant state, the pulsation can be amplified into a resonant vibration of the process gas (PG) with a resonant frequency and a resonant pressure amplitude, and wherein the process gas supply unit (3) and the process gas outlet unit (4) each include a pressure loss generating device (13) that generates pressure loss, wherein the pressure loss generating device (13) is configured such that one of the resonant states can be selectively adjusted, wherein the pulsation device (7) is configured such that the pulsation frequency and / or pulsation pressure amplitude of the pulsation is adapted to one of the inherent resonant frequencies of the resonator (12), thereby achieving the selected resonant state, wherein the pressure loss generating device (13) is variably arranged in its respective position in the reactor system (1), wherein, in the operating state, the pressure loss generating device (13) is invariable in its previously adjusted position.

2. The reactor system (1) according to claim 1, characterized in that, The pulsation device (7) is configured as a flameless pulsation device (7).

3. The reactor system (1) according to claim 1, characterized in that, The reactor system (1) has a heating device (6) for heating the process gas (PG).

4. The reactor system (1) according to claim 3, characterized in that, The heating device (6) is arranged upstream of or downstream of the pulsating device (7).

5. The reactor system (1) according to any one of claims 1 to 4, characterized in that, The pulsation device (7) is configured as a pressure loss generating device (13).

6. The reactor system (1) according to claim 1, characterized in that, A process gas volume flow regulating device (17) is arranged upstream of the at least one reactor (9).

7. The reactor system (1) according to claim 6, characterized in that, The process gas volume flow regulating device (17) is arranged downstream of the pulsation device (7).

8. The reactor system (1) according to claim 6, characterized in that, The process gas volume flow regulating device (17) is constructed as a sliding valve, regulating valve, regulating plug or adjustable aperture throttle valve.

9. The reactor system (1) according to any one of claims 6 to 8, characterized in that, The process gas volume flow regulating device (17) has a regulating accuracy of less than or equal to 3%.

10. The reactor system (1) according to claim 1, characterized in that, A process gas flow distribution device (18) is arranged upstream of the at least one reactor (9) such that each reactor (9) of the reactor unit (2) is provided with at least one process gas inlet line (19).

11. The reactor system (1) according to claim 10, characterized in that, The process gas flow distribution device (18) is arranged downstream of the pulsation device (7).

12. The reactor system (1) according to claim 10, characterized in that, Each process gas inlet line (19) has a process gas volume flow regulating device (17).

13. The reactor system (1) according to any one of claims 10 to 12, characterized in that, Each process gas inlet line (19) is constructed such that each process gas inlet line (19) has a pressure loss between the process gas flow distribution device (18) and the reactor inlet (20), wherein the pressure loss in each process gas inlet line (19) is substantially the same.

14. The reactor system (1) according to any one of claims 10 to 12, characterized in that, The process gas input line (19) has the same process gas input line length and / or the same process gas input line inner diameter and / or other identical built-in components.

15. The reactor system (1) according to any one of claims 1 to 4, characterized in that, The process gas supply unit (3) and the process gas output unit (4) have a process gas pressure regulating device (15) which enables the regulation of the static process gas pressure in the reactor system (1).

16. The reactor system (1) according to any one of claims 1 to 4, characterized in that, The process gas discharge unit (4) has multiple process gas discharge lines (21), wherein each process gas discharge line (21) has a pressure loss generating device (13).

17. The reactor system (1) according to any one of claims 1 to 4, characterized in that, The pulsation device (7) is constructed as a compression module, or as a rotating slider or a modified rotating gate.

18. The reactor system (1) according to any one of claims 1 to 4, characterized in that, The process gas outlet unit (4) has a process gas cooling section (16) and / or a separation device (11) and / or a process gas conveying device (5).

19. The reactor system (1) according to any one of claims 6 to 8, characterized in that, The process gas volume flow regulating device (17) has a regulating accuracy of less than or equal to 2%.

