A microchannel reactor and fully automated sulfentrazone production process

Abstract

The present invention relates to the technical field of chemical reaction equipment, and discloses a microchannel reactor and a fully automated sulfentrazone production process. The microchannel reactor comprises a substrate, wherein a first channel is provided on one end surface of the substrate, an outermost vertical section serves as a liquid inlet end, a first groove is provided on the liquid inlet end, and a plug connector is provided on the first groove; another outermost vertical section serves as a liquid outlet end, a second groove is provided on the liquid outlet end, and the plug connector is provided on the second groove; a second channel connected to the vertical section is provided on the substrate, a water drop-shaped guide portion is formed between the second channel and the first channel, and the guide portion separates the first channel from the second channel; by providing the second channel, the present application can divert the fluid in the first channel, slow down the flow rate of the fluid, ensure sufficient reaction of the fluid, and the diverted fluid flows back into the first channel at the curved section, which further slows down the flow rate of the fluid, further improves the reaction time of the fluid, and has a good reaction effect.

Description

Technical Field

[0001] The present invention relates to the technical field of chemical reaction equipment, and in particular to a microchannel reactor and a fully automated sulfentrazone production process. Background Art

[0002] Microchannel reactors, also known as microreactors, typically feature small and diverse channels. They are devices fabricated from solid substrates using specialized micromachining techniques and can be used to conduct chemical reactions. Compared to conventional reactors, microchannel reactors offer advantages such as compact size, large surface area, continuous processing, and ease of scale-up. The unique structure of microreactors enables very high heat and mass transfer efficiencies, maintaining a near-constant temperature in the reaction layer, facilitating various chemical reactions and finding applications in a wide range of fields.

[0003] Chinese patent application number 201480064474.0 discloses a microchannel reactor, which is formed by arranging a flat plate-shaped upper plate and a flat plate-shaped lower plate to face each other, and the flat plate-shaped upper plate and the flat plate-shaped lower plate respectively have channels. The microchannel reactor is characterized in that the channels include: one or more introduction channels, into which different fluids are introduced respectively; a mixing channel, through which the fluids introduced into the introduction channels meet and pass through the mixing channel; and a discharge channel, through which the fluids met through the mixing channel are discharged; the mixing channel includes a main channel and one or more branch channels, the main channel extends from the introduction channel to the discharge channel, the branch channel diverges from the main channel and terminates in the middle, and by repeatedly mixing the branched and met fluids, the fluids undergo a mixing process of branching in an upward / downward direction and then meeting each other in a left / right direction.

[0004] The flow channel of the microchannel reactor is a zigzag flow path. By extending the flow path, the fluid is fully reacted, but the flow rate is still relatively fast, and the adequacy of the fluid reaction process needs to be improved. Summary of the Invention

[0005] The object of the present invention is to provide a microchannel reactor and a fully automated sulfentrazone production process, which solve the problem of the existing microchannel reactor having a relatively fast flow rate and insufficient reaction as mentioned in the background art.

[0006] The technical solution adopted by the present invention is as follows: a microchannel reactor, comprising a substrate, the substrate being rectangular in shape, a first channel being provided on one end face of the substrate, the first channel being composed of a plurality of vertical segments and a plurality of circular arc segments, the vertical segments and the circular arc segments being arranged at intervals to form a serpentine-shaped first channel; an outermost vertical segment being used as a liquid inlet end, the liquid inlet end being provided with a first groove, the first groove being provided with a plug connector; another outermost vertical segment being used as a liquid outlet end, the liquid outlet end being provided with a second groove, the second groove being provided with the plug connector; a second channel being provided on the substrate and being connected to the vertical segment, second channels being provided on both sides of the vertical segment, the plurality of second channels being arranged at equal intervals from top to bottom, and the positions of the second channels on both sides being staggered, the second channel being composed of a slanted segment and a curved segment, the slanted segment being used as the upstream side through which the fluid flows, and the curved segment being used as the downstream side through which the fluid flows, a water drop-shaped guide portion being formed between the second channel and the first channel, the guide portion separating the first channel from the second channel.

[0007] First springs are provided on opposite surfaces of the two substrates. The number of the first springs is at least 6, and each group of three first springs is arranged from top to bottom.

[0008] The clamping member includes a first carrier connected to the cover body, the number of the first carriers is two, the two first carriers are symmetrically arranged, the first carriers are slidably connected to the first guide rods, the number of the first guide rods is two, the first guide rods are provided with a chuck, the two chucks are used to clamp the hexagonal rotating head, the chuck is pushed by the bolt rod, and the bolt rod is threadedly connected to the first carrier.

[0009] A sealing piece is threadedly connected to the first air injection hole, and a second air injection hole is provided on the shell body, which passes through the first air injection hole; a disc is provided on the second air injection hole, which closes the second air injection hole, and a third spring is provided on the disc, and a cylindrical valve body is provided at the free end of the third spring, which is used to close the first air injection hole. The cylindrical valve body is slidably adapted to the second air injection hole, and an air injection chamber is formed between the cylindrical valve body and the disc, and a third air injection hole connected to the air injection chamber is provided on the shell body.

[0010] The bottom surface of the shell is provided with two pipe openings, which are located between the T-shaped holes. Heat exchange tubes are arranged on the pipe openings. The heat exchange tubes are serpentine in shape and are located in the heat exchange gap.

