A microreactor

Abstract

This invention relates to a microreactor device, comprising at least one microreactor and at least one tubular reactor connected in series. The tubular reactor includes a tube side and a shell side. The tube side contains several internal component units, each including two or more rotatable blades. These blades have auxiliary structures for increasing material flow disturbance. According to the microreactor device of this invention, multiple reactant streams can be thoroughly mixed in the microreactor. When the material flowing from the microreactor enters the tubular reactor, the material flow impacts the blades, causing them to rotate. Furthermore, the auxiliary structures on the blades increase material flow disturbance, thereby continuously cutting and disturbing the material, maintaining a turbulent state and allowing the reaction to continue. Therefore, using the microreactor device of this invention can maintain the material in a well-mixed state, thus achieving better reaction efficiency.

Description

Technical Field

[0001] This invention relates to a microreactor, specifically a high-throughput microreactor for material mixing and reaction. Background Technology

[0002] Microreactors are reaction devices with microstructures (channels, sieves, and grooves, etc.) that can form micron-scale dispersed single-phase or multiphase systems to enhance reaction processes. They offer advantages such as small characteristic scale, high transfer efficiency, and near-plug flow, enabling precise control of fluids and reaction conditions. In recent years, they have experienced rapid development in the pharmaceutical, chemical, and fine chemical production industries, demonstrating superior equipment performance.

[0003] The unique characteristics of microreactors—their small scale—enhance mass and heat transfer, but also bring problems such as large system pressure drop, low reaction throughput, and short material residence time, severely limiting their application and promotion. Current industrial applications are limited to small-volume chemical production or specific second-level fast reactions; large-scale industrial production of most chemicals remains impossible. Therefore, developing high-throughput reaction equipment suitable for industrial production is of great significance.

[0004] Patent application CN215901720U discloses a microreactor structure and a microchannel reactor, which adopts an elliptical cavity structure and sets a flow guide inside to promote material mixing.

[0005] Patent application CN211725714U discloses a high-throughput microreactor for preparing di-tert-butyl peroxide. This equipment includes a feeding device, a microreactor, and a post-processing device. The microreactor includes a primary microreactor and a secondary microreactor. The post-processing device includes a stirred reactor or a tubular reactor. In this equipment, the material at the reactor outlet is not yet fully reacted. If it enters the subsequent stirred reactor, similar to existing batch reactor production methods, or if it enters the tubular reactor, the material may stratify due to the unclear configuration of the tubular reactor, leading to incomplete reaction.

[0006] Patent application CN105617957A discloses a method for enhancing fluid mixing and reaction within a microreactor, comprising a tubular reactor with internal components, wherein the internal components are mesh-structured foam metal, foam ceramic, or quartz packing.

[0007] Patent application CN108514855A discloses a reaction apparatus comprising a microreactor and a tubular reactor. The tubular reactor is either a coil reactor or a straight tube reactor. When the inner diameter of the tubular reactor is large, it can cause material stratification, limiting production capacity.

[0008] Increasing the pipe size can cause reactants to stratify, affecting mass and heat transfer efficiency. Filling the pipe with appropriately structured components can act as a mixer, satisfying the mixing requirements of the reaction and increasing the reaction throughput, thus enabling large-scale industrial production. Summary of the Invention

[0009] The purpose of this invention is to provide a microreactor device suitable for large-scale industrial production, which aims to increase reaction throughput, maintain a high reaction rate, shorten material residence time, and reduce equipment investment.

[0010] To achieve the above objectives, the present invention provides a microreactor device comprising at least one microreactor and at least one tubular reactor connected in series, wherein the tubular reactor comprises a tube side and a shell side, and a plurality of internal component units are disposed within the tube side, each internal component unit comprising two or more rotatable blades, the blades having auxiliary structures for increasing material flow disturbance.

[0011] Preferably, several internal component units are arranged side by side along the central axis of the tube.

[0012] Preferably, the central axis of the tube is a hollow tube.

[0013] Preferably, each internal component unit comprises three or four rotatable blades.

[0014] Preferably, the auxiliary structure is a plate with serrations and holes, one side of which is mounted on the surface of the blade.

[0015] Preferably, on the blade on which the serrated and perforated plate is mounted, the serrated and perforated plate is located on the feed side.

[0016] Preferably, the angle between the plate with serrations and holes and the surface of the blade is 45-90°.

[0017] Preferably, the inner diameter of the tubular reactor is 1-40 cm, more preferably 5-20 cm; the length of the tubular reactor is 0.5-100 m, more preferably 1-50 m.

[0018] Preferably, the microreactor device includes two or more microreactors and two or more tubular reactors, and the microreactors and the tubular reactors are arranged at intervals.

[0019] Preferably, along the flow direction of the reactants, the first reactor is a microreactor and the last reactor is a tubular reactor.

[0020] Preferably, the microreactor is a microchannel or a microreactor plate with mixing and heat dissipation functions, and the microreactor plate is preferably heart-shaped or umbrella-shaped.

[0021] Preferably, the microreactor further includes multiple material supply channels for supplying reactants and a post-processing device for processing the reactants.

[0022] According to the microreactor of this invention, multiple reactants can be thoroughly mixed in the microreactor. After flowing out of the microreactor and into the tubular reactor, the material flow impacts the blades, causing them to rotate. Furthermore, auxiliary structures on the blades increase the material flow disturbance, continuously cutting and disrupting the material, maintaining a turbulent flow state and allowing the reaction to continue. Therefore, using the microreactor of this invention can maintain the material in a well-mixed state, thereby achieving better reaction efficiency.

[0023] In addition, the microreactor described in this invention can achieve large-scale continuous production, reduce the liquid hold-up in the reaction, reduce reaction risks, and reduce the occurrence of accidents. Attached Figure Description

[0024] Figure 1 This is a schematic diagram of the microreactor device described in this invention;

[0025] Figure 2 This is a schematic diagram of the internal structure of the tubular reactor in the microreactor described in this invention;

[0026] Figure 3 This is a schematic diagram of the internal component unit in the tubular reactor of the present invention.

