Micro-channel reactor and full-automatic sulfentrazone production process

Abstract

The invention relates to the technical field of chemical reaction equipment, and discloses a micro-channel reactor and a full-automatic sulfentrazone production technology.The micro-channel reactor comprises a base plate, a first channel is formed in one end face of the base plate, a vertical section on the outermost side serves as a liquid inlet end, a first groove is formed in the liquid inlet end, and a connecting plug is arranged on the first groove; the other vertical section on the outermost side serves as a liquid outlet end, a second groove is formed in the liquid outlet end, and the connecting plug is arranged on the second groove; a second channel communicated with the vertical section is formed in the base plate, a water-drop-shaped flow guide part is formed between the second channel and the first channel, and the first channel and the second channel are separated by the flow guide part; by arranging the second channel, fluid in the first channel can be shunted, the flow speed of the fluid is slowed down, full reaction of the fluid is guaranteed, the shunted fluid flows back into the first channel at the bent section, the flow speed of the fluid is slowed down again, the reaction time of the fluid is further prolonged, and the reaction effect is good.

Description

Technical Field

[0001] The 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, usually have small channel sizes and channel diversity. They are devices that can be used for chemical reactions and are made of solid matrices using special micromachining technology. Compared with conventional reactors, microchannel reactors have the characteristics of small size, large specific surface area, continuous process, and easy scale-up. The unique structure of microreactors gives them very high heat and mass transfer efficiency, which can keep the reaction layer close to constant temperature, which is conducive to the conduct of various chemical reactions and has been applied in many 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, and the microchannel reactor is characterized in that the channels include: one or more introduction channels, different fluids are introduced into the introduction channels respectively; a mixing channel, each fluid introduced into the introduction channel is merged and passes through the mixing channel; and a discharge channel, the fluids merged through the mixing channel are discharged through the discharge channel; 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 merged fluids, the fluids undergo a mixing process of branching in the upward / downward direction and then merging with each other in the 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 to solve the problem that the flow rate of the existing microchannel reactor mentioned in the above background technology is still relatively fast and the reaction is insufficient.

[0006] The technical solution adopted by the present invention is as follows: a microchannel reactor comprises a substrate, the substrate is rectangular in shape, a first channel is provided on one end surface of the substrate, the first channel is composed of a plurality of vertical segments and a plurality of circular arc segments, the vertical segments and the circular arc segments are arranged at intervals to form a snake-shaped first channel; an outermost vertical segment is used as a liquid inlet end, the liquid inlet end is provided with a first groove, and the first groove is provided with a plug connector; another outermost vertical segment is used as a liquid outlet end, the liquid outlet end is provided with a second groove, and the second groove is provided with the plug connector; a second channel connected to the vertical segment is provided on the substrate, second channels are provided on both sides of the vertical segment, a 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 line segment serves as the downstream side through which the fluid flows, 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.

[0007] First springs are arranged 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 2, the two first carriers are symmetrically arranged, the first carrier is slidably connected with a first guide rod, the number of the first guide rods is 2, the first guide rod is provided with a chuck, the two chucks are used to clamp the hexagonal rotating head, the chuck is pushed by a bolt rod, and the bolt rod is threadedly connected to the first carrier.

[0009] A sealing plate is threadedly connected to the first air injection hole, and a second air injection hole that penetrates the first air injection hole is opened on the shell; 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 fitted with 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 opened on the shell.

[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, which are in a snake shape and are located in the heat exchange gap.

[0011] The end surface of the shell is provided with a plug hole connected to the vertical section, and a wire plug is threadedly connected to the plug hole, and a second spring is provided on the wire plug, and a first push plate is provided at the free end of the second spring, and the second spring makes the first push plate 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, and the number of the iron plates is 2, and the two iron plates are symmetrically arranged, and the projection area of ​​the iron plates is larger than the projection area of ​​the serpentine first channel, and the first magnet is adsorbed in the gap between the two iron plates, and 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, and the position of the fixed seat corresponds to the position of the first magnet, and 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, and a magnet seat is provided on the top surface of the rotating seat, and a second magnet and a third magnet are adsorbed on the magnet seat, and the N poles of the second magnet and the third magnet are on the right and the S poles are on the left, and 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, a second guide rod is slidably connected to the second carrier, a clamping plate is slidably connected to the second guide rod, 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 first bidirectional screw is rotatably connected to the second carrier, 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 arranged in the second sealing groove.