[0011] The end face of the shell is provided with a plug hole connecting the vertical section, and the plug hole is threadedly connected to a wire plug, and the wire plug is provided with a second spring, and the free end of the second spring is provided with a first push plate, and the second spring causes the first push plate to close the plug hole in the initial state, and the first push plate is located in the vertical section; the bottom surface of the cover body is provided with a support, and an iron plate is provided on the support, the number of iron plates is 2, and the two iron plates are symmetrically arranged, the projection area of ​​the iron plates is larger than the projection area of ​​the serpentine first channel, and the gap between the two iron plates is adsorbed with a first magnet, the N pole of the first magnet is on the left and the S pole is on the right; a fixed seat is provided on the iron plate, the position of the fixed seat corresponds to the position of the first magnet, the fixed seat is a tubular structure, and a rotating seat is rotatably connected to the fixed seat, and the rotating seat is a tubular structure. The top surface of the rotating seat is provided with a magnet seat, and the magnet seat is adsorbed with a second magnet and a third magnet, and the N poles of the second magnet and the third magnet are on the right and the S poles are on the left. A rotating handle is provided on the magnet seat, and the rotating handle is rotatably connected to the cover body.

[0012] The clamping member includes a second carrier connected to the cover body, the number of the second carriers is 2, the two second carriers are symmetrically arranged, the second carrier is slidably connected to a second guide rod, the second guide rod is slidably connected to a clamping plate, the number of the clamping plates is 2, the opposite surfaces of the two clamping plates have arc grooves, the arc grooves are adapted to the hexagonal rotating head; the second carrier is rotatably connected to the first bidirectional screw, and the first bidirectional screw is threadedly connected to the clamping plate.

[0013] The end surface of the shell is provided with a serpentine heat exchange channel; the end surface of the shell is provided with a second sealing groove, the second sealing groove surrounds the serpentine heat exchange channel, and a second sealing ring is provided in the second sealing groove.

[0014] Furthermore, a fully automated sulfentrazone production process using a microchannel reactor comprises the following steps:

[0015] ① Condensation: Phenylhydrazine and tert-butyl alcohol are mixed uniformly in a microreactor, acetaldehyde is added dropwise, and after testing, sodium cyanate is added, acetic acid is added dropwise, and sodium hypochlorite is added dropwise after insulation. After reaction in a coil reactor and a continuous flow YX microreactor, desolventization, crystallization, and filtration are performed to obtain intermediate 1;

[0016] ② Fluoromethylation: DMF, intermediate 1, and potassium carbonate were added to the reactor, the temperature was raised to reflux for dehydration, and then freon was introduced to react. If the product was qualified, it was filtered to obtain intermediate 2;

[0017] ③ Chlorination: Add intermediate 2 into the reactor, introduce chlorine gas to react, degas and desolventize after the monochlorination reaction is qualified to obtain intermediate 3; then carry out dichlorination reaction, add acetic acid into the reactor, stir and introduce chlorine gas again, cool and crystallize after the reaction test is qualified, filter and dry to obtain intermediate 4;

[0018] ④ Nitration: Add concentrated sulfuric acid and intermediate 4 into the microchannel reactor, stir evenly, and then add fuming nitric acid dropwise. After the reaction is completed, add water dropwise and extract with toluene to obtain intermediate 5;

[0019] ⑤ Reduction: intermediate 5 and catalyst are placed in an autoclave, and hydrogen is introduced after nitrogen replacement to react. After passing the test, the temperature is lowered and the pressure is released, and the catalyst is filtered through ethanol, and then desolventizing and crystallizing to obtain intermediate 6;

[0020] ⑥ Acylation: intermediate 6 is added into the kettle, and methylsulfonyl chloride is added dropwise to carry out the reaction at a temperature of 100 °C. After the reaction is qualified, the solvent is removed, and the sulfentrazone product is obtained after cooling, crystallization, filtration, and drying.

[0021] The beneficial effect of the present invention is that: by setting up a second channel, the present application can divert the fluid in the first channel, slow down the flow rate of the fluid, ensure the full reaction of the fluid, and the diverted fluid flows back into the first channel in the curved section, which once again slows down the flow rate of the fluid, further improves the reaction time of the fluid, and has a good reaction effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 This is a side view structural diagram of this application.

[0023] Figure 2 Schematic diagram of the side structure of the first channel.

[0024] Figure 3 Schematic diagram of the side structure of the second channel.

[0025] Figure 4 It is a schematic diagram of the three-dimensional structure of the first groove and the second groove.

[0026] Figure 5 It is a schematic diagram of the main cross-sectional structure of the plug connector.

[0027] Figure 6 It is a schematic side view of the structure of the first sealing groove.

[0028] Figure 7 It is a schematic diagram of the main cross-sectional structure of the shell and substrate.

[0029] Figure 8 It is a schematic diagram of the main cross-sectional structure of the shell.

[0030] Figure 9 It is a schematic diagram of the side cross-sectional structure of the positioning mechanism.

[0031] Figure 10 It is a schematic diagram of the main cross-sectional structure of the through hole.

[0032] Figure 11 This is a schematic diagram of the main cross-sectional structure of the plug connector and the funnel groove.

[0033] Figure 12 This is a schematic diagram of the main cross-sectional structure of the U-shaped channel.

[0034] Figure 13 It is a schematic diagram of the main cross-sectional structure of the U-shaped channel and the plug connector.

[0035] Figure 14 It is a schematic diagram of the top view of the positioning mechanism.

[0036] Figure 15 It is a schematic diagram of the top structure of the pressing part.

[0037] Figure 16 It is a schematic diagram of the three-dimensional structure of the pressing part.

[0038] Figure 17 It is a schematic diagram of the three-dimensional structure of the clamping part.

[0039] Figure 18 Schematic diagram of the top structure of the first spring.