[0027] Explanation of reference numerals in the attached figures

[0028] 1-First material supply tank; 2-Second material supply tank; 3-Third material supply tank; 4-First material pump; 5-Second material pump; 6-Third material pump; 7-First microreactor; 8-First tubular reactor; 9-Second microreactor; 10-Second tubular reactor; 11-Heat exchanger; 12-Post-treatment device; 20-Internal component unit; 21-Blade; 22-Auxiliary structure. Detailed Implementation

[0029] The specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings. It should be understood that the specific embodiments described herein are for illustration and explanation only and are not intended to limit the present invention.

[0030] In the description of this application, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating relative importance or implying the number of indicated technical features. Therefore, unless otherwise stated, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature; "multiple" means two or more. The term "comprising" and any variations thereof mean a non-exclusive inclusion, the possibility of the presence or addition of one or more other features, units, components, and / or combinations thereof.

[0031] Furthermore, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to fixed connections, detachable connections, or integral connections; they can refer to mechanical connections or electrical connections; they can refer to direct connections or indirect connections through an intermediate medium, or internal connections between two components. Those skilled in the art can understand the specific meaning of the above terms in this application based on the specific circumstances.

[0032] like Figure 1-3 As shown, the microreactor device of the present invention includes at least one microreactor and at least one tubular reactor connected in series. Preferably, the microreactor device includes two or more microreactors and two or more tubular reactors, with the microreactors and tubular reactors arranged at intervals. More preferably, along the flow direction of the reactants, the first reactor is a microreactor, and the last reactor is a tubular reactor. As a specific embodiment, along the flow direction of the reactants, the microreactor device sequentially includes a first microreactor 7, a first tubular reactor 8, a second microreactor 9, and a second tubular reactor 10.

[0033] In the microreactor of this invention, the tubular reactor includes a tube side and a shell side. The tube side contains several internal component units 20, each including two or more rotatable blades 21. These blades have auxiliary structures 22 for increasing material flow disturbance. By configuring the internal component units with specific structures, after the reactants enter the tubular reactor, the material flow impacts the blades, causing them to rotate. Furthermore, the auxiliary structures on the blades increase material flow disturbance, thereby continuously cutting and disturbing the material, maintaining a better mixing state. In the tubular reactor, the shell side can be filled with a heat exchange medium for heat exchange with the reactants in the tube side.

[0034] In the microreactor device of the present invention, the length of the tubular reactor can be appropriately configured according to the heat and mass transfer requirements of the material. In a specific embodiment, the inner diameter of the tubular reactor can be 1-40 cm, preferably 5-20 cm; the length of the tubular reactor can be 0.5-100 m, preferably 1-50 m. In the tubular reactor, preferably, several internal component units are arranged side by side along the central axis of the tubular section. The distance between two adjacent internal component units can be 0-5 m, preferably 0.1-3 m, more preferably 0.1-2 m.

[0035] In the tubular reactor, the central axis of the tube side can be a solid tube or a hollow tube. Preferably, the central axis of the tube side is a hollow tube with heat exchange function. When the central axis of the tube side is a hollow tube, the hollow tube can be filled with a heat exchange medium for heat exchange with the reactants within the tube side.

[0036] In the tubular reactor, each internal component unit 20 includes two or more rotatable blades 21. Specifically, the number of blades in each internal component unit 20 can be two, three, or four or more. In a preferred embodiment, each internal component unit includes three or more rotatable blades 21, more preferably three or four rotatable blades 21.

[0037] In the tubular reactor, the auxiliary structure 22 in the blades is used to increase the flow disturbance, allowing for more thorough mixing of the reactants. In a preferred embodiment of the invention, the auxiliary structure 22 is a plate with serrations and perforations, one side of which is mounted on the surface of the blade. With this preferred configuration, the auxiliary structure effectively disturbs the flow during blade rotation without hindering it. The plate with serrations and perforations can be fixed or detachably mounted.

[0038] In a further preferred embodiment, on the blade on which the serrated and perforated plate is mounted, the serrated and perforated plate is located on the feed side. Even more preferably, the angle between the serrated and perforated plate and the blade surface is 45-90°, more preferably 75-90°. By configuring the auxiliary structure 22 in this preferred manner, the effect of disrupting airflow can be further improved, allowing the reactants to mix and react better.

[0039] In the microreactor device described in this invention, the microreactor can use individual microchannels or microreactor plates with mixing and heat dissipation functions. The microreactor has a small channel size, primarily achieving rapid mixing of materials and preliminary reaction. Pressure drop can be reduced by controlling the length of the microchannel or the number of microreactor plates. In specific embodiments, the channel size (i.e., channel diameter) of the microchannel can be 20 μm to 5 mm, preferably 100 μm to 2 mm, more preferably 150 μm to 1 mm; the length of the microchannel can be 0.5-20 m, preferably 1-15 m, more preferably 1-10 m. The microreactor plates can be heart-shaped, umbrella-shaped, or other shaped microreactor plates. In a preferred embodiment, the microreactor uses microreactor plates with mixing and heat dissipation functions. In this preferred embodiment, the microreactor plates have a heat extraction function, which can rapidly remove the heat of reaction.

[0040] In one embodiment, the microreactor includes at least one microreactor and at least one tubular reactor connected in series. The tubular reactor includes a tube side and a shell side. A plurality of internal component units 20 are disposed within the tube side. Each internal component unit 20 includes two or more rotatable blades 21. The blades have auxiliary structures 22 for increasing material flow disturbance. The auxiliary structure 22 is a plate with serrations and perforations. One side of the plate with serrations and perforations is mounted on the surface of the blade. On the blade on which the plate with serrations and perforations is mounted, the plate with serrations and perforations is located on the feed side.

