Dynamic tubular reactor and process for preparing flumioxazin

Abstract

The invention discloses a dynamic tubular reactor and a process for preparing flumioxazin, and solves the problems that a blade type spoiler of an existing reactor cannot be automatically adjusted to be retracted and released according to the reaction degree, so that the discharge of a reaction product is influenced; in order to solve the problems that the flow rate and the pressure of a reaction fluid are changed and leakage is easily caused at a flow channel inlet and a flow channel outlet, the dynamic tubular reactor comprises an equipment base, a dynamic reaction mechanism and a reaction driving mechanism, and the dynamic reaction mechanism comprises a dynamic reaction tube, an anti-blocking protection part and a nitrification stirring part; the reaction driving mechanism comprises a driving motor and a reaction driving shaft; according to the device, the anti-blocking protection part and the reaction driving mechanism are arranged, the technical means that the reaction driving mechanism and the anti-blocking protection part are cooperatively matched is adopted, fluid dynamic balance in nitration reaction can be broken, leakage of the reaction feeding port and the reaction discharging port is avoided, the anti-blocking protection part can be automatically retracted and released after reaction, and therefore flumioxazin intermediates can be conveniently discharged; and blockage is avoided.

Description

Technical Field

[0001] The invention belongs to the technical field of tubular reactors, and in particular relates to a dynamic tubular reactor and a process for preparing fluazifop-butyl. Background Art

[0002] Flumioxazin is an N-phenylphthalimide herbicide and a highly effective protoporphyrinogen oxidase (PPO) inhibitor. It causes a large accumulation of protoporphyrin in sensitive crops, enhances cell membrane lipid peroxidation, and thus leads to irreversible damage to cell membrane structure and cell function. In the synthesis process of flumioxazin intermediates, it is necessary to undergo multiple steps of fluorine hydrolysis, nitration, cyclization, propynylation, phthalic anhydride acylation, etc., and the nitration reaction of flumioxazin intermediates is one of the key steps in the synthesis of the herbicide, which involves introducing a nitro group (-NO2) into a specific compound through nitration to provide the necessary functional groups for subsequent reactions.

[0003] At present, the nitration reactor is a common reaction vessel for the nitration reaction of the intermediate of fluazifop-butyl, which has the characteristics of acid and alkali resistance, high temperature resistance, corrosion resistance, etc. Chinese patent CN115212838A discloses a tubular continuous flow reactor with self-rotating turbulence. The reactor of the present invention includes a reaction fluid mixing channel, and the two ends of the reaction fluid mixing channel are respectively provided with a channel inlet and a channel outlet. The reaction fluid mixing channel is filled with a blade-type spoiler, and the spoiler completes the collision and rotary cutting of multiple fluids in the fluid mixing channel to achieve efficient heat and mass transfer. A heat exchange channel is provided adjacent to the outside of the reaction fluid mixing channel, and a heat exchange medium inlet and outlet are provided at both ends of the channel. A heat pipe is provided adjacent to the outside of the heat exchange channel, but the existing reactor blade spoiler cannot automatically adjust the retraction and release according to the degree of reaction, which affects the discharge of the reaction product. At the same time, the flow channel inlet and the flow channel outlet are prone to leakage due to changes in the flow rate and pressure of the reaction fluid. In view of the above problems, we propose a dynamic tubular reactor and process for preparing fluazifop-butyl. Summary of the invention

[0004] The purpose of the present invention is to address the deficiencies of the prior art and provide a dynamic tubular reactor and process for preparing fluazifop-butyl, which solves the problem that the blade-type spoilers of the existing reactor cannot automatically adjust their retraction and extension according to the degree of reaction, affecting the discharge of the reaction products, and the flow channel inlet and outlet are prone to leakage due to changes in the flow rate and pressure of the reaction fluid.