[0040] Figure 19 Schematic diagram of the top view of the bolt rod.

[0041] Figure 20 Schematic diagram of the top cross-sectional structure of the bellows.

[0042] Figure 21 Schematic diagram of the top cross-sectional structure of the second air injection hole.

[0043] Figure 22 This is a schematic diagram of the side cross-sectional structure of the third air injection hole.

[0044] Figure 23 This is a schematic diagram of the main cross-sectional structure of the diversion component.

[0045] Figure 24 It is a schematic diagram of the main cross-sectional structure of the diversion component.

[0046] Figure 25 It is a schematic diagram of the side cross-sectional structure of the heat exchange tube.

[0047] Figure 26 It is a schematic diagram of the top cross-sectional structure of the plug hole.

[0048] Figure 27 It is a schematic diagram of the side structure of the iron plate.

[0049] Figure 28 Schematic diagram of the main structure of the first magnet.

[0050] Figure 29 It is a schematic diagram of the three-dimensional structure of the fixed seat and the rotating seat.

[0051] Figure 30Schematic diagram of the top structure of the first bidirectional screw.

[0052] Figure 31 It is a schematic diagram of the three-dimensional structure of the second bidirectional screw and the third bidirectional screw.

[0053] Figure 32 It is a schematic diagram of the cross-sectional structure of the butt joint pipe from a top view.

[0054] Figure 33 It is a side view structural diagram of the heat exchange channel.

[0055] Figure 34 This is a simplified process flow diagram for the synthesis of sulfentrazone.

[0056] In the figure: 1, base plate; 2, first channel; 3, vertical section; 4, arc section; 5, first groove; 6, plug connector; 7, second groove; 8, transverse hole; 9, vertical hole; 10, second channel; 11, oblique line section; 12, curved section; 13, flow guide; 14, third groove; 15, first sealing groove; 16, first sealing ring; 17, housing; 18, receiving groove; 19, cover; 20, positioning mechanism; 21, heat exchange gap; 22, T-shaped hole; 23, T-shaped tube; 2 4. Positioning nut; 25. Funnel groove; 26. Through hole; 27. U-shaped channel; 28. Sealed bearing; 29. ​​Rotating rod; 30. Pressing member; 31. Semicircular cam; 32. Square stopper; 33. Hexagonal swivel head; 34. Clamping member; 35. First spring; 36. First carrier; 37. First guide rod; 38. Collet; 39. Bolt rod; 40. Plug hole; 41. Expanding hole; 42. Threaded plug; 43. Second spring; 44. First push plate; 45. Bellows; 46 , first air injection hole; 47, blocking piece; 48, second air injection hole; 49, disc; 50, third spring; 51, cylindrical valve body; 52, air injection chamber; 53, third air injection hole; 54, flow guide assembly; 55, first shaft seat; 56, first flow guide plate; 57, second shaft seat; 58, second flow guide plate; 59, rotating shaft; 60, pipe mouth; 61, heat exchange tube; 62, support; 63, iron plate; 64, first magnet; 65, fixed seat; 66, rotating seat; 67, magnet seat; 68. Second magnet; 69. Third magnet; 70. Rotating handle; 71. Second carrier; 72. Second guide rod; 73. Clamp; 74. Arc groove; 75. First bidirectional lead screw; 76. Bottom frame; 77. Top frame; 78. First bearing seat; 79. Second bidirectional lead screw; 80. First clamping seat; 81. Docking hole; 82. Docking tube; 83. Second bearing seat; 84. Third bidirectional lead screw; 85. Second clamping seat; 86. Heat exchange channel; 87. Second sealing groove. DETAILED DESCRIPTION

[0057] The embodiments of the present invention are described in detail below. Examples of the embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals throughout represent the same or similar elements or elements with the same or similar functions. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain the present invention, and should not be understood as limiting the present invention.

[0058] In the description of the present invention, it should be understood that the terms "center", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "circumferential", etc., indicating the orientation or position relationship, are based on the orientation or position relationship shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present invention.

[0059] In addition, the terms "first", "second" and "third" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the quantity of the indicated technical features.

[0060] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "install", "connect" and "connect" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0061] like Figures 1 to 5As shown, in the first embodiment, a microchannel reactor comprises a substrate 1, the shape of the substrate 1 is rectangular, and a first channel 2 is provided on one end surface of the substrate 1. The first channel 2 is composed of a plurality of vertical segments 3 and a plurality of arc segments 4. The vertical segments 3 and the arc segments 4 are arranged at intervals to form a snake-shaped first channel 2; an outermost vertical segment 3 serves as a liquid inlet end, and a first groove 5 is provided on the liquid inlet end, and a plug connector 6 is connected to the first groove 5; the other outermost vertical segment 3 serves as a liquid outlet end, and a second groove 7 is provided on the liquid outlet end, and the plug connector 6 is connected to the second groove 7; the plug connector 6 protrudes from the outside of the substrate 1, and the protruding end of the plug connector 6 has a tapered surface, a transverse hole 8 is provided at the center of the plug connector 6, and a vertical hole 9 connected to the transverse hole 8 is provided on the side wall of the plug connector 6, and the vertical hole 9 is communicated with the first channel 2; an opening is provided on the substrate 1 A second channel 10 is provided that is connected to the vertical section 3. Second channels 10 are provided on both sides of the vertical section 3. Several second channels 10 are arranged at equal intervals from top to bottom, and the second channels 10 on both sides are staggered. The second channel 10 is composed of a slanted section 11 and a curved section 12. The slanted section 11 serves as the upstream side through which the fluid flows, and the curved section 12 serves as the downstream side through which the fluid flows. A water drop-shaped guide portion 13 is formed between the second channel 10 and the first channel 2, and the guide portion 13 separates the first channel 2 from the second channel 10. By setting the second channel 10, the present application can divert the fluid in the first channel 2, slow down the flow rate of the fluid, ensure sufficient reaction of the fluid, and the diverted fluid flows back into the first channel 2 at the curved section 12, which once again slows down the flow rate of the fluid, further improves the reaction time of the fluid, and has a good reaction effect.

