Electric field enhanced high-heat-release multiphase continuous flow microreactor
By using the structure of the coolant flow channels on both sides and the inner graphite electrode plate and the snake-shaped microchannel in the high-exothermal multi-phase continuous flow micro reactor, the problem of poor electric field strengthening and heat removal is solved, and high efficiency is achieved , safe reaction process and high-volume production.
Patent Information
- Application Number
- CN202411380876.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-30
- Publication Date
- 2024-12-31
AI Technical Summary
The existing high-exothermic multiphase continuous flow reactors are difficult to have or have poor results in both electric field strengthening and heat exchange strengthening, and there is a problem of channel blockage, which affects the reaction yield and safety.
An electric field-strengthening high-exothermal multi-phase continuous flow micro reactor was designed, and the structure in which the coolant flow channels on both sides and the inner graphite electrode plates were in contact with the snake-shaped microchannel was designed to achieve full coverage of the electric field and efficient heat removal, reducing blockage. Risk, improve reaction yield and safety.
It significantly improves reaction yield and safety, realizes the multifunctional integration of electric field strengthening and efficient heat removal, and ensures high mass production and operation safety.
Smart Images
Figure CN119215806A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the field of micro-chemical engineering and its application, and in particular to an electric field enhanced high heat release multi-phase continuous flow micro-reactor. Background Art
[0002] Some highly exothermic reactions, such as nitro-containing reactions and peroxidation reactions, are often accompanied by the formation of solid products. However, these reactions are highly exothermic and heat is easily accumulated locally in the reactor, causing side reactions.
[0003] In order to avoid the occurrence of side reactions and improve the reaction yield, strategies for such reactions include structurally enhanced heat exchange and external electric field enhancement. In the chemical industry, traditional kettle reactors are still used for such reactions. Their overall mass transfer and heat transfer performance is poor, resulting in a decrease in reaction selectivity and the generation of by-products. At the same time, heat accumulation poses a major safety hazard, and strengthening measures for such reactors are difficult to achieve. Therefore, it is urgent to seek new technologies to solve the problems of traditional reactors for such reactions.
[0004] Microchannel reactor technology has thus emerged. As a flow chemical reactor with a channel size in the range of 10μm-3mm, its small channel size and high specific surface area can provide more uniform temperature distribution and stronger mixing effect, thereby improving the selectivity and yield of the reaction, and is suitable for a variety of intensification methods. Therefore, microreactors have broad application prospects, especially in the field of high exothermic continuous flow reactions. By precisely controlling the reaction conditions and process intensification, a more efficient, safe and sustainable reaction process can be achieved.
[0005] Among the existing microreactors, the plate-type microreactor is more compact in structure and has a higher specific surface area. It can enhance heat exchange through the cooling flow channels in the structure. However, for high-exothermic multiphase systems that require both electric field enhancement and heat exchange enhancement to improve the reaction yield, the existing plate-type reactors rarely have electrode parts in their structures, or have problems such as poor electric field effect and easy channel blockage.
[0006] The present application is compared with the prior art as follows: Patent CN 115928115 A_An electrochemical synthesis microreactor and its preparation method and application method Patent CN 115928115 A proposes an electrochemical synthesis microreactor and its preparation method and application method. It improves the design of the existing electrochemical synthesis microreactor in which reaction by-products are difficult to remove in time. By optimizing the structure of the insulating microchannel layer and the supporting substrate and coordinating the use of a separation membrane, a separation chamber for separating reaction by-products is realized. The reaction by-products are separated in time by purging protective gas without adding additional reagents, thereby realizing the timely separation of by-products. The electrochemical synthesis microreactor structure has low investment cost and simple manufacturing method.
[0007] Field and method of the invention The present invention proposes a high-exothermic multiphase continuous flow microreactor for electric field enhancement. Aiming at the problem that the electric field enhancement and heat exchange enhancement effects in the existing high-exothermic multiphase continuous flow reaction are difficult to have at the same time or the effect is not good, an improved design is made. The reaction heat is removed in time through the coolant flow channels on both sides, and the inner graphite electrode plate is in contact with the serpentine microchannel to form a microfluidic reaction area, so as to achieve full coverage of the contact area by the electric field, and reduce the possibility of blockage. The overall structure integrates electric field enhancement, high heat removal, and microfluidic reaction structure, which enhances and improves the heat exchange performance while increasing the electric field contact area, realizing multifunctional integration, compact structure, safe operation, and high-volume production, and improving production efficiency. Summary of the invention
[0008] In view of the shortcomings of the plate-type microreactor that replaces the traditional reactor, the present invention proposes an electric field enhanced high exothermic multiphase continuous flow microreactor, which has both an electric field enhancement structure and an enhanced heat transfer structure in structure, while effectively improving the electric field enhancement effect and the channel blockage problem, realizing the continuous preparation of high exothermic multiphase reaction products within a certain period, significantly improving the reaction yield, and the process is efficient and safe.