[0041] In another embodiment, the microreactor includes at least one microreactor and at least one tubular reactor connected in series. The tubular reactor includes a tube side and a shell side. A plurality of internal component units 20 are disposed within the tube side. Each internal component unit 20 includes three or more rotatable blades 21. The blades have auxiliary structures 22 for increasing material flow disturbance. The auxiliary structure 22 is a plate with serrations and holes. One side of the plate with serrations and holes is mounted on the surface of the blade. On the blade on which the plate with serrations and holes is mounted, the plate with serrations and holes is located on the feed side. The angle between the plate with serrations and holes and the surface of the blade is 45-90°.

[0042] In another embodiment, the microreactor includes at least one microreactor and at least one tubular reactor connected in series. The tubular reactor includes a tube side and a shell side. A plurality of internal component units 20 are disposed within the tube side. Each internal component unit 20 includes three rotatable blades 21. The blades have auxiliary structures 22 for increasing material flow disturbance. The auxiliary structures 22 are plates with serrations and perforations. One side of the plate with serrations and perforations is mounted on the surface of the blade. On the blade on which the plate with serrations and perforations is mounted, the plate with serrations and perforations is located on the feed side. The angle between the plate with serrations and perforations and the surface of the blade is 75-90°.

[0043] In another embodiment, the microreactor device includes two or more microreactors and two or more tubular reactors connected in series, with the microreactors and tubular reactors arranged at intervals. The tubular reactor includes a tube side and a shell side. A plurality of internal component units 20 are arranged in the tube side. Each internal component unit 20 includes three rotatable blades 21. The blades have auxiliary structures 22 for increasing material flow disturbance. The auxiliary structure 22 is a plate with serrations and holes. One side of the plate with serrations and holes is mounted on the surface of the blade. On the blade on which the plate with serrations and holes is mounted, the plate with serrations and holes is located on the feed side. The angle between the plate with serrations and holes and the surface of the blade is 75-90°.

[0044] In another embodiment, the microreactor device includes two or more microreactors and two or more tubular reactors connected in series, with the microreactors and tubular reactors arranged at intervals along the flow direction of the reactants. The first reactor is a microreactor, and the last reactor is a tubular reactor. The tubular reactor includes a tube side and a shell side. A plurality of internal component units 20 are arranged in the tube side. Each internal component unit 20 includes three rotatable blades 21. The blades have auxiliary structures 22 for increasing material flow disturbance. The auxiliary structure 22 is a plate with serrations and holes. One side of the plate with serrations and holes is mounted on the surface of the blade. On the blade on which the plate with serrations and holes is mounted, the plate with serrations and holes is located on the feed side. The angle between the plate with serrations and holes and the surface of the blade is 75-90°.

[0045] In another embodiment, the microreactor includes a first microreactor 7, a first tubular reactor 8, a second microreactor 9, and a second tubular reactor 10 connected in series. The first tubular reactor 8 and the second tubular reactor 10 each include a tube side and a shell side. A plurality of internal component units 20 are arranged in the tube side. Each internal component unit 20 includes three rotatable blades 21. The blades have an auxiliary structure 22 for increasing material flow disturbance. The auxiliary structure 22 is a plate with serrations and holes. One side of the plate with serrations and holes is mounted on the surface of the blade. On the blade on which the plate with serrations and holes is mounted, the plate with serrations and holes is located on the feed side. The angle between the plate with serrations and holes and the surface of the blade is 75-90°.

[0046] In another embodiment, the microreactor includes a first microreactor 7, a first tubular reactor 8, a second microreactor 9, and a second tubular reactor 10 connected in series. The first tubular reactor 8 and the second tubular reactor 10 each include a tube side and a shell side. The length of the tubular reactor can be 0.5-100m, and the inner diameter of the tube side is 1-40cm. Several internal component units 20 are arranged in the tube side. The spacing between two adjacent internal component units can be 0-5m. Each internal component unit 20 includes three rotatable blades 21. The blades have an auxiliary structure 22 for increasing material flow disturbance. The auxiliary structure 22 is a plate with serrations and holes. One side of the plate with serrations and holes is mounted on the surface of the blade. On the blade on which the plate with serrations and holes is mounted, the plate with serrations and holes is located on the feed side. The angle between the plate with serrations and holes and the surface of the blade is 75-90°.

[0047] In another embodiment, the microreactor includes a first microreactor 7, a first tubular reactor 8, a second microreactor 9, and a second tubular reactor 10 connected in series. The first tubular reactor 8 and the second tubular reactor 10 each include a tube side and a shell side. The length of the tubular reactor can be 1-50m, and the inner diameter of the tube side is 5-20cm. Several internal component units 20 are arranged in the tube side. The spacing between two adjacent internal component units can be 0.1-3m. Each internal component unit 20 includes three rotatable blades 21. The blades have an auxiliary structure 22 for increasing material flow disturbance. The auxiliary structure 22 is a plate with serrations and holes. One side of the plate with serrations and holes is mounted on the surface of the blade. On the blade on which the plate with serrations and holes is mounted, the plate with serrations and holes is located on the feed side. The angle between the plate with serrations and holes and the surface of the blade is 75-90°.

[0048] In this invention, the microreactor may further include multiple material supply channels for supplying reactants and a post-processing device for processing the reacted materials. In one specific embodiment, such as... Figure 1 As shown, the microreactor includes a first material supply tank 1, a second material supply tank 2, a third material supply tank 3, a first material pump 4, a second material pump 5, a third material pump 6, a first microreactor 7, a first tubular reactor 8, a second microreactor 9, a second tubular reactor 10, a heat exchanger 11, and a post-processing device 12. The first stream of material is fed through the first material supply tank 1 and via the first material pump 4; the second stream of material is pumped through the second material supply tank 2 and via the second material pump 5; and the third stream of material is pumped through the third material supply tank 3 and via the third material pump 6. The three streams of material sequentially enter the first microreactor 7, the first tubular reactor 8, the second microreactor 9, and the second tubular reactor 10. The reaction is carried out in reactor 10. The resulting material first enters heat exchanger 11 for heat exchange, and then enters post-processing device 12 for product separation. The first tubular reactor 8 and the second tubular reactor 10 each include a tube side and a shell side. The tube side is provided with a number of internal component units 20. Each internal component unit 20 includes two or more rotatable blades 21. The blades have auxiliary structures 22 for increasing material flow disturbance. The auxiliary structure 22 is a plate with serrations and holes. One side of the plate with serrations and holes is installed on the surface of the blade. On the blade on which the plate with serrations and holes is installed, the plate with serrations and holes is located on the feed side.