[0062] like Figure 3 As shown, as an optimization of the first embodiment, the vertical section 3 of the first channel 2 is provided with third grooves 14 arranged at equal intervals. The third grooves 14 slow down the flow rate of the fluid and improve the reaction time of the fluid.

[0063] like Figure 6 As shown, as an optimization of embodiment 1, taking into account the sealing performance of the substrate 1, a first sealing groove 15 is opened on the end face of the substrate 1, and the first sealing groove 15 surrounds the snake-shaped first channel 2. The first sealing groove 15 has at least three layers, and a first sealing ring 16 is installed in the first sealing groove 15. By providing the first sealing ring 16, the leakage problem is avoided.

[0064] like Figures 7 to 13As shown, as an optimization of the first embodiment, considering that the fluid reaction will release heat, the existing microchannel reactor connects the substrate 1 with the microchannel and the heat exchange plate together by a number of bolts, which makes disassembly and assembly complicated. It also includes a shell 17 for placing the substrate 1. The shell 17 is a rectangular structure. The top surface of the shell 17 has a receiving groove 18. A cover 19 that closes the receiving groove 18 is fixed to the shell 17 by bolts; the receiving groove 18 is used to install the substrate 1, and the number of substrates 1 is 2. The serpentine first channels 2 of the two substrates 1 are offset from the receiving groove 18. The two substrates 1 are squeezed and fixed by a positioning mechanism 20, and the positioning mechanism 20 is provided on the cover 19; a heat exchange gap 21 is formed between the two substrates 1, and the bottom surface of the shell 17 is provided with two T-shaped holes 22. A T-shaped tube 23 is installed on the T-shaped hole 22, and the T-shaped tube 23 is fixed by a positioning nut 24. One T-shaped tube 23 is used as The cooling medium inlet and the other T-shaped tube 23 serve as the cooling medium outlet; the reaction heat is taken away from the inside, which avoids the influence of the ambient temperature on the heat exchange effect and has a good heat exchange effect; a funnel groove 25 adapted to the plug connector 6 is provided on the accommodating groove 18, and a through hole 26 connected to the upper funnel groove 25 is provided on the shell 17. The through hole 26 on the left side serves as a liquid inlet port and the through hole 26 on the right side serves as a liquid outlet port; a U-shaped channel 27 connected to the lower funnel groove 25 is provided on the shell 17. The fluid first enters the first channel 2 of the left substrate 1 from the through hole 26 on the left, and then enters the first channel 2 of the right substrate 1 through the U-shaped channel 27, and finally is discharged through the through hole 26 on the right, thus forming a flow path for the fluid reaction; the substrate 1 is fixed by setting a positioning mechanism 20, which is simple to assemble and disassemble, and a heat exchange gap 21 is formed between the substrates 1, which greatly improves the heat exchange effect.

[0065] like Figures 14 to 17As shown, as an optimization of the first embodiment, there are two positioning mechanisms 20, and the two positioning mechanisms 20 are symmetrically arranged. The positioning mechanism 20 includes a sealed bearing 28, which is rotatably connected to the cover body 19. A rotating rod 29 is rotatably connected to the sealed bearing 28, and the lower end of the rotating rod 29 is rotatably connected to the shell 17. The rotating rod 29 is located in the middle of the accommodating groove 18. The side wall of the rotating rod 29 is connected with a pressing member 30 arranged at equal intervals. The number of the pressing members 30 is at least 3, and the pressing member 30 is composed of two semicircular cams 31 connected together. The maximum outer diameter of the semicircular cam 31 is interference fit with the two substrates 1, and the straight section of the semicircular cam 31 has Square limit block 32, after the square limit block 32 abuts against the substrate 1, the rotating rod 29 stops rotating, and the two substrates 1 are squeezed and fixed at the same time; the upper end of the rotating rod 29 extends out of the cover body 19, and the upper end of the rotating rod 29 is connected with a hexagonal rotating head 33, and the hexagonal rotating head 33 is positioned by a clamping member 34, and the clamping member 34 is provided on the cover body 19; by rotating the hexagonal rotating head 33, the position of the clamping member 30 can be adjusted. When the minimum outer diameter of the clamping member 30 is opposite to the substrate 1, the substrate 1 can be quickly removed. When the maximum outer diameter of the clamping member 30 abuts against the substrate 1, the two substrates 1 are fixed at the same time, so that the reaction process of the microchannel can be carried out.

[0066] like Figure 18 As shown, as an optimization of the first embodiment, the opposite surfaces of the two substrates 1 are connected with first springs 35. The number of the first springs 35 is at least 6, and each group of 3 is arranged from top to bottom. By providing the first springs 35, the two substrates 1 are close to each other in the initial state, which facilitates the removal of the substrates 1.