[0009] To achieve the above object, the technical solution adopted by the present invention is: A multiphase continuous flow microreactor for electric field enhanced high heat release, characterized in that: The invention comprises a first cooling channel assembly, a second cooling channel assembly and a microchannel plate located between the first cooling channel assembly and the second cooling channel assembly and connected to the first cooling channel assembly and the second cooling channel assembly, wherein the first cooling channel assembly comprises a first cooling channel structural plate and a first graphite electrode plate, and the second cooling channel assembly comprises a second graphite electrode plate and a second cooling channel structural plate. The first cooling channel structure plate has the same structure as the second cooling channel structure plate, and comprises a cooling channel plate, a rubber pad and an outer pressure plate which are connected and fixed in sequence. The cooling channel plate is provided with a serpentine cooling channel for the flow of cooling medium, the serpentine cooling channel is provided with a cooling medium inlet and a cooling medium outlet, the inner side of the cooling channel plate is provided with a first bottomed groove, the first graphite electrode plate and the second graphite electrode plate are respectively constrained and fixed by the first bottomed groove on the cooling channel plate; The first graphite electrode plate and the second graphite electrode plate are respectively provided with a first electrode mounting hole and a second electrode mounting hole for fixing the copper rod electrode. The first graphite electrode plate and the second graphite electrode plate are respectively provided with second bottom recesses, and the microchannel plate is constrained and fixed between the first graphite electrode plate and the second graphite electrode plate by the second bottom recesses. The microchannel plate is a place for the reaction of the reaction liquid, and is provided with a serpentine flow channel, and the two sides are respectively in close contact with the inner side of the first graphite electrode plate and the inner side of the second graphite electrode plate to form a fluid flow area, and the serpentine flow channel is provided with a reaction liquid inlet and a reaction product outlet, and the reaction liquid inlet includes a reaction liquid A inlet, a reaction liquid B inlet, and a reaction liquid C inlet. A reaction liquid injection port and a reaction liquid output port are respectively provided at the top and bottom of the cooling channel plate on the first cooling channel structure plate. The reaction liquid injection port has three ports, namely, a first reaction liquid injection port, a second reaction liquid injection port, and a third reaction liquid injection port. The first reaction liquid injection port, the second reaction liquid injection port, and the third reaction liquid injection port are respectively connected with the reaction liquid A inlet, the reaction liquid B inlet, and the reaction liquid C inlet to form a first reaction liquid inlet hole, a second reaction liquid inlet hole, and a third reaction liquid inlet hole, respectively. The reaction product outlet is connected with the reaction liquid output port to form a reaction product outlet hole.
[0010] In the above structure: the present invention proposes a high-exothermic multiphase continuous flow microreactor for electric field enhancement, comprising a first cooling channel structure plate, a first graphite electrode plate, a microchannel plate, a second graphite electrode plate and a second cooling channel structure plate stacked together in sequence, wherein the first and second cooling channel structure plates have similar structures and are composed of a cooling channel plate, a rubber pad and an outer pressure plate in sequence, a serpentine cooling channel for cooling medium flow is arranged on the cooling channel plate to ensure high-throughput coolant flow, and at the same time, the first graphite electrode plate and the second graphite electrode plate are installed and constrained on the inner side of the cooling channel plate, and the first graphite electrode plate and the second graphite electrode plate are both provided with a first electrode mounting hole and a second electrode mounting hole for fixing a copper rod electrode, which are used to generate an electric field for an external electrode, and the microchannel plate is a place for the reaction liquid to react, and a serpentine flow channel is arranged therein, which can prolong the reaction residence time and reduce the possibility of blockage, and three reaction liquid inlets and a reaction product outlet are opened thereon, and its two sides are respectively in close contact with the inner side of the first graphite electrode plate and the inner side of the second graphite electrode plate to form a fluid flow area, so as to achieve an electric field enhancement effect with a maximum contact area.
[0011] The top and bottom of the cooling channel plate are also respectively provided with a reaction liquid injection port and a reaction liquid output port, which are connected to the inner side of the cooling channel plate through an extended cylindrical long hole to form a corresponding first reaction liquid inlet hole, a second reaction liquid inlet hole, a third reaction liquid inlet hole, and a reaction product outlet hole for the reaction liquid to pass through.
[0012] The second cooling channel structural plate has the same outer structural composition as the first cooling channel structural plate, and both are made of stainless steel with good thermal conductivity. They can achieve continuous flow of cooling medium during the reaction, cover the entire reaction area, and remove reaction heat in time.
[0013] The microchannel plate is the place where the reaction liquid reacts. It is made of glass fiber board. While ensuring the microchannel, it has sufficient hardness. The length and width are both 150mm. It is equipped with a serpentine flow channel with a width and thickness of 3mm and a length of 2m. It can ensure the full flow of microfluids and extend the residence time. At the same time, it can avoid the blockage of the flow channel caused by particle generation. The two sides are respectively tightly attached to the inner side of the first graphite electrode plate and the inner side of the second graphite electrode plate to form a fluid flow area, realizing the electric field enhancement effect with the maximum contact area; the serpentine flow channel is provided with three reaction liquid inlets, including reaction liquid A inlet, reaction liquid B inlet, reaction liquid C inlet, and a reaction product outlet.
[0014] Before the three reaction liquids enter the continuous flow microreactor, the cooling medium is first introduced into the first cooling channel structural plate and the first cooling channel structural plate. Taking the first cooling channel structural plate as an example, the cooling medium is water. Water flows into the serpentine cooling channel through the cooling medium inlet on the cooling channel plate, and flows out from the cooling medium outlet after complete flow. The external refrigerator cools the water and circulates it in the first cooling channel structural plate and the first cooling channel structural plate to ensure that the temperature of the cooling medium is consistent.
[0015] The serpentine cooling channel is a heat sink structure. Setting it in a serpentine shape can ensure a certain flow rate. The overall cooling effect is excellent and meets the heating requirements of the highly exothermic reaction system.
[0016] Three reaction liquids, including reaction liquid A, reaction liquid B, and electrolyte C, enter the microchannel plate in sequence, and the external injection pump drives the reaction liquid and the reaction liquid through the polytetrafluoroethylene tube into the first reaction liquid injection port and the second reaction liquid injection port of the cooling channel plate respectively, and then successively reach the reaction liquid A inlet and the reaction liquid B inlet on the microchannel plate. The two reaction liquids contact, mix, and react in the serpentine flow channel on the microchannel plate. Subsequently, the electrolyte C is driven into the third reaction liquid injection port through the polytetrafluoroethylene tube by the injection pump, flows to the reaction liquid C inlet, and enters the serpentine flow channel to improve the reaction effect.
[0017] An external power supply is connected to the copper rod electrodes placed on the first electrode mounting hole and the second electrode mounting hole on the first graphite electrode plate and the second graphite electrode plate. The power supply voltage can be set to 3V. After the electrolyte C is introduced into the microreactor, it can be used to strengthen the electric field and reduce the generation of by-products.
[0018] During the reaction, the three reaction liquids mix and react in the serpentine flow channel, releasing a large amount of heat. At this time, the cooling medium water circulating in and out of the first cooling channel structure plate and the second cooling channel structure plate promptly draws out the heat generated by the reaction through graphite. The continuously flowing cooling medium can remove a large amount of reaction heat in time, reduce the risk of the experiment, reduce the generation of by-products, and improve the yield.