[0049] In another specific implementation, such as Figure 1As shown, the microreactor includes a first material supply tank 1, a second material supply tank 2, a third material supply tank 3, a first material pump 4, a second material pump 5, a third material pump 6, a first microreactor 7, a first tubular reactor 8, a second microreactor 9, a second tubular reactor 10, a heat exchanger 11, and a post-processing device 12. The first material stream is fed through the first material supply tank 1 and via the first material pump 4; the second material stream is pumped through the second material supply tank 2 and via the second material pump 5; and the third material stream is pumped through the third material supply tank 3 and via the third material pump 6. The three material streams sequentially enter the first microreactor 7, the first tubular reactor 8, the second microreactor 9, and the second tubular reactor 10 for mixing and reaction, yielding... The reacted material first enters the heat exchanger 11 for heat exchange, and then enters the post-processing device 12 for product separation. The first tubular reactor 8 and the second tubular reactor 10 each include a tube side and a shell side. The tube side is provided with a number of internal component units 20. Each internal component unit 20 includes three or more rotatable blades 21. The blades have auxiliary structures 22 for increasing material flow disturbance. The auxiliary structure 22 is a plate with serrations and holes. One side of the plate with serrations and holes is installed on the surface of the blade. On the blade with the plate with serrations and holes installed, the plate with serrations and holes is located on the feed side. The angle between the plate with serrations and holes and the surface of the blade is 45-90°.

[0050] In another specific implementation, such as Figure 1As shown, the microreactor includes a first material supply tank 1, a second material supply tank 2, a third material supply tank 3, a first material pump 4, a second material pump 5, a third material pump 6, a first microreactor 7, a first tubular reactor 8, a second microreactor 9, a second tubular reactor 10, a heat exchanger 11, and a post-processing device 12. The first material stream is fed through the first material supply tank 1 and via the first material pump 4; the second material stream is pumped through the second material supply tank 2 and via the second material pump 5; and the third material stream is pumped through the third material supply tank 3 and via the third material pump 6. The three material streams sequentially enter the first microreactor 7, the first tubular reactor 8, the second microreactor 9, and the second tubular reactor 10 for mixing and reaction, yielding... The reacted material first enters the heat exchanger 11 for heat exchange, and then enters the post-processing device 12 for product separation. The first tubular reactor 8 and the second tubular reactor 10 each include a tube side and a shell side. The tube side is provided with a number of internal component units 20. Each internal component unit 20 includes three rotatable blades 21. The blades have an auxiliary structure 22 for increasing material flow disturbance. The auxiliary structure 22 is a plate with serrations and holes. One side of the plate with serrations and holes is installed on the surface of the blade. On the blade with the plate with serrations and holes installed, the plate with serrations and holes is located on the feed side. The angle between the plate with serrations and holes and the surface of the blade is 75-90°.

[0051] In another specific implementation, such as Figure 1As shown, the microreactor includes a first material supply tank 1, a second material supply tank 2, a third material supply tank 3, a first material pump 4, a second material pump 5, a third material pump 6, a first microreactor 7, a first tubular reactor 8, a second microreactor 9, a second tubular reactor 10, a heat exchanger 11, and a post-processing device 12. The first material stream is fed through the first material supply tank 1 and via the first material pump 4; the second material stream is pumped through the second material supply tank 2 and via the second material pump 5; and the third material stream is pumped through the third material supply tank 3 and via the third material pump 6. The three material streams sequentially enter the first microreactor 7, the first tubular reactor 8, the second microreactor 9, and the second tubular reactor 10 for mixing and reaction. The resulting reacted material first enters the heat exchanger 11 for heat exchange, and then enters the post-processing device 12. Product separation is performed in the treatment device 12; wherein, the first tubular reactor 8 and the second tubular reactor 10 each include a tube side and a shell side, the length of the tubular reactor can be 0.5-100m, the inner diameter of the tube side is 1-40cm, and a number of internal component units 20 are arranged in the tube side, the spacing between two adjacent internal component units can be 0-5m, each internal component unit 20 includes three rotatable blades 21, the blades have an auxiliary structure 22 for increasing material flow disturbance, the auxiliary structure 22 is a plate with serrations and holes, one side of the plate with serrations and holes is mounted on the surface of the blade, on the blade on which the plate with serrations and holes is mounted, the plate with serrations and holes is located on the feed side, the angle between the plate with serrations and holes and the surface of the blade is 75-90°.

[0052] In another specific implementation, such as Figure 1As shown, the microreactor includes a first material supply tank 1, a second material supply tank 2, a third material supply tank 3, a first material pump 4, a second material pump 5, a third material pump 6, a first microreactor 7, a first tubular reactor 8, a second microreactor 9, a second tubular reactor 10, a heat exchanger 11, and a post-processing device 12. The first material stream is fed through the first material supply tank 1 and via the first material pump 4; the second material stream is pumped through the second material supply tank 2 and via the second material pump 5; and the third material stream is pumped through the third material supply tank 3 and via the third material pump 6. The three material streams sequentially enter the first microreactor 7, the first tubular reactor 8, the second microreactor 9, and the second tubular reactor 10 for mixing and reaction. The resulting reacted material first enters the heat exchanger 11 for heat exchange, and then enters the post-processing device 12. Product separation is performed in the processing device 12; wherein, the first tubular reactor 8 and the second tubular reactor 10 each include a tube side and a shell side, the length of the tubular reactor can be 1-50m, the inner diameter of the tube side is 5-20cm, and a number of internal component units 20 are arranged in the tube side, the spacing between two adjacent internal component units can be 0.1-3m, each internal component unit 20 includes three rotatable blades 21, the blades have an auxiliary structure 22 for increasing material flow disturbance, the auxiliary structure 22 is a plate with serrations and holes, one side of the plate with serrations and holes is mounted on the surface of the blade, on the blade on which the plate with serrations and holes is mounted, the plate with serrations and holes is located on the feed side, the angle between the plate with serrations and holes and the surface of the blade is 75-90°.