[0014] Furthermore, a fully automated sulfentrazone production process using a microchannel reactor comprises the following steps: ① Condensation: Phenylhydrazine and tert-butyl alcohol are mixed evenly in a microreactor, acetaldehyde is added dropwise, and after testing, sodium cyanate is added dropwise, acetic acid is added dropwise, sodium hypochlorite is added dropwise after heat preservation, and 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 are added to the reaction kettle, and after heating and refluxing for dehydration, freon is introduced for reaction. If the product is qualified, it is 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 and stir, 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 drop fuming nitric acid. After the reaction is completed, drop water and extract with toluene to obtain intermediate 5; ⑤ Reduction: intermediate 5 and catalyst are placed in the autoclave, and hydrogen is introduced to react after nitrogen replacement. After the test is qualified, the temperature is reduced and the pressure is released, and the catalyst is filtered by ethanol, and then desolventization and crystallization are performed to obtain intermediate 6; ⑥ Acylation: put the intermediate 6 into the kettle, add methylsulfonyl chloride dropwise and keep warm for reaction, remove the solvent after the reaction is qualified, and obtain the sulfentrazone finished product after cooling, crystallization, filtration and drying.

[0015] 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

[0016] Figure 1 This is a side view structural diagram of the present application.

[0017] Figure 2 It is a schematic diagram of the side structure of the first channel.

[0018] Figure 3 It is a schematic diagram of the side structure of the second channel.

[0019] Figure 4 It is a schematic diagram of the three-dimensional structure of the first groove and the second groove.

[0020] Figure 5 It is a schematic diagram of the main cross-sectional structure of the plug connector.

[0021] Figure 6 It is a schematic diagram of the side structure of the first sealing groove.

[0022] Figure 7 It is a schematic diagram of the main cross-sectional structure of the shell and substrate.

[0023] Figure 8 It is a schematic diagram of the main cross-sectional structure of the shell.

[0024] Fig. 9 It is a schematic diagram of the side cross-sectional structure of the positioning mechanism.

[0025] Fig.10 It is a schematic diagram of the main cross-sectional structure of the through hole.

[0026] Fig.11 It is a schematic diagram of the main cross-sectional structure of the plug connector and the funnel groove.

[0027] Fig.12 It is a schematic diagram of the main cross-sectional structure of the U-shaped channel.

[0028] Fig.13It is a schematic diagram of the main cross-sectional structure of the U-shaped channel and the plug connector.

[0029] Fig.14 It is a schematic diagram of the top view of the positioning mechanism.

[0030] Fig.15 It is a schematic diagram of the structure of the clamping member from a top view.

[0031] Fig.16 It is a schematic diagram of the three-dimensional structure of the pressing piece.

[0032] Fig.17 It is a schematic diagram of the three-dimensional structure of the clamping part.

[0033] Fig.18 It is a schematic diagram of the top view of the structure of the first spring.

[0034] Fig.19 Schematic diagram of the top view of the bolt rod.

[0035] Fig. 20 It is a schematic diagram of the top-down cross-sectional structure of the bellows.

[0036] Fig.21 Schematic diagram of the top cross-sectional structure of the second air injection hole.

[0037] Fig. 22 It is a schematic diagram of the side cross-sectional structure of the third air injection hole.

[0038] Fig.23 It is a schematic diagram of the main cross-sectional structure of the guide component.

[0039] Fig.24 It is a schematic diagram of the main cross-sectional structure of the guide component.

[0040] Fig.25 It is a schematic diagram of the side cross-sectional structure of the heat exchange tube.

[0041] Fig.26 It is a schematic diagram of the top view cross-sectional structure of the plug hole.

[0042] Fig. 27 It is a schematic diagram of the side structure of the iron plate.

[0043] Fig.28 It is a schematic diagram of the main structure of the first magnet.