[0019] During the reaction process, the length of the serpentine flow channel is sufficient to extend the residence time and realize the continuous reaction of a batch of reaction liquids. For multiphase reactions that produce particulate products, the serpentine channel structure can reduce channel blockage caused by particle accumulation and ensure smooth flow during the reaction process.
[0020] After the reaction is finished, the reaction product flows out through the reaction product outlet on the serpentine flow channel on the microchannel plate, and finally flows out from the output liquid flow hole on the cooling flow channel plate and is collected.
[0021] It should be noted that before the reaction liquid enters the microreactor, a certain amount of solvent can be driven into the reactor first, which can flush out the tiny residual impurities in the microchannel plate and achieve the effect of polishing the microchannel; after the reaction is completed, the serpentine flow channel needs to be flushed clean with a solvent or a washing liquid, especially the participating particle products are completely flushed to avoid channel blockage due to residues during the next test.
[0022] It should be noted that when assembling the microreactor, attention should be paid to the order of assembly and the complete installation of all components. If leakage, circuit short circuit, etc. occur, the entire structure needs to be dismantled, checked and reinstalled.
[0023] Through the serpentine flow channel structure of sufficient length, while ensuring the reaction, it can avoid channel blockage caused by particle generation. At the same time, the first graphite electrode plate and the second graphite electrode plate on both sides cooperate with the microchannel plate to form a microchannel structure, which can ensure the electric field enhancement of the maximum contact area and improve the enhancement effect; through the flow of the cooling medium in the first cooling channel structure plate and the second cooling channel structure plate on both sides, the cooling of the entire cross-sectional area of the reaction is fully covered, and the heat generated by the reaction is removed in time. In one reaction cycle, it is possible to achieve electric field enhancement, immediate removal of highly exothermic heat, and successful generation and flow of multiphase particles, which improves the safety of the reaction, simplifies and makes the operation safer, and achieves an increase in the reaction yield. At the same time, it is conducive to the simultaneous reaction of multiple continuous flow microreactors, improves the generation efficiency, and helps to scale up the generation.
[0024] As a further improvement of the present invention, the outer side of the cooling channel plate is tightly attached to the rubber pad and is pressed by the outer pressure plate. The outer pressure plate is provided with an outer pressure plate countersunk hole, the rubber pad is provided with a rubber pad through hole, and the cooling channel plate is provided with a cooling channel plate bolt hole. The countersunk screws are passed through the outer pressure plate countersunk hole, the rubber pad through hole and the cooling channel plate bolt hole in sequence and tightened. The top of the cooling channel plate is provided with an electrode constraint hole for avoiding the copper rod electrode.
[0025] In the above structure: the outer side of the cooling channel plate is tightly attached to the rubber pad, which is pressed by the outer pressure plate. The countersunk screws pass through the countersunk hole of the outer pressure plate-the rubber pad through hole-the cooling channel plate bolt hole in sequence and are tightened to ensure the sealing. At the same time, an electrode restraint hole for avoiding the copper rod electrode is provided on the top to avoid the influence of the electrode on the physical structure when the overall structure is tightened.
[0026] As a further improvement of the present invention, an injection liquid circulation hole and an output liquid circulation hole are provided on the first graphite electrode plate, the aperture of the output liquid circulation hole is larger than the aperture of the injection liquid circulation hole, and the injection liquid circulation hole includes a first injection liquid circulation hole, a second injection liquid circulation hole, and a third injection liquid circulation hole. When one side of the first graphite electrode plate is placed tightly against the first bottom groove on the inner side of the cooling flow channel plate, the first reaction liquid injection port, the second reaction liquid injection port, and the third reaction liquid injection port are connected to the reaction liquid A inlet, the reaction liquid B inlet, and the reaction liquid C inlet respectively through the first injection liquid circulation hole, the second injection liquid circulation hole, and the third injection liquid circulation hole, and the reaction liquid output port is connected to the reaction product outlet through the output liquid circulation hole.
[0027] In the above structure: when one side of the first graphite electrode plate is placed tightly against the first bottom groove on the inner side of the cooling channel plate, the first reaction liquid injection port, the second reaction liquid injection port, and the third reaction liquid injection port are connected to the reaction liquid A inlet, the reaction liquid B inlet, and the reaction liquid C inlet respectively through the first injection liquid flow hole, the second injection liquid flow hole, and the third injection liquid flow hole, and the reaction liquid output port is connected to the reaction product outlet through the output liquid flow hole to achieve successful inflow and outflow of multiple streams of reaction liquid. The reason why the aperture of the output liquid flow hole is larger than the aperture of the injection liquid flow hole is that particles will be generated in the reaction. Increasing the aperture of the liquid outlet through hole can avoid the accumulation of particles and blockage of the channel due to insufficient physical size when the reaction product flows out, thereby ensuring smooth outflow of the reaction liquid.
[0028] As a further improvement of the present invention, a first O-ring groove is opened on the inner side of the cooling channel plate, which is respectively located at the first reaction liquid inlet hole, the second reaction liquid inlet hole, the third reaction liquid inlet hole and the reaction product outlet hole, and an O-ring is installed in the first O-ring groove.
[0029] As a further improvement of the present invention, a second O-ring groove is further opened on the inner side of the cooling channel plate, and O-rings are respectively installed in the second O-ring grooves to balance the sealing effect of the first O-ring grooves between the first reaction liquid inlet hole and the first injection liquid flow hole, between the second reaction liquid inlet hole and the second injection liquid flow hole, between the third reaction liquid inlet hole and the third injection liquid flow hole, and between the reaction product outlet hole and the output liquid flow hole.
[0030] In the above structure: four first O-ring grooves are provided, which are respectively located at the first reaction liquid inlet hole, the second reaction liquid inlet hole, the third reaction liquid inlet hole and the reaction product outlet hole. The reaction liquid is restricted from entering and exiting by embedding the O-ring, thereby playing a sealing role. Five second O-ring grooves are provided, which are used to balance the effects of the four first O-ring grooves during sealing and ensure smooth reaction liquid entry and exit.