[0053] In another specific implementation, such as Figure 1As shown, the microreactor includes a first material supply tank 1, a second material supply tank 2, a third material supply tank 3, a first material pump 4, a second material pump 5, a third material pump 6, a first microreactor 7, a first tubular reactor 8, a second microreactor 9, a second tubular reactor 10, a heat exchanger 11, and a post-processing device 12. The first material stream is fed through the first material supply tank 1 and via the first material pump 4; the second material stream is pumped through the second material supply tank 2 and via the second material pump 5; and the third material stream is pumped through the third material supply tank 3 and via the third material pump 6. The three material streams sequentially enter the first microreactor 7, the first tubular reactor 8, the second microreactor 9, and the second tubular reactor 10 for mixing and reaction. The resulting reacted material first enters the heat exchanger 11 for heat exchange, and then enters the post-processing device 12 for product separation. The first microreactor 7 and the second microreactor 9... Each reactor 9 is a microchannel with a size ranging from 100 μm to 2 mm. The first tubular reactor 8 and the second tubular reactor 10 each include a tube side and a shell side. The length of the tubular reactor can be 1-50 m. The central axis of the tube side is a hollow tube with heat extraction function. The inner diameter of the tube side is 5-20 cm. Several internal component units 20 are arranged inside the tube side. The spacing between two adjacent internal component units can be 0.1-3 m. Each internal component unit 20 includes three rotatable blades 21. The blades have an auxiliary structure 22 for increasing material flow disturbance. The auxiliary structure 22 is a plate with serrations and holes. One side of the plate with serrations and holes is installed on the surface of the blade. On the blade on which the plate with serrations and holes is installed, the plate with serrations and holes is located on the feed side. The angle between the plate with serrations and holes and the surface of the blade is 75-90°.

[0054] In another specific implementation, such as Figure 1As shown, the microreactor includes a first material supply tank 1, a second material supply tank 2, a third material supply tank 3, a first material pump 4, a second material pump 5, a third material pump 6, a first microreactor 7, a first tubular reactor 8, a second microreactor 9, a second tubular reactor 10, a heat exchanger 11, and a post-processing device 12. The first material stream is fed through the first material supply tank 1 and via the first material pump 4; the second material stream is pumped through the second material supply tank 2 and via the second material pump 5; and the third material stream is pumped through the third material supply tank 3 and via the third material pump 6. The three material streams sequentially enter the first microreactor 7, the first tubular reactor 8, the second microreactor 9, and the second tubular reactor 10 for mixing and reaction. The resulting reacted material first enters the heat exchanger 11 for heat exchange, and then enters the post-processing device 12 for product separation. The first microreactor 7... Both the first tubular reactor 8 and the second tubular reactor 10 are plate-type microchannel reactors; the first tubular reactor 8 and the second tubular reactor 10 each include a tube side and a shell side. The length of the tubular reactor can be 1-50m. The central axis of the tube side is a hollow tube with heat extraction function. The inner diameter of the tube side is 5-20cm. Several internal component units 20 are arranged inside the tube side. The spacing between two adjacent internal component units can be 0.1-3m. Each internal component unit 20 includes three rotatable blades 21. The blades have an auxiliary structure 22 for increasing material flow disturbance. The auxiliary structure 22 is a plate with serrations and holes. One side of the plate with serrations and holes is installed on the surface of the blade. On the blade on which the plate with serrations and holes is installed, the plate with serrations and holes is located on the feed side. The angle between the plate with serrations and holes and the surface of the blade is 75-90°.

[0055] In another specific implementation, such as Figure 1As shown, the microreactor includes a first material supply tank 1, a second material supply tank 2, a third material supply tank 3, a first material pump 4, a second material pump 5, a third material pump 6, a first microreactor 7, a first tubular reactor 8, a second microreactor 9, a second tubular reactor 10, a heat exchanger 11, and a post-processing device 12. The first material stream is fed through the first material supply tank 1 and via the first material pump 4; the second material stream is pumped through the second material supply tank 2 and via the second material pump 5; and the third material stream is pumped through the third material supply tank 3 and via the third material pump 6. The three material streams sequentially enter the first microreactor 7, the first tubular reactor 8, the second microreactor 9, and the second tubular reactor 10 for mixing and reaction. The resulting reacted material first enters the heat exchanger 11 for heat exchange, and then enters the post-processing device 12 for product separation. The first microreactor 7 and the second... Each microreactor 9 is a microreactor plate, and the microreactor plate is heart-shaped or umbrella-shaped; the first tubular reactor 8 and the second tubular reactor 10 each include a tube side and a shell side. The length of the tubular reactor can be 1-50m. The central axis of the tube side is a hollow tube with heat extraction function. The inner diameter of the tube side is 5-20cm. Several internal component units 20 are arranged in the tube side. The spacing between two adjacent internal component units can be 0.1-3m. Each internal component unit 20 includes three rotatable blades 21. The blades have an auxiliary structure 22 for increasing material flow disturbance. The auxiliary structure 22 is a plate with serrations and holes. One side of the plate with serrations and holes is installed on the surface of the blade. On the blade on which the plate with serrations and holes is installed, the plate with serrations and holes is located on the feed side. The angle between the plate with serrations and holes and the surface of the blade is 75-90°.

[0056] The microreactor device of the present invention will be further illustrated below through embodiments. These embodiments are implemented based on the technical solution of the present invention, providing detailed implementation methods and specific operating procedures; however, the scope of protection of the present invention is not limited to the following embodiments.

[0057] Unless otherwise specified, the experimental methods used in the following embodiments are conventional methods in the art. Unless otherwise specified, the experimental materials used in the following embodiments are commercially available.