[0044] Fig.29 It is a schematic diagram of the three-dimensional structure of the fixed seat and the rotating seat.

[0045] Fig.30 It is a schematic diagram of the top view of the structure of the first bidirectional screw.

[0046] Fig.31 It is a schematic diagram of the three-dimensional structure of the second bidirectional lead screw and the third bidirectional lead screw.

[0047] Fig.32 It is a schematic diagram of the top view cross-sectional structure of the butt-jointed pipe.

[0048] Fig.33 It is a schematic diagram of the side structure of the heat exchange channel.

[0049] Fig.34 This is a simplified process flow diagram for the synthesis of sulfentrazone.

[0050] In the figure: 1, substrate; 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, guide part; 14, third groove; 15, first sealing groove; 16, first sealing ring; 17, shell; 18, accommodating 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 rotating head; 34. Clamping member; 35. First spring; 36. First carrier; 37. First guide rod; 38. Clamp; 39. Bolt rod; 40. Plug hole; 41. Expanding hole; 42. Screw 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

[0051] 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 construed as limiting the present invention.

[0052] In the description of the present invention, it is necessary to understand that the terms "center", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "circumferential", etc., indicating orientations or positional relationships, are based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply 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.

[0053] In addition, the terms "first", "second", and "third" are used for descriptive purposes only and cannot be understood as indicating or implying relative importance or implicitly indicating the quantity of the indicated technical features.

[0054] In the description of the present invention, it should be noted that, unless otherwise clearly stipulated and limited, the terms "installation", "connection" and "connection" 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.

[0055] like Figure 1~Figure 5As shown, in the first embodiment, a microchannel reactor comprises a substrate 1, the substrate 1 is in the shape of a rectangle, a first channel 2 is provided on one end face of the substrate 1, the first channel 2 is composed of a plurality of vertical sections 3 and a plurality of arc sections 4, the vertical sections 3 and the arc sections 4 are arranged at intervals to form a snake-shaped first channel 2; an outermost vertical section 3 is used as a liquid inlet end, the liquid inlet end is provided with a first groove 5, and a plug connector 6 is connected to the first groove 5; another outermost vertical section 3 is used as a liquid outlet end, the liquid outlet end is provided with a second groove 7, and the plug connector 6 is connected to the second groove 7; the plug connector 6 protrudes out 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 connected to the first channel 2; the substrate 1 is provided with a A second channel 10 connected to the vertical section 3 is provided, and 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 positions of the second channels 10 on both sides are staggered. The second channel 10 is composed of an oblique line segment 11 and a curved section 12. The oblique line segment 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 providing 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 the full 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.

[0056] 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.

[0057] like Figure 6 As shown, as an optimization of the first embodiment, 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 first serpentine-shaped 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 problem of liquid leakage is avoided.

[0058] like Figure 7 to Figure 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, and the disassembly and assembly are cumbersome, and 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, and the shell 17 is fixed with a cover 19 that closes the receiving groove 18 by bolts; the receiving groove 18 is used to install the substrate 1, the number of substrates 1 is 2, the serpentine first channels 2 of the two substrates 1 are against the receiving groove 18, the two substrates 1 are squeezed and fixed by a positioning mechanism 20, and the positioning mechanism 20 is arranged 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, and 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, and a 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, avoiding the influence of the ambient temperature on the heat exchange effect, and the heat exchange effect is good; the accommodating groove 18 is provided with a funnel groove 25 adapted to the plug connector 6, and the shell 17 is provided with a through hole 26 connected to the upper funnel groove 25, 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; the shell 17 is provided with a U-shaped channel 27 connected to the lower funnel groove 25, and the fluid first enters the first channel 2 of the left substrate 1 from the through hole 26 on the left side, 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 side, thus forming a flow path for the fluid reaction; the substrate 1 is fixed by setting a positioning mechanism 20, which is simple to disassemble and assemble, and a heat exchange gap 21 is formed between the substrates 1, which greatly improves the heat exchange effect.