[0031] As a further improvement of the present invention, one side of the microchannel plate is bonded to the first graphite electrode plate through the first bottom groove on the inner side thereof, and the other side is bonded to the second graphite electrode plate with a flat structure. The microchannel plate is clamped to form a microfluid flow area, and the area of all regions bonded to the serpentine flow channel on the microchannel plate is the area that generates an electric field when power is turned on.
[0032] In the above structure: one side of the microchannel plate is fitted with the second bottom groove on the inner side of the first graphite electrode plate, and the other side is fitted with the second graphite electrode plate with a flat structure. The microchannel plate is clamped to form a microfluid flow area, and the area of all areas fitted with the serpentine flow channel of the microchannel plate is the area where the electric field is generated when power is turned on, so that the electric field of the contact surface is fully covered to achieve the best electric field enhancement effect.
[0033] As a further improvement of the present invention, the first cooling channel structural plate and the second cooling channel structural plate are both provided with bolt holes for overall fastening connection, and the first cooling channel structural plate, the first graphite electrode plate, the microchannel plate, the second graphite electrode plate and the second cooling channel structural plate are tightly connected by bolts and nuts.
[0034] As a further improvement of the present invention, a T-shaped gasket tube is installed on the nut to isolate the transmission of current on the first cooling channel structure plate and the second cooling channel structure plate which are in contact with each other due to the connection of the positive and negative voltages to the first graphite electrode plate and the second graphite electrode plate.
[0035] In the above structure: the whole device is tightly connected by bolts and nuts, and a T-shaped gasket tube is installed on the nut to isolate the transmission of current on the first cooling channel structure plate and the second cooling channel structure plate which are in contact with each other due to the connection of the positive and negative voltages between the first graphite electrode plate and the second graphite electrode plate, thereby avoiding the overall short circuit caused by the connection to the circuit and ensuring the normal operation of the electric field on both sides of the microchannel plate.
[0036] Compared with the prior art, the present invention has the following significant advantages: The invention has clear structure, strong pertinence, relatively compact structure, efficient production and high integration degree.
[0037] The electric field strengthening effect is good. By fully fitting with both sides of the microfluidic flow channel, the electric field fully covers the contact area on the cross-section on both sides of the microchannel, thereby improving the electric field strengthening effect.
[0038] The cooling structure is reasonable and the effect is good. The cooling medium is successfully introduced into the microreactor through the cooling plates on both sides. The serpentine coolant flow channel has a large cooling flux, which can remove the high heat of the reaction in time and has a good cooling effect.
[0039] The residence time is extended and the possibility of blockage is reduced. Through the structure of the serpentine reaction microchannel, it has better anti-blocking performance when facing a system containing particle generation. At the same time, the channel is long enough to ensure sufficient reaction.
[0040] The overall structure integrates functional structures such as electric field enhancement, high heat removal, and microfluidic reaction, achieving multifunctional integration, with reasonable overall size and compact structure.
[0041] The operation is highly safe and flexible. The potential danger caused by heat accumulation can be avoided by timely removal of heat. At the same time, the reaction can be completed by simply operating the injection pump to feed.
[0042] It can realize multi-channel reaction with high production efficiency. At the same time, multiple continuous flow microreactors can carry out reactions to achieve high-batch production and improve production efficiency. BRIEF DESCRIPTION OF THE DRAWINGS
[0043] Figure 1 It is a schematic diagram of the three-dimensional overall structure of the present invention; Figure 2 It is an exploded schematic diagram of the three-dimensional plate structure of the present invention; Figure 3 This is a schematic diagram of the split structure of the first cooling channel structural plate of the present invention; Figure 4 It is a front schematic diagram of a cooling channel plate on a first cooling channel structure plate of the present invention; Figure 5 A schematic diagram of the back side of the cooling channel plate on the first cooling channel structure plate of the present invention Figure 6 This is a schematic diagram of the planar structure of the first graphite electrode plate of the present invention; Figure 7 It is a schematic diagram of the planar structure of the microchannel plate of the present invention; Figure 8 It is a schematic diagram of the position structure of the graphite electrode plate and the microchannel plate of the present invention; Fig. 9 This is a schematic diagram of the position structure of the first cooling channel structure plate-first graphite electrode plate-microchannel plate of the present invention; Fig.10 Schematic diagram of the position relationship of the reaction liquid inlet of the present invention.