[0058] Example 1

[0059] This embodiment is in Figure 1The microreactor shown is implemented in a microreactor device, which includes a first material supply tank 1, a second material supply tank 2, a third material supply tank 3, a first material pump 4, a second material pump 5, a third material pump 6, a first microreactor 7, a first tubular reactor 8, a second microreactor 9, a second tubular reactor 10, a heat exchanger 11, and a post-processing device 12. A first stream of material is fed through the first material supply tank 1 and via the first material pump 4; a second stream of material is pumped through the second material supply tank 2 and via the second material pump 5; and a third stream of material is pumped through the third material supply tank 3 and via the third material pump 6. The three streams of material sequentially enter the first microreactor 7, the first tubular reactor 8, the second microreactor 9, and the second tubular reactor 10 for mixing and reaction. The resulting reacted material first enters the heat exchanger 11 for heat exchange, and then enters the post-processing device 12 for product separation. Among them, the first microreactor 7 and the second microreactor 9 are sheet-type microchannel reactors; the first tubular reactor 8 and the second tubular reactor 10 each include a shell side and a tube side. Several internal component units are arranged along the central axis of the tube side. Each internal component unit has rotatable blades. Plates with serrations and holes are vertically installed on the blades. The central axis of the tube side is a hollow tube.

[0060] The first material supply tank 1 is used to supply 98% concentrated sulfuric acid, the second material supply tank 2 is used to supply 95% concentrated nitric acid, and the third material supply tank 3 is used to supply chlorobenzene.

[0061] The feed mixture consists of 98% concentrated sulfuric acid, 95% concentrated nitric acid, and chlorobenzene, with a feed molar ratio of sulfuric acid:nitric acid:chlorobenzene of 2:2.3:1. (Following the attached...) Figure 1 As shown, three streams of material are continuously pumped into the reactor section by pumps. The microreactor is a plate-type microchannel reactor with a liquid holding capacity of 280 ml and a controlled temperature of 80℃. The first tubular reactor 8 has an inner diameter of 4 cm and a length of 20 m. Each internal component unit has 3 blades, and the angle between the plate with serrations and perforations and the surface of the blades is 75°. The spacing between internal component units is 0.2 m, and the controlled temperature is 95℃. The second microreactor 9 has a controlled temperature of 95℃. The second tubular reactor 10 has an inner diameter of 4 cm and a length of 30 m. Each internal component unit has 3 blades, and the angle between the plate with serrations and perforations and the surface of the blades is 75°. The spacing between internal component units is 0.2 m, and the controlled temperature is 100℃. The heat exchanger is the same as that of the microreactor, and the controlled temperature is 30℃. The product undergoes a subsequent separation device. After water and oil phase separation, the oil phase is washed with alkali, washed with water, and dried to obtain the product, which has a dinitrochlorobenzene content of 99.8%.

[0062] Example 2

[0063] The structure of the microreactor and the reactants used are the same as in Example 1.

[0064] The feed mixture consists of 98% concentrated sulfuric acid, 95% concentrated nitric acid, and chlorobenzene, with a feed molar ratio of sulfuric acid:nitric acid:chlorobenzene of 2:2.3:1. (Following the attached...) Figure 1 As shown, three streams of material are continuously pumped into the reactor section by pumps. The microreactor is a plate-type microchannel reactor with a liquid holding capacity of 280 ml and a controlled temperature of 80℃. The first tubular reactor 8 has an inner diameter of 4 cm and a length of 20 m. Each internal component unit has 4 blades, and the angle between the serrated and perforated plate and the blade surface is 75°. The spacing between internal component units is 0.2 m, and the controlled temperature is 95℃. The second microreactor 9 has a controlled temperature of 95℃. The second tubular reactor 10 has an inner diameter of 4 cm and a length of 30 m. Each internal component unit has 4 blades, and the angle between the serrated and perforated plate and the blade surface is 75°. The spacing between internal component units is 0.2 m, and the controlled temperature is 100℃. The heat exchanger is the same as that of the microreactor, and the controlled temperature is 30℃. The product undergoes a subsequent separation device. After water and oil phase separation, the oil phase is washed with alkali, washed with water, and dried to obtain the product, which has a dinitrochlorobenzene content of 99.8%.

[0065] Example 3

[0066] The structure of the microreactor and the reactants used are the same as in Example 1.

[0067] The feed mixture consists of 98% concentrated sulfuric acid, 95% concentrated nitric acid, and chlorobenzene, with a feed molar ratio of sulfuric acid:nitric acid:chlorobenzene of 2:2.3:1. (Following the attached...) Figure 1 As shown, three streams of material are continuously pumped into the reactor section by pumps. The microreactor is a plate-type microchannel reactor with a liquid holding capacity of 280 ml and a controlled temperature of 80℃. The first tubular reactor 8 has an inner diameter of 4 cm and a length of 20 m. Each internal component unit has 3 blades, and the angle between the serrated and perforated plate and the blade surface is 85°. The spacing between internal component units is 0.2 m, and the controlled temperature is 95℃. The second microreactor 9 has a controlled temperature of 95℃. The second tubular reactor 10 has an inner diameter of 4 cm and a length of 30 m. Each internal component unit has 3 blades, and the angle between the serrated and perforated plate and the blade surface is 85°. The spacing between internal component units is 0.2 m, and the controlled temperature is 100℃. The heat exchanger is the same as the microreactor, and the controlled temperature is 30℃. The product undergoes a subsequent separation device. After water and oil phase separation, the oil phase is washed with alkali, washed with water, and dried to obtain the product, which has a dinitrochlorobenzene content of 99.7%.

[0068] Example 4

[0069] The structure of the microreactor and the reactants used are the same as in Example 1.