[0059] like Figure 14~Figure 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, and the sealed bearing 28 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 to a clamping member 30 arranged at equal intervals. The number of the clamping members 30 is at least 3. The clamping 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 The 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 arranged on the cover body 19; by rotating the hexagonal rotating head 33, the position of the clamping member 30 can be adjusted, and when the minimum outer diameter of the clamping member 30 is opposite to the substrate 1, the substrate 1 can be quickly removed, and 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.

[0060] like Fig.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 3 forms a group and are arranged from top to bottom. By setting the first springs 35, the two substrates 1 in the initial state are close to each other, which facilitates the removal of the substrates 1.

[0061] like Fig.19 As shown, as an optimization of the first embodiment, the clamping member 34 includes a first carrier 36 connected to the cover body 19, the number of the first carriers 36 is 2, the two first carriers 36 are symmetrically arranged, the first carrier 36 is slidably connected with a first guide rod 37, the number of the first guide rods 37 is 2, the first guide rods 37 are connected with a chuck 38, the shape of the chuck 38 is U-shaped, the two chucks 38 are used to clamp the hexagonal rotating head 33, the chuck 38 is pushed by a bolt rod 39, the bolt rod 39 is threadedly connected to the first carrier 36, and the two chucks 38 are moved toward each other by rotating the bolt rod 39 until the chuck 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.

[0062] like Fig. 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 surface of the shell 17 is provided with a plug hole 40 connected to the vertical section 3, and at least two plug holes 40 are corresponding to one vertical section 3. The plug hole 40 is provided with an expanded hole 41 opposite to the vertical section 3, and a threaded plug 42 is connected to the plug hole 40, and a second spring 43 is connected to the threaded plug 42. The free end of the second spring 43 is connected to a first push plate 44, and the first push plate 44 is against the accommodating groove 18, and the second spring 4 3 makes the first push plate 44 close 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, and the bellows 45 can prevent the fluid from entering the plug hole 40; a first air injection hole 46 is opened at the center of the wire plug 42, and air is injected into the first air injection hole 46 to expand the bellows 45, 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 substrate 1.

[0063] like Fig.21 and Fig. 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 plugging piece 47 is threadedly connected to the first gas injection hole 46, and a second gas injection hole 48 penetrating the first gas injection hole 46 is provided on the shell 17, and 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, and 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, and the cylindrical valve body 51 is used to close the first gas injection hole 46, and 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, which will not affect the stacking of multiple shells 17.

[0064] like Fig.23 and Fig.24As shown, the second embodiment is different from the first embodiment 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 plurality 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 layered, the flow rate of the cooling air is slowed down, and the cooling effect is improved; and the first guide plate 56 and the second guide plate 58 can be folded, which is convenient for disassembly and assembly of the substrate 1.

[0065] like Fig.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, and 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, and 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, and 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.

[0066] like Figure 26~Figure 29As shown, the fourth embodiment is different from the first embodiment 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, and the end face of the shell 17 is provided with a plug hole 40 connected to the vertical section 3, and at least two plug holes 40 are corresponding to one vertical section 3, and a plug hole 40 is threadedly connected with a plug 42, and the plug 42 is connected with a second spring 43, and the free end of the second spring 43 is connected with 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, and the first push plate 44 is located The cover 19 is in the vertical section 3 and does not affect the flow of the fluid; the bottom surface of the cover 19 is connected to a support 62, the number of the support 62 is 2, the two supports 62 are located in the heat exchange gap 21, the support 62 is connected to an iron plate 63, the number of the iron plates 63 is 2, the two iron plates 63 are symmetrically arranged, the projection area of ​​the iron plates 63 is larger than the projection area of ​​the snake-shaped first channel 2, the gap between the two iron plates 63 is adsorbed with a first magnet 64, the number of the first magnet 64 is at least 3, the three first magnets 64 are arranged in sequence from front to back, the N pole of the first magnet 64 is on the left and the S pole is on the right; the iron plate 63 is connected to a fixing seat 65, 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 a 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 N pole of the second magnet 68 and the third magnet 69 is on the right side, and the S pole is on the left side. At this time, the upper and lower magnetic poles are opposite, forming a closed circuit. The iron plate 63 is non-magnetic to the outside. When the blockage needs to be cleared, the rotating handle 70 is rotated 180°. At this time, the N pole of the second magnet 68 and the third magnet 69 is on the left side, and the S pole is on the right side. 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 is magnetic 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 and expand the first channel 2, so that the blockage can be cleared without disassembling the substrate 1.