[0044] Attachment Tags: 1. First cooling channel structure plate; 2. First graphite electrode plate; 3. Microchannel plate; 4. Second graphite electrode plate; 5. Second cooling channel structure plate; 6. O-ring; 7. T-type gasket tube; 8. Bolt; 9. Nut; 11. Cooling channel plate; 12. Rubber pad; 13. Outer pressure plate; 111. Serpentine cooling channel; 112. Cooling medium inlet; 113. Cooling medium outlet; 1141. First reaction liquid injection port; 1142. Second reaction liquid injection port; 1143. Third reaction liquid injection port; 115. Reaction liquid outlet; 116. Inner side of cooling channel plate; 117. Bolt hole; 118. Electrode constraint hole; 119. Cooling channel plate bolt hole ; 1161, first reaction liquid inlet hole; 1162, second reaction liquid inlet hole; 1163, third reaction liquid inlet hole; 1164, reaction product outlet hole; 1165, first sink groove; 1166, first O-ring groove; 121, rubber pad through hole; 131, outer pressure plate sink hole; 21, second sink groove; 22, first injection liquid flow hole; 23, second injection liquid flow hole; 24, third injection liquid flow hole; 25, output liquid flow hole; 26, first electrode mounting hole; 31, serpentine flow channel; 32, reaction liquid A inlet; 33, reaction liquid B inlet; 34, reaction liquid C inlet; 35, reaction product outlet; 41, second electrode mounting hole. DETAILED DESCRIPTION
[0045] The present invention is further described in detail below in conjunction with the accompanying drawings and specific embodiments: See also Figure 1-10 The present invention provides an electrode-enhanced high-exothermic multiphase continuous flow microreactor, comprising a first cooling channel assembly, a second cooling channel assembly, and a microchannel plate 3 located between the first cooling channel assembly and the second cooling channel assembly and connected to the two. The first cooling channel assembly comprises a first cooling channel structural plate 1 and a first graphite electrode plate 2, and the second cooling channel assembly comprises a second graphite electrode plate 4 and a second cooling channel structural plate 5. The first cooling channel structure plate 1 has the same structure as the second cooling channel structure plate 5, and includes a cooling channel plate 11, a rubber pad 12 and an outer pressure plate 13 which are connected and fixed in sequence. The cooling channel plate 11 is provided with a serpentine cooling channel 111 for the flow of cooling medium, and the serpentine cooling channel 111 is provided with a cooling medium inlet 112 and a cooling medium outlet 113. The inner side of the cooling channel plate 11 is provided with a first bottomed groove 1165, and the first graphite electrode plate 2 and the second graphite electrode plate 4 are respectively constrained and fixed by the first bottomed groove 1165 on the cooling channel plate 11; The first graphite electrode plate 2 and the second graphite electrode plate 4 are respectively provided with a first electrode mounting hole 26 and a second electrode mounting hole 41 for fixing the copper rod electrode. The first graphite electrode plate 2 and the second graphite electrode plate 4 are respectively provided with a second bottom recess 21, and the microchannel plate 3 is constrained and fixed between the first graphite electrode plate 2 and the second graphite electrode plate 4 by the second bottom recess 21. The microchannel plate 3 is a place for the reaction of the reaction liquid, and is provided with a serpentine flow channel 31, and its two sides are respectively in close contact with the inner side of the first graphite electrode plate 2 and the inner side of the second graphite electrode plate 4 to form a fluid flow area. The serpentine flow channel 31 is provided with a reaction liquid inlet and a reaction product outlet 35, and the reaction liquid inlet includes a reaction liquid A inlet 32, a reaction liquid B inlet 33, and a reaction liquid C inlet 34. A reaction liquid injection port and a reaction liquid output port 115 are respectively provided at the top and bottom of the cooling channel plate 11 on the first cooling channel structure plate 1. The reaction liquid injection port has three portions, namely a first reaction liquid injection port 1141, a second reaction liquid injection port 1142, and a third reaction liquid injection port 1143. The first reaction liquid injection port 1141, the second reaction liquid injection port 1142, and the third reaction liquid injection port 1143 are respectively connected to the reaction liquid A inlet 32, the reaction liquid B inlet 33, and the reaction liquid C inlet 34 to form a first reaction liquid inlet hole 1161, a second reaction liquid inlet hole 1162, and a third reaction liquid inlet hole 1163. The reaction product output port 35 is connected to the reaction liquid output port 115 to form a reaction product outlet hole 1164.
[0046] The outer side of the cooling channel plate 11 is tightly attached to the rubber pad 12 and is pressed by the outer pressure plate 13. The outer pressure plate 13 is provided with an outer pressure plate countersunk hole 131, and the rubber pad 12 is provided with a rubber pad through hole 121. The cooling channel plate 11 is provided with a cooling channel plate bolt hole 119. The countersunk screws are sequentially passed through the outer pressure plate countersunk hole 131, the rubber pad through hole 121 and the cooling channel plate bolt hole 119 and tightened. The top of the cooling channel plate 11 is provided with an electrode restraint hole 118 for avoiding the copper rod electrode.
[0047] A first O-ring groove 1166 is opened on the inner side of the cooling channel plate 11 , which is respectively located at the first reaction liquid inlet hole 1161 , the second reaction liquid inlet hole 1162 , the third reaction liquid inlet hole 1163 and the reaction product outlet hole 1164 , and an O-ring 6 is installed in the first O-ring groove 1166 .
[0048] A second O-ring groove is also provided on the inner side of the cooling channel plate 11, in which an O-ring 6 is installed respectively, for balancing the sealing effect of the first O-ring groove 1166 between the first reaction liquid inlet hole 1161 and the first injection liquid circulation hole 22, between the second reaction liquid inlet hole 1162 and the second injection liquid circulation hole 23, between the third reaction liquid inlet hole 1163 and the third injection liquid circulation hole 24, and between the reaction product liquid outlet hole 1164 and the output liquid circulation hole 25.
[0049] One side of the microchannel plate 3 is bonded to the first graphite electrode plate 2 through the first bottom groove 1165 on the inner side thereof, and the other side is bonded to the second graphite electrode plate 4 with a flat structure. The microchannel plate 3 is clamped to form a microfluid flow area, and the area of all regions bonded to the serpentine flow channel 31 on the microchannel plate 3 is the area where an electric field is generated when power is turned on.
[0050] The first cooling channel structural plate 1 and the second cooling channel structural plate 5 are both provided with bolt holes 117 for integral fastening connection, and the first cooling channel structural plate 1, the first graphite electrode plate 2, the microchannel plate 3, the second graphite electrode plate 4 and the second cooling channel structural plate 5 are tightly connected by bolts 8 and nuts 9.
[0051] A T-shaped gasket tube 7 is installed on the nut 9 to isolate the first graphite electrode plate 2 and the second graphite electrode plate 4 from the transmission of current on the first cooling channel structure plate 1 and the second cooling channel structure plate 5 which are in contact with each other due to the connection of positive and negative voltages.
[0052] The present invention proposes a multiphase continuous flow microreactor for electrode strengthening and high heat release, comprising a first cooling channel structure plate 1, a first graphite electrode plate 2, a microchannel plate 3, a second graphite electrode plate 4 and a second cooling channel structure plate 5 stacked in sequence, wherein the first and second cooling channel structure plates 5 have similar structures and are composed of a cooling channel plate 11, a rubber pad 12 and an outer pressure plate 13 in sequence, a serpentine cooling channel 111 for cooling medium to flow is arranged on the cooling channel plate 11, ensuring high-throughput coolant flow, and at the same time, a first graphite electrode plate is installed on the inner side of the cooling channel plate 11 to constrain the first graphite electrode plate. 2 and a second graphite electrode plate 4, the first graphite electrode plate 2 and the second graphite electrode plate 4 are both provided with a first electrode mounting hole 26 and a second electrode mounting hole 41 for fixing a copper rod electrode, which are used for external electrodes to generate an electric field, the microchannel plate 3 is a place for the reaction liquid to react, and a serpentine flow channel 31 is arranged therein, which can prolong the reaction residence time and reduce the possibility of blockage, and three reaction liquid inlets and a reaction product outlet 35 are arranged thereon, and the two sides thereof are respectively closely attached to the inner side of the first graphite electrode plate 2 and the inner side of the second graphite electrode plate 4, forming a fluid flow area, thereby achieving an electric field strengthening effect with a maximum contact area.