[0070] The feed mixture consists of 98% concentrated sulfuric acid, 95% concentrated nitric acid, and chlorobenzene, with a feed molar ratio of sulfuric acid:nitric acid:chlorobenzene of 2:2.3:1. (Following the attached...) Figure 1As shown, three streams of material are continuously pumped into the reactor section by pumps. The microreactor is a plate-type microchannel reactor with a liquid holding capacity of 280 ml and a controlled temperature of 80℃. The first tubular reactor 8 has an inner diameter of 4 cm and a length of 20 m. Each internal component unit has 3 blades, and the angle between the plate with serrations and perforations and the surface of the blades is 75°. The spacing between internal component units is 0.1 m, and the controlled temperature is 95℃. The second microreactor 9 has a controlled temperature of 95℃. The second tubular reactor 10 has an inner diameter of 4 cm and a length of 30 m. Each internal component unit has 3 blades, and the angle between the plate with serrations and perforations and the surface of the blades is 75°. The spacing between internal component units is 0.1 m, and the controlled temperature is 100℃. The heat exchanger is the same as that of the microreactor, and the controlled temperature is 30℃. The product undergoes a subsequent separation device. After the water and oil phases are separated, the oil phase is washed with alkali, washed with water, and dried to obtain the product, which has a dinitrochlorobenzene content of 99.9%.

[0071] Example 5

[0072] The structure of the microreactor and the reactants used are the same as in Example 1.

[0073] The feed mixture consists of 98% concentrated sulfuric acid, 95% concentrated nitric acid, and chlorobenzene, with a feed molar ratio of sulfuric acid:nitric acid:chlorobenzene of 2:2.3:1. (Following the attached...) Figure 1 As shown, three streams of material are continuously pumped into the reactor section by pumps. The microreactor is a plate-type microchannel reactor with a liquid holding capacity of 280 ml and a controlled temperature of 80℃. The first tubular reactor 8 has an inner diameter of 4 cm and a length of 20 m. Each internal component unit has 3 blades, and the angle between the plate with serrations and perforations and the surface of the blades is 75°. The spacing between internal component units is 1 m, and the controlled temperature is 95℃. The second microreactor 9 has a controlled temperature of 95℃. The second tubular reactor 10 has an inner diameter of 4 cm and a length of 30 m. Each internal component unit has 3 blades, and the angle between the plate with serrations and perforations and the surface of the blades is 75°. The spacing between internal component units is 1 m, and the controlled temperature is 100℃. The heat exchanger is the same as that of the microreactor, and the controlled temperature is 30℃. The product undergoes a subsequent separation device. After water and oil phase separation, the oil phase is washed with alkali, washed with water, and dried to obtain the product, which has a dinitrochlorobenzene content of 99.6%.

[0074] Example 6

[0075] The structure of the microreactor and the reactants used are the same as in Example 1.

[0076] The feed mixture consists of 98% concentrated sulfuric acid, 95% concentrated nitric acid, and chlorobenzene, with a feed molar ratio of sulfuric acid:nitric acid:chlorobenzene of 2:2.3:1. (Following the attached...) Figure 1As shown, three streams of material are continuously pumped into the reactor section by pumps. The microreactor is a plate-type microchannel reactor with a liquid holding capacity of 400 ml and a controlled temperature of 80℃. The first tubular reactor 8 has an inner diameter of 4 cm and a length of 20 m. Each internal component unit has 3 blades, and the angle between the plate with serrations and perforations and the surface of the blades is 75°. The spacing between internal component units is 0.2 m, and the controlled temperature is 95℃. The second microreactor 9 has a controlled temperature of 95℃. The second tubular reactor 10 has an inner diameter of 4 cm and a length of 30 m. Each internal component unit has 3 blades, and the angle between the plate with serrations and perforations and the surface of the blades is 75°. The spacing between internal component units is 0.2 m, and the controlled temperature is 100℃. The heat exchanger is the same as that of the microreactor, and the controlled temperature is 30℃. The product undergoes a subsequent separation device. After water and oil phase separation, the oil phase is washed with alkali, washed with water, and dried to obtain the product, which has a dinitrochlorobenzene content of 99.6%.

[0077] Example 7

[0078] The structure of the microreactor and the reactants used are the same as in Example 1.

[0079] The feed mixture consists of 98% concentrated sulfuric acid, 95% concentrated nitric acid, and chlorobenzene, with a feed molar ratio of sulfuric acid:nitric acid:chlorobenzene of 2:2.3:1. (Following the attached...) Figure 1 As shown, three streams of material are continuously pumped into the reactor section by pumps. The microreactor is a plate-type microchannel reactor with a liquid holding capacity of 400 ml and a controlled temperature of 80℃. The first tubular reactor 8 has an inner diameter of 12 cm and a length of 6 m. Each internal component unit has 3 blades, and the angle between the plate with serrations and perforations and the surface of the blades is 75°. The spacing between internal component units is 0.2 m, and the controlled temperature is 95℃. The second microreactor 9 has a controlled temperature of 95℃. The second tubular reactor 10 has an inner diameter of 12 cm and a length of 6 m. Each internal component unit has 3 blades, and the angle between the plate with serrations and perforations and the surface of the blades is 75°. The spacing between internal component units is 0.2 m, and the controlled temperature is 100℃. The heat exchanger is the same as that of the microreactor, and the controlled temperature is 30℃. The product undergoes a subsequent separation device. After water and oil phase separation, the oil phase is washed with alkali, washed with water, and dried to obtain the product, which has a dinitrochlorobenzene content of 99.6%.

[0080] Example 8

[0081] The structure of the microreactor and the reactants used are the same as in Example 1.

[0082] The feed mixture consists of 98% concentrated sulfuric acid, 95% concentrated nitric acid, and chlorobenzene, with a feed molar ratio of sulfuric acid:nitric acid:chlorobenzene of 2:2.3:1. (Following the attached...) Figure 1As shown, three streams of material are continuously pumped into the reactor section by pumps. The microreactor is a plate-type microchannel reactor with a liquid holding capacity of 400 ml and a controlled temperature of 80℃. The first tubular reactor 8 has an inner diameter of 12 cm and a length of 6 m. Each internal component unit has 3 blades, and the angle between the plate with serrations and perforations and the surface of the blades is 75°. The spacing between internal component units is 0.1 m, and the controlled temperature is 95℃. The second microreactor 9 has a controlled temperature of 95℃. The second tubular reactor 10 has an inner diameter of 12 cm and a length of 6 m. Each internal component unit has 3 blades, and the angle between the plate with serrations and perforations and the surface of the blades is 75°. The spacing between internal component units is 0.1 m, and the controlled temperature is 100℃. The heat exchanger is the same as that of the microreactor, and the controlled temperature is 30℃. The product undergoes a subsequent separation device. After the water and oil phases are separated, the oil phase is washed with alkali, washed with water, and dried to obtain the product, which has a dinitrochlorobenzene content of 99.7%.