[0067] like Fig.30As shown, embodiment 5 is different from embodiment 1 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 an arc groove 74, and the arc groove 74 is adapted to the inner hexagonal rotating head 33; the second carrier 71 is rotatably connected with a 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 and the inner hexagonal rotating head 33 are completely pressed, thereby realizing the positioning of the pressing member 30, and then the two substrates 1 can carry out the microchannel reaction process.

[0068] like Fig.31 and Fig.32 As shown, the sixth embodiment is different from the first embodiment in that, considering that a single housing 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 lead screw 79, the second bidirectional lead screw 79 is threadedly connected to a first clamping seat 80, and a plurality of housings 17 are arranged between the two first clamping seats 80, the through holes 26 of adjacent housings 17 are opposite, and a docking hole 81 is opened on the through hole 26, and the diameter of the docking hole 81 is greater than The diameter of the through hole 26 is a butt joint 82 inserted into the butt joint 81. By setting the butt joint 82, the end faces of the two shells 17 are completely fitted together to avoid leakage. The top frame 77 is connected to a second bearing seat 83. The number of the second bearing seats 83 is 2. The second bearing seat 83 is rotatably connected to the third bidirectional lead screw 84. The third bidirectional lead screw 84 is threadedly connected to a second clamping seat 85. 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 achieves a better reaction effect.

[0069] like Fig.33 As shown, as an optimization of the sixth embodiment, 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 setting the second sealing ring, the problem of coolant leakage is avoided.

[0070] At present, there are two main production processes of sulfentrazone (one-step reaction method and two-step reaction method): 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) and methylsulfonyl chloride react in dichloromethane solvent under the action of acid-binding agent triethylamine to generate a bismethylsulfonylamine derivative (compound II); then compound II is hydrolyzed with sodium hydroxide aqueous solution in ethanol solution to obtain sulfentrazone with a yield of 66%. In the reaction, each molecule of compound I consumes 2.25 mol of methylsulfonyl chloride and 2.25 mol of triethylamine. One-step reaction method: Compound I and methylsulfonyl chloride are used to synthesize sulfentrazone in one step under the action of a catalyst. The problems with these processes are: Mass transfer and heat transfer limitations: The mass transfer and heat transfer efficiency in the reactor used in the current production process is extremely low, which limits the improvement of the reaction rate and product selectivity.

[0071] like Fig.34 As shown, further, a fully automated sulfentrazone production process using a microchannel reactor is proposed, comprising the following steps: ① Condensation: Phenylhydrazine and tert-butyl alcohol are mixed evenly in a microreactor, acetaldehyde is added dropwise, and after testing, sodium cyanate is added, acetic acid is added dropwise, sodium hypochlorite is added dropwise after heat preservation, and after reaction in a coil reactor and a continuous flow YX microreactor, desolventization, crystallization, and filtration are performed to obtain intermediate 1 (MTZ); ② Fluoromethylation: DMF, intermediate 1 (MTZ) and potassium carbonate were added to the reactor, and after heating and refluxing for dehydration, freon was introduced for reaction. After the test was qualified, the intermediate 2 (F-MTZ) was obtained by filtration; ③ Chlorination: Add intermediate 2 (F-MTZ) into the reactor, introduce chlorine gas to react, and after the monochlorination reaction is qualified, degas and then desolventize to obtain intermediate 3 (CMTZ); then carry out dichlorination reaction, add acetic acid into the reactor and stir, and then introduce chlorine gas again. After the reaction test is qualified, cool and crystallize, filter and dry to obtain intermediate 4 (DCMTZ); ④ Nitration: Add concentrated sulfuric acid and intermediate 4 (DCMTZ) into the microchannel reactor, stir evenly and then add fuming nitric acid. After the reaction is completed, add water and extract with toluene to obtain intermediate 5 (nitrate toluene liquid). Microchannel reactor is very suitable for nitration reaction, and the reaction time is generally 0.3~2min. The reaction temperature can be higher than that of traditional reactors. The higher the concentration of sulfuric acid, the faster the nitration rate. Microchannel reactor strengthens the heat transfer and mass transfer process, weakens the steric hindrance effect in the reaction, weakens the relationship between selectivity and various factors, and improves selectivity. The reaction is safer, and the strengthening of the transfer process makes the reaction process in the reactor easier to control. ⑤ Reduction: intermediate 5 (nitrate toluene liquid) and catalyst are placed in the autoclave, and hydrogen is introduced after nitrogen replacement for reaction. After the test is qualified, the catalyst is filtered by ethanol after cooling and pressure relief, and then desolventization and crystallization are performed to obtain intermediate 6 (amide toluene liquid); ⑥ Acylation: put intermediate 6 (amide toluene solution) into the kettle, add methylsulfonyl chloride dropwise and keep warm for reaction. After the reaction is qualified, desolventize and obtain the sulfentrazone finished product after cooling, crystallization, filtration and drying.