[0053] The top and bottom of the cooling channel plate 11 are also respectively provided with a reaction liquid injection port and a reaction liquid output port 115, which are connected to the inner side of the cooling channel plate 11 through an extended cylindrical long hole, forming a corresponding first reaction liquid inlet hole 1161, a second reaction liquid inlet hole 1162, a third reaction liquid inlet hole 1163, and a reaction product outlet hole 1164 for the reaction liquid to pass through.
[0054] The second cooling channel structural plate 5 has the same outer structural composition as the first cooling channel structural plate 1 and is made of stainless steel with good thermal conductivity. It can realize the continuous flow of cooling medium during the reaction process, cover the entire reaction area, and remove the reaction heat in time.
[0055] The microchannel plate 3 is the place where the reaction liquid reacts. It is made of glass fiber board. While ensuring the microchannel, it has sufficient hardness. The length and width are both 150mm. It is equipped with a serpentine flow channel 31 with a width and thickness of 3mm and a length of 2m. It can ensure the full flow of microfluids and extend the residence time. At the same time, it can avoid the blockage of the flow channel caused by particle generation. The two sides are respectively tightly attached to the inner side of the first graphite electrode plate 2 and the inner side of the second graphite electrode plate 4 to form a fluid flow area, realizing the electric field strengthening effect with the maximum contact area; the serpentine flow channel 31 is provided with three reaction liquid inlets, including a reaction liquid A inlet 32, a reaction liquid B inlet 33, a reaction liquid C inlet 34, and a reaction product outlet 35.
[0056] Before the three streams of reaction liquid enter the continuous flow microreactor, the cooling medium is first introduced into the first cooling channel structural plate 1 and the first cooling channel structural plate 1. Taking the first cooling channel structural plate 1 as an example, the cooling medium is water. The water flows into the serpentine cooling channel 111 through the cooling medium inlet 112 on the cooling channel plate 11, and flows out from the cooling medium outlet 113 after complete flow. The external refrigerator cools the water and circulates it in the first cooling channel structural plate 1 and the first cooling channel structural plate 1 to ensure that the temperature of the cooling medium is consistent.
[0057] The serpentine cooling channel 111 is a heat sink structure, and setting it in a serpentine shape can ensure a certain flow rate, and the overall cooling effect is excellent, meeting the heating requirements of the highly exothermic reaction system.
[0058] Three reaction liquids, including reaction liquid A, reaction liquid B, and electrolyte C, enter the microchannel plate 3 in sequence. The external injection pump drives the reaction liquid and the reaction liquid through the polytetrafluoroethylene tube into the first reaction liquid injection port 1141 and the second reaction liquid injection port 1142 on the cooling channel plate 11 respectively, and then successively reach the reaction liquid A inlet 32 and the reaction liquid B inlet 33 on the microchannel plate 3. The two reaction liquids contact, mix, and react in the serpentine channel 31 on the microchannel plate 3. Subsequently, the electrolyte C is driven into the third reaction liquid injection port 1143 through the polytetrafluoroethylene tube by the injection pump, flows to the reaction liquid C inlet 34, and enters the serpentine channel 31 to enhance the reaction.
[0059] An external power supply is connected to the copper rod electrodes placed on the first electrode mounting hole 26 and the second electrode mounting hole 41 on the first graphite electrode plate 2 and the second graphite electrode plate 4. The power supply voltage can be set to 3V. After the electrolyte C is introduced into the microreactor, it can be used to strengthen the electric field and reduce the generation of by-products.
[0060] During the reaction, the three reaction liquids mix and react in the serpentine flow channel 31, releasing a large amount of heat. At this time, the cooling medium water circulating in and out of the first cooling channel structure plate 1 and the second cooling channel structure plate 5 promptly draws out the heat generated by the reaction through the graphite. The continuously flowing cooling medium can promptly remove a large amount of reaction heat, reduce the risk of the experiment, reduce the generation of by-products, and improve the yield.
[0061] During the reaction process, the length of the serpentine flow channel 31 is sufficient to extend the residence time and realize the continuous reaction of a batch of reaction liquids. For multiphase reactions that produce particulate products, the serpentine channel structure can reduce channel blockage caused by particle accumulation and ensure smooth flow during the reaction process.
[0062] After the reaction is finished, the reaction product flows out through the reaction product outlet 35 on the serpentine flow channel 31 on the microchannel plate 3, and finally flows out from the output liquid flow hole 25 on the cooling flow channel plate 11 and is collected.
[0063] It should be noted that before the reaction liquid enters the microreactor, a certain amount of solvent can be driven into the reactor first, which can flush out the fine residual impurities in the microchannel plate 3 and achieve the effect of polishing the microchannel; after the reaction is completed, the serpentine flow channel 31 needs to be flushed clean with a solvent or a washing liquid, especially the participating particulate products are completely flushed to avoid channel blockage due to residues during the next test.
[0064] It should be noted that when assembling the microreactor, attention should be paid to the order of assembly and the complete installation of all components. If leakage, circuit short circuit, etc. occur, the entire structure needs to be dismantled, checked and reinstalled.