[0067] like Figure 19 As shown, as an optimization of Example 1, the clamping member 34 includes a first carrier 36 connected to the cover body 19, the number of the first carriers 36 is 2, and the two first carriers 36 are symmetrically arranged. A first guide rod 37 is slidably connected to the first carrier 36, the number of the first guide rods 37 is 2, and a clamp 38 is connected to the first guide rod 37. The shape of the clamp 38 is U-shaped, and the two clamps 38 are used to clamp the hexagonal rotating head 33. The clamp 38 is pushed by a bolt rod 39, and the bolt rod 39 is threadedly connected to the first carrier 36. By rotating the bolt rod 39, the two clamps 38 are moved toward each other until the clamp 38 and the hexagonal rotating head 33 are completely pressed, thereby realizing the positioning of the clamping member 30, and then the two substrates 1 can carry out the microchannel reaction process.

[0068] like Figure 20As shown, as an optimization of the first embodiment, considering that the microchannel is a tiny structure, the vertical section 3 of the first channel 2 may be blocked and needs to be disassembled and cleaned after being blocked, the end face of the shell 17 is provided with a plug hole 40 connected to the vertical section 3, and one vertical section 3 corresponds to at least two plug holes 40, and the plug hole 40 is provided with a flared hole 41 opposite to the vertical section 3, a plug 42 is threadedly connected to the plug hole 40, and a second spring 43 is connected to the plug 42, and the free end of the second spring 43 is connected to a first push plate 44, the first push plate 44 is against the accommodating groove 18, and the second spring 4 3 so that the first push plate 44 closes the expanded hole 41 in the initial state. The first push plate 44 is located in the vertical section 3 and does not affect the flow of the fluid. A bellows 45 is connected between the first push plate 44 and the plug hole 40. The bellows 45 can prevent the fluid from entering the plug hole 40. A first air injection hole 46 is opened in the center of the wire plug 42. By injecting air into the first air injection hole 46, the bellows 45 expands, and the first push plate 44 is pushed away from the accommodating groove 18. The moving first push plate 44 can squeeze the obstruction at the vertical section 3 and expand the first channel 2, so that the obstruction can be cleared without disassembling the base plate 1.

[0069] like Figure 21 and Figure 22 As shown, as an optimization of the first embodiment, considering that multiple existing microchannel reactors are used in a stacked manner, the position of the first gas injection hole 46 affects the stacking of multiple shells 17, and a sealing piece 47 is threadedly connected to the first gas injection hole 46. A second gas injection hole 48 is provided on the shell 17, which passes through the first gas injection hole 46. The diameter of the second gas injection hole 48 is larger than the diameter of the first gas injection hole 46; a disc 49 is connected to the second gas injection hole 48, and the disc 49 closes the second gas injection hole 48. A third spring 50 is connected to the disc 49, and the free end of the third spring 50 is connected to a cylindrical valve body 51, which is used to close the first gas injection hole 46. The cylindrical valve body 51 is slidably adapted to the second gas injection hole 48. An injection chamber 52 is formed between the cylindrical valve body 51 and the disc 49. A third injection hole 53 connected to the injection chamber 52 is opened on the shell 17. The third injection hole 53 injects gas into the injection chamber 52, and a row of cylindrical valve bodies 51 are pushed and exceed the first injection hole 46. The gas enters the first injection hole 46, causing the bellows 45 to expand, and the first push plate 44 is pushed away from the accommodating groove 18. The moving first push plate 44 can squeeze the obstruction at the vertical section 3 and expand the first channel 2, so that the blockage can be cleared without disassembling the substrate 1. In addition, the cylindrical valve body 51 can prevent the fluid from flowing out through the third injection hole 53. In this way, the third injection hole 53 is located on the side of the shell 17 and will not affect the stacking of multiple shells 17.

[0070] like Figure 23 and Figure 24As shown, embodiment 2 is different from embodiment 1 in that, considering that the cooling medium is air, there is no guide structure in the heat exchange gap 21, the air will be discharged quickly, and the cooling effect is poor. A number of guide components 54 are installed on the opposite surfaces of the two substrates 1, and the guide components 54 are arranged at equal intervals from top to bottom; a first shaft seat 55 is connected to one substrate 1, and the number of the first shaft seats 55 is 2. A first guide plate 56 is rotatably connected to the first shaft seat 55, and the first guide plate 56 is arranged obliquely upward; a second shaft seat 57 is connected to the other substrate 1, and the number of the second shaft seats 57 is 2. A second guide plate 58 is rotatably connected to the second shaft seat 57, and the second guide plate 58 is arranged obliquely upward, and the second guide plate 58 is rotatably connected to the first guide plate 56 through a rotating shaft 59; by setting the guide component 54, the cooling air can be stratified, the flow rate of the cooling air can be slowed down, and the cooling effect can be improved; and the first guide plate 56 and the second guide plate 58 can be folded to facilitate the disassembly and assembly of the substrate 1.

[0071] like Figure 25 As shown, embodiment 3 is different from embodiment 1 in that, considering that the cooling medium is air and the heat exchange effect is single, a pipe opening 60 is opened on the bottom surface of the shell 17, and the number of the pipe openings 60 is 2. The two pipe openings 60 are located between the T-shaped holes 22. A heat exchange tube 61 is installed on the pipe opening 60. The shape of the heat exchange tube 61 is a snake shape. The heat exchange tube 61 is located in the heat exchange gap 21. Coolant is injected into the heat exchange tube 61. By setting the coolant heat exchange and coordinating the air heat exchange, the heat exchange effect is further improved.