20. The reactor system (1) according to any one of claims 6 to 8, characterized in that, The process gas volume flow regulating device (17) has a regulating accuracy of less than or equal to 1%.

21. The reactor system (1) according to any one of claims 6 to 8, characterized in that, The process gas volume flow regulating device (17) has a regulating accuracy of less than or equal to 0.5%.

22. A method for manufacturing and / or processing particles (P) in a vibrating process gas stream, comprising a reactor system (1) having reactor units (2) having a pre-process gas supply unit (3) and a post-process gas outlet unit (4), the reactor unit having at least one reactor (9) comprising a reaction chamber (8) for manufacturing and / or processing particles and a feed device (10) for introducing raw materials into the reaction chamber (8), wherein, The process gas (PG) flowing through the reactor unit (2) in the direction of the process gas outlet unit (4) is supplied to the reactor unit (2) via the process gas supply unit (3), and the reactor system (1) includes a pulsation device (7) suitable for generating pulsations of the process gas (PG), wherein pulsations with a pulsation frequency and a pulsation pressure amplitude are applied to the process gas (PG) by means of the pulsation device (7), characterized in that the reactor system (1) having an adjustable static process gas pressure is configured as an acoustic resonator (12), the resonator having an inherent resonant frequency that correspondingly defines the resonant state, and the process gas (PG) constructs a resonant gas column in the reactor system (1), thereby exciting the resonator (12) by the pulsation frequency and / or pulsation pressure amplitude of the pulsations generated by the pulsation device (7). Furthermore, in the resonant state, the pulsation is amplified into a resonant vibration of the process gas (PG) having a resonant frequency and a resonant pressure amplitude, wherein the process gas supply unit (3) and the process gas outlet unit (4) each include a pressure loss generating device (13) that generates pressure loss, wherein the pressure loss generating device (13) is configured such that one of the resonant states is selectively adjusted, wherein the pulsation frequency and / or pulsation pressure amplitude of the pulsation is adapted to one of the inherent resonant frequencies of the resonator (12) by means of the pulsation device (7) in order to achieve the selected resonant state, wherein the pressure loss generating device (13) is variably arranged in its respective position in the reactor system (1), wherein the pressure loss generating device (13) does not change in its previously adjusted position in the operating state.

23. The method according to claim 22, characterized in that, Periodic pulsations are applied to the process gas (PG).

24. The method according to claim 22, characterized in that, The pulsation frequency or an integer multiple thereof is adjusted to be near the resonant frequency of the resonator (12).

25. The method according to any one of claims 22 to 24, characterized in that, The reactor system (1) has a heating device (6) for heating the process gas, wherein the process gas (PG) is heated to a temperature of 100°C to 3000°C.

26. The method according to any one of claims 22 to 24, characterized in that, The process gas (PG) flows through the reactor system (1) with a residence time of 0.1 s to 25 s.

27. The method according to any one of claims 22 to 24, characterized in that, The process gas (PG) is subjected to a pulsation frequency of 1 Hz to 2000 Hz by the pulsation device (7).

28. The method according to any one of claims 22 to 24, characterized in that, The process gas (PG) is subjected to a pulsating pressure amplitude of 0.1 mbar to 350 mbar by the pulsating device (7).

29. The method according to any one of claims 22 to 24, characterized in that, The process gas (PG) is subjected to a pulsation frequency of 40 Hz to 160 Hz and a pulsation pressure amplitude of 10 mbar to 40 mbar by the pulsation device (7).

30. The method according to any one of claims 22 to 24, characterized in that, The process gas supply unit (3) and the process gas output unit (4) have a process gas pressure regulating device (15) so that the static process gas pressure in the reactor system (1) is adjustable or adjustable.

31. The method according to any one of claims 22 to 24, characterized in that, The reactor system (1) used in the method is the reactor system (1) according to any one of claims 1 to 21.

Images