[0065] Through the serpentine flow channel 31 structure of sufficient length, while ensuring the reaction, the channel blockage caused by particle generation can be avoided. At the same time, the first graphite electrode plate 2 and the second graphite electrode plate 4 on both sides cooperate with the microchannel plate 3 to form a microchannel structure, which can ensure the electric field enhancement of the maximum contact area and improve the electric field enhancement effect; through the flow of the cooling medium in the first cooling channel structure plate 1 and the second cooling channel structure plate 5 on both sides, the cooling of the entire cross-sectional area of the reaction is fully covered, and the heat generated by the reaction is removed in time. In one reaction cycle, the electric field enhancement, the immediate removal of high exothermic heat, and the successful generation and flow of multiphase particles can be achieved, which improves the safety of the reaction, simplifies and secures the operation, and realizes the improvement of the reaction yield. At the same time, it is beneficial to the simultaneous reaction of multiple continuous flow microreactors, improves the generation efficiency, and helps to amplify the generation.
[0066] In this embodiment: the outer side of the cooling channel plate 11 is tightly attached to the rubber pad 12, which is pressed by the outer pressure plate 13. The countersunk screws pass through the outer pressure plate countersunk hole 131-rubber pad through hole 121-cooling channel plate bolt hole 119 in sequence and are tightened to ensure the sealing. At the same time, an electrode restraint hole 118 for avoiding the copper rod electrode is provided on the top to avoid the influence of the electrode on the physical structure when the overall structure is tightened.
[0067] In this embodiment: when one side of the first graphite electrode plate 2 is placed tightly against the first bottom groove 1165 on the inner side of the cooling flow channel plate 11, the first reaction liquid injection port 1141, the second reaction liquid injection port 1142, and the third reaction liquid injection port 1143 are connected to the reaction liquid A inlet 32, the reaction liquid B inlet 33, and the reaction liquid C inlet 34 respectively through the first injection liquid circulation hole 22, the second injection liquid circulation hole 23, and the third injection liquid circulation hole 24, and the reaction liquid output port 115 is connected to the reaction product outlet 35 through the output liquid circulation hole 25, so as to realize the successful inflow and outflow of multiple streams of reaction liquid. The reason why the aperture of the output liquid circulation hole 25 is larger than the aperture of the injection liquid circulation hole is that the reaction will produce particles. Increasing the aperture of the liquid outlet through hole can avoid the accumulation of particles and blockage of the channel due to insufficient physical size when the reaction product flows out, so as to ensure the smooth outflow of the reaction liquid.
[0068] In this embodiment: four first O-ring grooves 1166 are provided, namely, the first reaction liquid inlet hole 1161, the second reaction liquid inlet hole 1162, the third reaction liquid inlet hole 1163 and the reaction product outlet hole 1164. The O-ring 6 is embedded to restrict the inflow and outflow of the reaction liquid and play a sealing role. Five second O-ring grooves are provided to balance the effect of the four first O-ring grooves 1166 during sealing and ensure smooth inflow and outflow of the reaction liquid.
[0069] In this embodiment: one side of the microchannel plate 3 is fitted with the second bottom groove 21 on the inner side of the first graphite electrode plate 2, and the other side is fitted with the second graphite electrode plate 4 with a flat structure, and the microchannel plate 3 is clamped to form a microfluid flow area. The area of all regions fitted with the serpentine flow channel 31 of the microchannel plate 3 is the area where the electric field is generated when power is turned on, so that the electric field of the contact surface is fully covered to achieve the best electric field enhancement effect.
[0070] In this embodiment: the whole device is tightly connected by bolts 8 and nuts 9, and a T-shaped gasket tube 7 is installed on the nut 9 to isolate the first graphite electrode plate 2 and the second graphite electrode plate 4 from the transmission of current on the first cooling channel structure plate 1 and the second cooling channel structure plate 5 which are in contact with each other due to the connection of the positive and negative voltages, avoid the overall short circuit caused by the connection to the circuit, and ensure the normal operation of the electric field on both sides of the microchannel plate 3.
[0071] Based on the above technical solution: The invention has clear structure, strong pertinence, relatively compact structure, efficient production and high integration degree.
[0072] The electric field strengthening effect is good. By fully fitting with both sides of the microfluidic flow channel, the electric field area on the cross-section on both sides of the microchannel is fully covered, thereby improving the electric field strengthening effect.
[0073] The cooling structure is reasonable and the effect is good. The cooling medium is successfully introduced into the microreactor through the cooling plates on both sides. The serpentine coolant flow channel has a large cooling flux, which can remove the high heat of the reaction in time and has a good cooling effect.
[0074] The residence time is extended and the possibility of blockage is reduced. Through the structure of the serpentine reaction microchannel, it has better anti-blocking performance when facing a system containing particle generation. At the same time, the channel is long enough to ensure sufficient reaction.
[0075] The overall structure integrates functional structures such as electric field enhancement, high heat removal, and microfluidic reaction, achieving multifunctional integration, with reasonable overall size and compact structure.
[0076] The operation is highly safe and flexible. The potential danger caused by heat accumulation can be avoided by timely removal of heat. At the same time, the reaction can be completed by simply operating the injection pump to feed.
[0077] It can realize multi-channel reaction with high production efficiency. At the same time, multiple continuous flow microreactors can carry out reactions to achieve high-batch production and improve production efficiency.
[0078] The above description is only a preferred embodiment of the present invention and does not constitute any other form of limitation to the present invention. Any modification or equivalent change made based on the technical essence of the present invention still falls within the scope of protection required by the present invention.