[0072] like Figures 26 to 29As shown, embodiment 4 is different from embodiment 1 in that, considering that the microchannel is a tiny structure, the vertical section 3 of the first channel 2 may be blocked and needs to be disassembled and cleaned after being blocked. The end face of the shell 17 is provided with a plug hole 40 connected to the vertical section 3. At least two plug holes 40 are corresponding to one vertical section 3. A plug 42 is threadedly connected to the plug hole 40. A second spring 43 is connected to the plug 42. The free end of the second spring 43 is connected to a first push plate 44. The first push plate 44 is against the accommodating groove 18, and the second spring 43 makes the first push plate 44 close the plug hole 40 in the initial state. The first push plate 44 is located at The vertical section 3 is provided, and does not affect the flow of the fluid; the bottom surface of the cover body 19 is connected to a support 62, the number of the supports 62 is 2, and the two supports 62 are located in the heat exchange gap 21, and the support 62 is connected to an iron plate 63, the number of the iron plates 63 is 2, and the two iron plates 63 are symmetrically arranged, and the projection area of ​​the iron plates 63 is larger than the projection area of ​​the snake-shaped first channel 2, and the gap between the two iron plates 63 is adsorbed with a first magnet 64, the number of the first magnets 64 is at least 3, and the three first magnets 64 are arranged in sequence from front to back, with the N pole of the first magnet 64 on the left and the S pole on the right; the iron plate 63 is connected to a fixing seat 65, and the fixing seat The number of 65 is at least 3, the position of the fixed seat 65 corresponds to the position of the first magnet 64, the fixed seat 65 is a tubular structure, the fixed seat 65 is rotatably connected to the rotating seat 66, the rotating seat 66 is a tubular structure, the top surface of the rotating seat 66 is connected to the magnet seat 67, the magnet seat 67 is surrounded by 3 iron sheets to form an inverted U-shaped structure, the second magnet 68 and the third magnet 69 are adsorbed on the magnet seat 67, the N pole of the second magnet 68 and the third magnet 69 are on the right and the S pole is on the left, the magnet seat 67 is connected to the rotating handle 70, the rotating handle 70 is rotatably connected to the cover body 19, in the initial state, the N pole of the first magnet 64 is on the left and the S pole is on the left. The north pole of the second magnet 68 and the third magnet 69 is on the right, and the south pole is on the left. At this time, the upper and lower magnetic poles are opposite, forming a closed circuit. The iron plate 63 shows no magnetism to the outside. When the blockage needs to be cleared, the rotating handle 70 rotates 180°. At this time, the north pole of the second magnet 68 and the third magnet 69 is on the left, and the south pole is on the right. The upper and lower magnetic poles are the same, and the magnetic field will be conducted downward along the iron plate 63. The iron plate 63 shows magnetism to the outside, and the first push plate 44 is adsorbed into the vertical section 3. The moving first push plate 44 can squeeze the obstruction at the vertical section 3, expand the first channel 2, and realize that the blockage can be cleared without disassembling the substrate 1.

[0073] like Figure 30As shown, embodiment five is different from embodiment one in that, considering that the above-mentioned clamping member 34 cannot move the positioning pressing member 30 at the same time, the clamping member 34 includes a second carrier 71 connected to the cover body 19, the number of the second carriers 71 is 2, and the two second carriers 71 are symmetrically arranged. The second carrier 71 is slidably connected with a second guide rod 72, and the second guide rod 72 is slidably connected with a clamping plate 73, the number of the clamping plates 73 is 2, and the opposite surfaces of the two clamping plates 73 have arc grooves 74, which are adapted to the inner hexagonal rotating head 33; the second carrier 71 is rotatably connected to the first bidirectional screw 75, and the first bidirectional screw 75 is threadedly connected to the clamping plate 73, and the two clamping plates 73 are moved toward each other at the same time by rotating the first bidirectional screw 75 until the clamping plate 73 is completely pressed against the inner hexagonal rotating head 33, thereby realizing the positioning of the pressing member 30, and then the two substrates 1 can carry out the microchannel reaction process.

[0074] like Figure 31 and Figure 32 As shown, embodiment 6 is different from embodiment 1 in that, considering that a single shell 17 can only mount two substrates 1 with microchannels, it also includes a bottom frame 76 and a top frame 77. The bottom frame 76 is connected to a first bearing seat 78. The number of the first bearing seats 78 is 2. The first bearing seat 78 is rotatably connected to a second bidirectional screw 79. The second bidirectional screw 79 is threadedly connected to a first clamping seat 80. Several shells 17 are arranged between the two first clamping seats 80. The through holes 26 of adjacent shells 17 are opposite. A docking hole 81 is opened on the through hole 26. The diameter of the docking hole 81 is greater than The diameter of the through hole 26 is 0.1mm, and a docking tube 82 is inserted into the docking hole 81. By setting the docking tube 82, the end faces of the two shells 17 are completely fitted together to avoid leakage problems; a second bearing seat 83 is connected to the top frame 77, and the number of the second bearing seats 83 is 2. A third bidirectional screw 84 is rotatably connected to the second bearing seat 83, and a second clamping seat 85 is threadedly connected to the third bidirectional screw 84. The two second clamping seats 85 are used to clamp the shell 17. By setting the first clamping seat 80 and the second clamping seat 85, multiple shells 17 can be connected, which extends the reaction path and has a better reaction effect.

[0075] like Figure 33 As shown, as an optimization of Example 6, a serpentine-shaped heat exchange channel 86 is provided on the end face of the shell 17, and the heat exchange channel 86 is used to inject coolant to take away the reaction heat from the outside of the shell 17; a second sealing groove 87 is provided on the end face of the shell 17, and the second sealing groove 87 surrounds the serpentine-shaped heat exchange channel 86. A second sealing ring is installed in the second sealing groove 87. By providing the second sealing ring, the problem of coolant leakage is avoided.