[0072] Although the present invention has been described in detail with reference to the aforementioned examples, it is still possible for those skilled in the art to make and modify the technical solutions described in the aforementioned 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 protection scope of the present invention.

Claims

1. A microchannel reactor, comprising a substrate (1), characterized in that: A first channel (2) is provided on one end surface of the substrate (1), the first channel (2) being composed of a plurality of vertical sections (3) and a plurality of arc sections (4), the vertical sections (3) and the arc sections (4) being arranged at intervals to form a snake-shaped first channel (2); an outermost vertical section (3) is used as a liquid inlet end, the liquid inlet end is provided with a first groove (5), and the first groove (5) is provided with a plug connector (6); another outermost vertical section (3) is used as a liquid outlet end, the liquid outlet end is provided with a second groove (7), and the second groove (7) is provided with the plug connector (6); the substrate (1) is provided with a plurality of vertical sections (3) and a plurality of arc sections (4) arranged at intervals to form a snake-shaped first channel (2); ) is connected to the first channel (2), the second channel (10) is arranged on both sides of the vertical section (3), the plurality of 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 an oblique line segment (11) and a curved section (12), the oblique line segment (11) serves as an upstream side for fluid to flow through, and the curved section (12) serves as a downstream side for fluid to flow through, 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).

2. A microchannel reactor according to claim 1, characterized in that: The plug connector (6) protrudes outside the base plate (1), and a tapered surface is provided on the protruding end of the plug connector (6). A transverse hole (8) is provided at the center of the plug connector (6), and a vertical hole (9) communicating with the transverse hole (8) is provided on the side wall of the plug connector (6). The vertical hole (9) communicates with the first channel (2).

3. A microchannel reactor according to claim 1, characterized in that: The vertical section (3) of the first channel (2) is provided with third grooves (14) arranged at equal intervals.

4. A microchannel reactor according to claim 1, characterized in that: The end surface of the substrate (1) is provided with a first sealing groove (15), 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 provided in the first sealing groove (15).

5. A microchannel reactor according to claim 1, characterized in that: The housing (17) further comprises a housing (17) for accommodating a substrate (1). The top surface of the housing (17) comprises a receiving groove (18). The housing (17) comprises a cover (19). The receiving groove (18) is used to install the substrate (1). The number of substrates (1) is two. The first channel (2) abuts against the receiving groove (18). The two substrates (1) are fixed by being squeezed by a positioning mechanism (20). A heat exchange gap (21) is formed between the two substrates (1). The bottom surface of the housing (17) comprises two T-shaped holes (22). The T-shaped holes (22) comprise T-shaped tubes (23). The T-shaped tubes (23) are fixed by positioning nuts (24). The receiving groove (18) comprises a funnel groove (25) adapted to the plug connector (6). The housing (17) comprises a through hole (26) communicating with the upper funnel groove (25). The housing (17) comprises a U-shaped channel (27) communicating with the lower funnel groove (25).