Claims
1. A multiphase continuous flow microreactor for electric field intensification with high heat release, characterized in that: The invention comprises a first cooling channel assembly, a second cooling channel assembly and a microchannel plate (3) located between the first cooling channel assembly and the second cooling channel assembly and connected to the first cooling channel assembly and the second cooling channel assembly, wherein the first cooling channel assembly comprises a first cooling channel structure plate (1) and a first graphite electrode plate (2), and the second cooling channel assembly comprises a second graphite electrode plate (4) and a second cooling channel structure plate (5). The first cooling channel structure plate (1) has the same structure as the second cooling channel structure plate (5), and comprises a cooling channel plate (11), a rubber pad (12) and an outer pressure plate (13) which are connected and fixed in sequence. The cooling channel plate (11) is provided with a serpentine cooling channel (111) for the flow of a cooling medium, the serpentine cooling channel (111) is provided with a cooling medium inlet (112) and a cooling medium outlet (113), the inner side of the cooling channel plate (11) is provided with a first bottomed groove (1165), and the first graphite electrode plate (2) and the second graphite electrode plate (4) are respectively constrained and fixed by the first bottomed groove (1165) on the cooling channel plate (11); The first graphite electrode plate (2) and the second graphite electrode plate (4) are respectively provided with a first electrode mounting hole (26) and a second electrode mounting hole (41) for fixing the copper rod electrode. The first graphite electrode plate (2) and the second graphite electrode plate (4) are respectively provided with a second bottom recess (21), and the microchannel plate (3) is constrained and fixed between the first graphite electrode plate (2) and the second graphite electrode plate (4) by the second bottom recess (21). The microchannel plate (3) is a place for the reaction of the reaction liquid, and is provided with a serpentine flow channel (31), and its two sides are respectively closely attached to the inner side of the first graphite electrode plate (2) and the inner side of the second graphite electrode plate (4), forming a fluid flow area, and the serpentine flow channel (31) is provided with a reaction liquid inlet and a reaction product outlet (35), and the reaction liquid inlet includes a reaction liquid A inlet (32), a reaction liquid B inlet (33), and a reaction liquid C inlet (34). The top and bottom of the cooling channel plate (11) on the first cooling channel structure plate (1) are respectively provided with a reaction liquid injection port and a reaction liquid output port (115); the reaction liquid injection port has three portions, namely a first reaction liquid injection port (1141), a second reaction liquid injection port (1142), and a third reaction liquid injection port (1143); the first reaction liquid injection port (1141), the second reaction liquid injection port (1142), and the third reaction liquid injection port (1143) are respectively connected to the reaction liquid A inlet (32), the reaction liquid B inlet (33), and the reaction liquid C inlet (34) to form a first reaction liquid inlet hole (1161), a second reaction liquid inlet hole (1162), and a third reaction liquid inlet hole (1163); the reaction product outlet (35) is connected to the reaction liquid output port (115) to form a reaction product outlet hole (1164).
2. The multiphase continuous flow microreactor for electric field enhanced high heat release according to claim 1, characterized in that: The outer side of the cooling channel plate (11) is tightly attached to the rubber pad (12) and is pressed by the outer pressure plate (13). The outer pressure plate (13) is provided with an outer pressure plate countersunk hole (131). The rubber pad (12) is provided with a rubber pad through hole (121). The cooling channel plate (11) is provided with a cooling channel plate bolt hole (119). The countersunk screws are passed through the outer pressure plate countersunk hole (131), the rubber pad through hole (121) and the cooling channel plate bolt hole (119) in sequence and tightened. The top of the cooling channel plate (11) is provided with an electrode restraining hole (118) for avoiding the copper rod electrode.
3. The multiphase continuous flow microreactor for electric field enhanced high heat release according to claim 1, characterized in that: The first graphite electrode plate (2) is provided with an injection liquid circulation hole and an output liquid circulation hole (25), the aperture of the output liquid circulation hole (25) is larger than the aperture of the injection liquid circulation hole, and the injection liquid circulation hole comprises a first injection liquid circulation hole (22), a second injection liquid circulation hole (23), and a third injection liquid circulation hole (24). When one side of the first graphite electrode plate (2) is placed in close contact with the first bottomed groove (1165) on the inner side of the cooling channel plate (11), the first reaction liquid injection port (1141), the second reaction liquid injection port (1142), and the third reaction liquid injection port (1143) are respectively connected to the reaction liquid A inlet (32), the reaction liquid B inlet (33), and the reaction liquid C inlet (34) through the first injection liquid circulation hole (22), the second injection liquid circulation hole (23), and the third injection liquid circulation hole (24), and the reaction liquid output port (115) is connected to the reaction product outlet (35) through the output liquid circulation hole (25).
4. The multiphase continuous flow microreactor for electric field enhanced high heat release according to claim 3, characterized in that: A first O-ring groove (1166) is provided on the inner side of the cooling channel plate (11), which is respectively located at the first reaction liquid inlet hole (1161), the second reaction liquid inlet hole (1162), the third reaction liquid inlet hole (1163) and the reaction product outlet hole (1164), and an O-ring (6) is installed in the first O-ring groove (1166).
5. A multiphase continuous flow microreactor for electric field enhanced high heat release according to claim 3 or 4, characterized in that: A second O-ring groove is also provided on the inner side of the cooling channel plate (11), and an O-ring (6) is installed in each of the second O-ring grooves to balance the sealing effect of the first O-ring groove (1166) between the first reaction liquid inlet hole (1161) and the first injection liquid circulation hole (22), between the second reaction liquid inlet hole (1162) and the second injection liquid circulation hole (23), between the third reaction liquid inlet hole (1163) and the third injection liquid circulation hole (24), and between the reaction product outlet hole (1164) and the output liquid circulation hole (25).
6. The multiphase continuous flow microreactor for electric field enhanced high heat release according to claim 1, characterized in that: One side of the microchannel plate (3) is bonded to the first graphite electrode plate (2) via the first bottomed groove (1165) on the inner side thereof, and the other side is bonded to the second graphite electrode plate (4) having a flat plate structure. The microchannel plate (3) is clamped to form a microfluid flow area, and the area of all regions bonded to the serpentine flow channel (31) on the microchannel plate (3) is the area where an electric field is generated when power is supplied.
7. The multiphase continuous flow microreactor for electric field enhanced high heat release according to claim 1, characterized in that: The first cooling channel structure plate (1) and the second cooling channel structure plate (5) are both provided with bolt holes (117) for integrally fastening the connection, and the first cooling channel structure plate (1), the first graphite electrode plate (2), the microchannel plate (3), the second graphite electrode plate (4) and the second cooling channel structure plate (5) are tightly connected by bolts (8) and nuts (9).
8. The high heat release continuous flow microreactor for electric field enhancement according to claim 7, characterized in that: A T-shaped gasket tube (7) is installed on the nut (9) to isolate the first graphite electrode plate (2) and the second graphite electrode plate (4) from the transmission of current on the first cooling channel structure plate (1) and the second cooling channel structure plate (5) which are in contact with each other due to the connection of positive and negative voltages.