[0076] At present, there are two main production processes for sulfentrazone (one-step reaction method and two-step reaction method):

[0077] The two-step reaction method: First, 2-(5-amino-2,4-dichlorophenyl)-3-methyl-4-difluoromethyl-2,4-dihydro-5-methyl-3-hydro-1,2,4-triazolin-3-one (hereinafter referred to as Compound I) reacts with methylsulfonyl chloride in the presence of triethylamine in dichloromethane to produce a bis(methylsulfonylamine) derivative (Compound II). Compound II is then hydrolyzed with aqueous sodium hydroxide in ethanol to yield sulfentrazone in a 66% yield. The reaction consumes 2.25 mol of methylsulfonyl chloride and 2.25 mol of triethylamine per molecule of Compound I. The one-step reaction method: Compound I reacts with methylsulfonyl chloride in the presence of a catalyst to synthesize sulfentrazone in a single step. These processes suffer from the following issues: Mass and heat transfer limitations: The mass and heat transfer efficiency in the reactor used in current production processes is extremely low, limiting the reaction rate and product selectivity.

[0078] like Figure 34 As shown, further, a fully automated sulfentrazone production process using a microchannel reactor is proposed, comprising the following steps:

[0079] ① Condensation: Phenylhydrazine and tert-butyl alcohol were mixed uniformly in a microreactor, acetaldehyde was added dropwise, and after testing, sodium cyanate was added, acetic acid was added dropwise, and sodium hypochlorite was added dropwise after insulation. After reaction in a coil reactor and a continuous flow YX microreactor, desolvation, crystallization, and filtration were performed to obtain intermediate 1 (MTZ);

[0080] ② Fluoromethylation: DMF, intermediate 1 (MTZ), and potassium carbonate were added to the reactor, the temperature was raised to reflux for dehydration, and then freon was introduced to react. After the test was qualified, the intermediate 2 (F-MTZ) was obtained by filtration;

[0081] ③ Chlorination: Add intermediate 2 (F-MTZ) into the reactor, introduce chlorine gas to react, and degas and desolventize after the monochlorination reaction is qualified to obtain intermediate 3 (CMTZ); then carry out dichlorination reaction, add acetic acid to the reactor, stir, and introduce chlorine gas again. After the reaction test is qualified, cool and crystallize, filter and dry to obtain intermediate 4 (DCMTZ);

[0082] ④ Nitration: Concentrated sulfuric acid and intermediate 4 (DCMTZ) are added to a microchannel reactor, stirred evenly, and then fuming nitric acid is added dropwise. After the reaction is completed, water is added dropwise and extracted with toluene to obtain intermediate 5 (nitrate toluene solution). Microchannel reactors are very suitable for nitration reactions, with a reaction time generally ranging from 0.3 to 2 minutes. The reaction temperature can be higher than that of traditional reactors. The higher the concentration of sulfuric acid, the faster the nitration rate. Microchannel reactors enhance heat and mass transfer processes, weaken the steric hindrance effect in the reaction, reduce the relationship between selectivity and various factors, and improve selectivity. The reaction is safer, and the enhanced transfer process makes the reaction process in the reactor easier to control.

[0083] ⑤ Reduction: intermediate 5 (nitrate toluene solution) and catalyst are placed in an autoclave, and hydrogen is introduced after nitrogen replacement to react. After passing the test, the temperature is lowered and the pressure is released, and the catalyst is filtered with ethanol, followed by desolvation and crystallization to obtain intermediate 6 (amide toluene solution);

[0084] ⑥ Acylation: intermediate 6 (amide toluene solution) was added into the kettle, and methylsulfonyl chloride was added dropwise to carry out the reaction at a temperature of 1 000 ℃. After the reaction was qualified, the solvent was removed, and the sulfentrazone product was obtained after cooling, crystallization, filtration, and drying.

[0085] Although the present invention has been described in detail with reference to the foregoing examples, it is still possible for those skilled in the art to make modifications to the technical solutions described in the foregoing embodiments, or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A microchannel reactor comprising a substrate, characterized in that: The first channel is formed on one end surface of the substrate, and the first channel is composed of several vertical sections and several arc sections, and the vertical sections and the arc sections are arranged at intervals to form a serpentine-shaped first channel; an outermost vertical section serves as a liquid inlet end, the liquid inlet end has a first groove, and the first groove is provided with a plug connector; the other outermost vertical section serves as a liquid outlet end, the liquid outlet end has a second groove, and the second groove is provided with the plug connector; the substrate is provided with a second channel connected to the vertical section, and second channels are provided on both sides of the vertical section, and the plurality of second channels are arranged at equal intervals from top to bottom, and the positions of the second channels on both sides are staggered, the second channel is composed of an oblique line segment and a curved line segment, the oblique line segment serves as the upstream side through which the fluid flows, and the curved section serves as the downstream side through which the fluid flows, and a water drop-shaped guide portion is formed between the second channel and the first channel, and the guide portion separates the first channel from the second channel; it also includes a shell for placing the substrate, the top surface of the shell has a receiving groove, and the shell is provided with a cover; the receiving groove is used to install the substrate, the number of substrates is 2, the first channel and the receiving groove are offset, and the two substrates are squeezed and fixed by a positioning mechanism; 2 A heat exchange gap is formed between the substrates, and two T-shaped holes are provided on the bottom surface of the shell, and the T-shaped holes are provided with T-shaped tubes; the accommodating groove is provided with a funnel groove adapted to the plug connector, and the shell is provided with a through hole connected to the upper funnel groove; the shell is provided with a U-shaped channel connected to the lower funnel groove; the bottom surface of the shell is provided with a pipe opening, the number of the pipe openings is 2, the two pipe openings are located between the T-shaped holes, and the pipe openings are provided with a heat exchange tube, the shape of the heat exchange tube is snake-shaped, and the heat exchange tube is located in the heat exchange gap; the end surface of the shell is provided with a snake-shaped heat exchange channel; the A plug hole connected to the vertical section is opened on the end surface of the shell, and the plug hole is threadedly connected to a plug, and the plug is provided with a second spring, and a first push plate is provided at the free end of the second spring, and the second spring causes the first push plate to close the plug hole in the initial state, and the first push plate is located in the vertical section; the bottom surface of the cover body is provided with a support, and the support is provided with an iron plate, the number of the iron plates is 2, and the two iron plates are symmetrically arranged, and the projected area of ​​the iron plates is larger than the projected area of ​​the serpentine first channel, and a first magnet is adsorbed in the gap between the two iron plates, with the N pole of the first magnet on the left and the S pole on the right; The iron plate is provided with a fixed seat, the position of the fixed seat corresponds to the position of the first magnet, the fixed seat is a tubular structure, the fixed seat is rotatably connected to the rotating seat, the rotating seat is a tubular structure, the top surface of the rotating seat is provided with a magnet seat, the magnet seat adsorbs the second magnet and the third magnet, the N pole of the second magnet and the third magnet is on the right and the S pole is on the left, the magnet seat is provided with a rotating handle, and the rotating handle is rotatably connected to the cover body; by rotating the rotating handle, the iron plate can be selectively magnetic or non-magnetic to the outside, and when the iron plate is magnetic to the outside, the first push plate is adsorbed into the vertical section.