6. A microchannel reactor according to claim 5, characterized in that: There are two positioning mechanisms (20), and the positioning mechanisms (20) include a sealed bearing (28), the sealed bearing (28) is rotatably connected to the cover body (19), a rotating rod (29) is rotatably connected to the sealed bearing (28), the lower end of the rotating rod (29) is rotatably connected to the housing (17), the rotating rod (29) is located in the middle of the accommodating groove (18), and the side wall of the rotating rod (29) is provided with a clamping member (30) arranged at equal intervals, and the clamping 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 base plates (1), and the straight section of the semicircular cam (31) has a square limit block (32); 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 provided with a hexagonal rotating head (33), and the hexagonal rotating head (33) is positioned by a clamping member (34).

7. A microchannel reactor according to claim 5, characterized in that: The end surface of the shell (17) is provided with a plug hole (40) connected to the vertical section (3); the plug hole (40) is provided with a flared hole (41) opposite to the vertical section (3); the plug hole (40) is provided with a thread plug (42); the thread plug (42) is provided with a second spring (43); a first push plate (44) is provided at the free end of the second spring (43); and the second spring (43) enables the first push plate (44) to close the flared hole (41) in an initial state; the first push plate (44) is located in the vertical section (3); a bellows (45) is provided between the first push plate (44) and the plug hole (40); and a first air injection hole (46) is provided at the center of the thread plug (42).

8. A microchannel reactor according to claim 5, characterized in that: A plurality of flow guide components (54) are arranged on opposite surfaces of the two substrates (1), and the flow guide components (54) are arranged at equal intervals from top to bottom; a first shaft seat (55) is provided on one substrate (1), and a first flow guide plate (56) is rotatably connected to the first shaft seat (55), and the first flow guide plate (56) is arranged obliquely upward; a second shaft seat (57) is provided on the other substrate (1), and a second flow guide plate (58) is rotatably connected to the second shaft seat (57), and the second flow guide plate (58) is arranged obliquely upward, and the second flow guide plate (58) is rotatably connected to the first flow guide plate (56) via a rotating shaft (59).

9. A microchannel reactor according to claim 5, characterized in that: The invention also comprises a bottom frame (76) and a top frame (77). The bottom frame (76) is provided with a first bearing seat (78). The number of the first bearing seats (78) is two. The first bearing seat (78) is rotatably connected to a second bidirectional lead screw (79). The second bidirectional lead screw (79) is threadedly connected to a first clamping seat (80). A plurality of housings (17) are arranged between the two first clamping seats (80). The through holes (26) of adjacent housings (17) are opposite to each other. The through holes (26) are provided with docking holes (81). The docking holes (81) are plugged with docking pipes (82). The top frame (77) is provided with a second bearing seat (83). The number of the second bearing seats (83) is two. The second bearing seat (83) is rotatably connected to a third bidirectional lead screw (84). The third bidirectional lead screw (84) is threadedly connected to a second clamping seat (85). The two second clamping seats (85) are used to clamp the housing (17).

10. A fully automated sulfentrazone production process using the microchannel reactor according to any one of claims 1 to 9, characterized in that: The following steps are involved: ① Condensation: Phenylhydrazine and tert-butyl alcohol are mixed evenly in a microreactor, acetaldehyde is added dropwise, and after testing, sodium cyanate is added dropwise, acetic acid is added dropwise, sodium hypochlorite is added dropwise after heat preservation, and 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 are added to the reaction kettle, and after heating and refluxing for dehydration, freon is introduced for reaction. If the product is qualified, it is 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 and stir, 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 drop fuming nitric acid. After the reaction is completed, drop water and extract with toluene to obtain intermediate 5; ⑤ Reduction: intermediate 5 and catalyst are placed in the autoclave, and hydrogen is introduced after nitrogen replacement for reaction. After the test is qualified, the temperature is reduced and the pressure is released, and the catalyst is filtered by ethanol, and then the intermediate 6 is obtained by desolventizing and crystallizing; ⑥ Acylation: intermediate 6 is added into the kettle, and methylsulfonyl chloride is added dropwise to carry out heat preservation reaction. After the reaction is qualified, desolventization is carried out, and the sulfentrazone finished product is obtained after cooling, crystallization, filtration and drying.

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