[0083] Example 9

[0084] The structure of the microreactor and the reactants used are the same as in Example 1.

[0085] The feed mixture consists of 98% concentrated sulfuric acid, 95% concentrated nitric acid, and chlorobenzene, with a feed molar ratio of sulfuric acid:nitric acid:chlorobenzene of 2:2.3:1. (Following the attached...) Figure 1 As shown, three streams of material are continuously pumped into the reactor section by pumps. The microreactor is a plate-type microchannel reactor with a liquid holding capacity of 400 ml and a controlled temperature of 80℃. The first tubular reactor 8 has an inner diameter of 20 cm and a length of 4 m. Each internal component unit has 3 blades, and the angle between the plate with serrations and perforations and the surface of the blades is 75°. The spacing between internal component units is 0.1 m, and the controlled temperature is 95℃. The second microreactor 9 has a controlled temperature of 95℃. The second tubular reactor 10 has an inner diameter of 20 cm and a length of 4 m. Each internal component unit has 3 blades, and the angle between the plate with serrations and perforations and the surface of the blades is 75°. The spacing between internal component units is 0.1 m, and the controlled temperature is 100℃. The heat exchanger is the same as that of the microreactor, and the controlled temperature is 30℃. The product undergoes a subsequent separation device. After water and oil phase separation, the oil phase is washed with alkali, washed with water, and dried to obtain the product, which has a dinitrochlorobenzene content of 99.7%.

[0086] Comparative Example 1

[0087] Based on Example 1, the tubes in both the first tubular reactor 8 and the second tubular reactor 10 were set to be empty tubes, without any internal component units. As a result, the product dinitrochlorobenzene content was 85.1%.

[0088] Example 10

[0089] Based on Example 1, the reaction apparatus consists of only one microreactor and one tubular reactor.

[0090] The reactor uses 98% concentrated sulfuric acid, 65% nitric acid, and isooctanol, with a feed molar ratio of sulfuric acid:nitric acid:isooctanol of 1.1:1.05:1. The three materials are continuously pumped into the reactor section. The microreactor is a two-plate microchannel reactor with a single plate holding capacity of 280 ml and a controlled temperature of 5°C. The tubular reactor has an inner diameter of 7 cm and a length of 16 m. Each internal component unit has three blades, with a serrated and perforated plate forming an 80° angle with the blade surface. The spacing between internal component units is 0.1 m, and the controlled temperature is 10°C. The heat exchanger is controlled at 25°C. The product undergoes subsequent separation. After water-oil phase separation, the oil phase is washed with alkali, water, and dried to obtain the product, isooctyl nitrate, with a purity of 99.2%.

[0091] Comparative Example 2

[0092] Based on Example 1, the tubular reactor was configured with empty tubes throughout, without any internal components. As a result, the purity of the product isooctyl nitrate was 83.2%.

[0093] As can be seen from the above embodiments and comparative examples, the microreactor according to the present invention can achieve better reaction results by setting internal component units with specific structures in the tube side of the tubular reactor.

[0094] The preferred embodiments of the present invention have been described in detail above; however, the present invention is not limited thereto. Within the scope of the inventive concept, various simple modifications can be made to the technical solutions of the present invention, including combinations of various technical features in any other suitable manner. These simple modifications and combinations should also be considered as the content disclosed in the present invention and are all within the protection scope of the present invention.

Claims

1. A microreactor device, comprising at least one microreactor and at least one tubular reactor connected in series, characterized in that, The tubular reactor includes a tube side and a shell side. The tube side is provided with several internal component units. Each internal component unit includes two or more rotatable blades. The material flow impacts the blades, causing them to rotate. The blades have an auxiliary structure for increasing material flow disturbance. The auxiliary structure is a plate with serrations and holes. One side of the plate with serrations and holes is mounted on the surface of the blade. On the blade with the plate with serrations and holes mounted, the plate with serrations and holes is located on the feed side. The angle between the plate with serrations and holes and the surface of the blade is 45-90°. The saw teeth and the holes are respectively set independently. The holes are located at the end of the plate near the blade, and the saw teeth are located at the edge of the plate away from the blade.

2. The microreactor according to claim 1, characterized in that, Several internal component units are arranged side by side along the central axis of the tube.

3. The microreactor according to claim 2, characterized in that, The central axis of the tube is a hollow tube.

4. The microreactor according to claim 1, characterized in that, Each internal component unit includes three or four rotatable blades.

5. The microreactor according to claim 1, characterized in that, The tubular reactor has an inner diameter of 1-40 cm and a length of 0.5-100 m.

6. The microreactor according to claim 5, characterized in that, The tubular reactor has an inner diameter of 5-20 cm and a length of 1-50 m.

7. The microreactor according to any one of claims 1-5, characterized in that, The microreactor device includes two or more microreactors and two or more tubular reactors, with the microreactors and tubular reactors arranged at intervals.

8. The microreactor according to claim 7, characterized in that, Along the flow direction of the reactants, the first reactor is a microreactor, and the last reactor is a tubular reactor.

9. The microreactor according to any one of claims 1-5, characterized in that, The microreactor is a microchannel or a microreactor plate with mixing and heat dissipation functions.

10. The microreactor according to claim 9, characterized in that, The microreactor sheet is heart-shaped or umbrella-shaped.

11. The microreactor according to any one of claims 1-5, characterized in that, The microreactor also includes multiple material supply channels for supplying reactants and a post-processing device for processing the reactants.

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