2. A microchannel reactor according to claim 1, characterized in that: The plug connector protrudes out of the base plate, and the protruding end of the plug connector has a tapered surface. A transverse hole is opened at the center of the plug connector, and a vertical hole connected to the transverse hole is opened on the side wall of the plug connector. The vertical hole is connected to the first channel.

3. A microchannel reactor according to claim 1, characterized in that: The vertical section of the first channel is provided with third grooves arranged at equal intervals.

4. A microchannel reactor according to claim 1, characterized in that: A first sealing groove is formed on the end surface of the substrate. The first sealing groove surrounds the first serpentine channel. The first sealing groove has at least three layers. A first sealing ring is provided in the first sealing groove.

5. A microchannel reactor according to claim 1, characterized in that: There are two positioning mechanisms, each including a sealed bearing, which is rotatably connected to the cover body. A rotating rod is rotatably connected to the sealed bearing, and the lower end of the rotating rod is rotatably connected to the shell. The rotating rod is located in the middle of the accommodating groove, and the side walls of the rotating rod are provided with equally spaced clamping members. The clamping members are composed of two semicircular cams connected to each other. The maximum outer diameter of the semicircular cam is interference fit with the two base plates, and the straight section of the semicircular cam has a square limit block; the upper end of the rotating rod extends out of the cover body, and the upper end of the rotating rod is provided with an inner hexagonal rotating head, which is positioned by a clamping member.

6. A microchannel reactor according to claim 1, characterized in that: Several guide components are provided on the opposite surfaces of the two base plates, and the guide components are arranged at equal intervals from top to bottom; a first shaft seat is provided on one base plate, and a first guide plate is rotatably connected to the first shaft seat, and the first guide plate is arranged obliquely upward; a second shaft seat is provided on the other base plate, and a second guide plate is rotatably connected to the second shaft seat, and the second guide plate is arranged obliquely upward, and the second guide plate is rotatably connected to the first guide plate through a rotating shaft.

7. A fully automated process for producing sulfentrazone using the microchannel reactor according to any one of claims 1 to 6, characterized in that: The following steps are involved: ① Condensation: Phenylhydrazine and tert-butyl alcohol are mixed uniformly in a microreactor, acetaldehyde is added dropwise, and after testing, sodium cyanate is added, acetic acid is added dropwise, and sodium hypochlorite is added dropwise after insulation. After reaction in a coil reactor and a continuous flow YX microreactor, desolventization, crystallization, and filtration are performed to obtain intermediate 1; ② Fluoromethylation: DMF, intermediate 1, and potassium carbonate were added to the reactor, the temperature was raised to reflux for dehydration, and then freon was introduced to react. If the product was qualified, it was filtered to obtain intermediate 2; ③ Chlorination: Add intermediate 2 into the reactor, introduce chlorine gas to react, degas and desolventize after the monochlorination reaction is qualified to obtain intermediate 3; then carry out dichlorination reaction, add acetic acid into the reactor, stir and introduce chlorine gas again, cool and crystallize after the reaction test is qualified, filter and dry to obtain intermediate 4; ④ Nitration: Add concentrated sulfuric acid and intermediate 4 into the microchannel reactor, stir evenly, and then add fuming nitric acid dropwise. After the reaction is completed, add water dropwise and extract with toluene to obtain intermediate 5; ⑤ Reduction: intermediate 5 and catalyst are placed in an autoclave, and hydrogen is introduced after nitrogen replacement to react. After passing the test, the temperature is lowered and the pressure is released, and the catalyst is filtered through ethanol, and then desolventizing and crystallizing to obtain intermediate 6; ⑥ Acylation: intermediate 6 is added into the kettle, and methylsulfonyl chloride is added dropwise to carry out the reaction at a temperature of 100 °C. After the reaction is qualified, the solvent is removed, and the sulfentrazone product is obtained after cooling, crystallization, filtration, and drying.

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