[0005] The blade-type spoilers of the existing reactor cannot automatically adjust their retraction and extension according to the degree of reaction, which affects the discharge of the reaction products. At the same time, leakage is prone to occur at the flow channel inlet and the flow channel outlet due to changes in the flow rate and pressure of the reaction fluid. In view of the above problems, we propose a dynamic tubular reactor and a process for preparing fluazifop-butyl. In short, the dynamic tubular reactor for preparing fluazifop-butyl is composed of an equipment base, a dynamic reaction mechanism, and a reaction driving mechanism, and the dynamic reaction mechanism includes a dynamic reaction tube, at least one group of anti-blocking protection parts, and a nitration stirring part. The reaction driving mechanism includes a driving motor and a reaction driving shaft; in the embodiment of the present invention, an anti-blocking protection part and a reaction driving mechanism are provided, and the technical means of the coordinated cooperation of the reaction driving mechanism and the anti-blocking protection part can break the dynamic balance of the fluid in the nitration reaction, thereby improving the nitration preparation efficiency of the fluazifop-butyl intermediate, and avoiding leakage of the reaction feed port and the reaction discharge port. The anti-blocking protection part can also be automatically retracted and extended after the reaction, thereby facilitating the discharge of the fluazifop-butyl intermediate and avoiding blockage. The invention effectively overcomes the problem that the existing reactor blade spoilers cannot automatically adjust their retraction and extension according to the degree of reaction, which affects the discharge of reaction products, and the flow channel inlet and outlet are prone to leakage due to changes in the flow rate and pressure of the reaction fluid.

[0006] The present invention is achieved by a dynamic tubular reactor for preparing fluazifop-butyl, wherein the dynamic tubular reactor for preparing fluazifop-butyl comprises:

[0007] Equipment base;

[0008] A dynamic reaction mechanism fixedly mounted on a base of the device;

[0009] A reaction drive mechanism, the reaction drive mechanism is arranged on the device base, and the reaction drive mechanism is used to drive the dynamic reaction mechanism;

[0010] Dynamic response mechanisms include:

[0011] A dynamic reaction tube, wherein a dynamic reaction chamber is provided in the dynamic reaction tube, a reaction feed port and a reaction discharge port are respectively provided on both sides of the dynamic reaction chamber, a metering feeding pipe is fixedly installed at one end of the reaction feed port, and the metering feeding pipe is used to inject the reaction raw materials for preparing fluazifop-butyl into the reaction feed port;

[0012] At least one group of anti-blocking protection parts, the anti-blocking protection parts are arranged in the reaction feed port and the reaction discharge port, and the anti-blocking protection parts are used to protect the reaction feed port and the reaction discharge port and prevent leakage of the reaction feed port and the reaction discharge port;

[0013] At least one nitration stirring section, wherein the nitration stirring section is arranged in the dynamic reaction chamber and is used for stirring and mixing the reaction raw materials for preparing fluazifop-butyl;

[0014] Wherein, the reaction drive mechanism comprises:

[0015] A driving motor, wherein the driving motor is fixedly mounted on the device base;

[0016] A reaction drive shaft is fixedly connected to the output end of the drive motor, and one end of the reaction drive shaft away from the drive motor passes through the equipment base and the side wall of the dynamic reaction tube, extends into the dynamic reaction chamber, and is respectively connected to the anti-blocking protection part and the nitrification stirring part.

[0017] Preferably, the nitrification stirring unit comprises:

[0018] A stirring mounting seat, the stirring mounting seat is fixedly mounted on the outer wall of the reaction drive shaft;

[0019] at least one set of nitrification stirring rods, wherein the outer wall of the nitrification stirring rods is provided with a flow disturbance auger, and

[0020] A nitration hammer ball detachably mounted on the end of the nitration stirring rod.

[0021] Preferably, the anti-blocking protection part comprises:

[0022] An inner positioning seat, the inner positioning seat is rotatably sleeved on the outer wall of the reaction drive shaft, and one end of the inner positioning seat is detachably connected to the inner wall of the dynamic reaction tube;

[0023] At least one set of inner limiting grooves, wherein the inner limiting grooves are arranged on the inner positioning seat;

[0024] An anti-blocking linkage seat is rotatably sleeved on the outer wall of the inner positioning seat, and the anti-blocking linkage seat is fixedly connected to the outer wall of the reaction drive shaft;

[0025] At least one set of retractable spoilers, wherein the retractable spoilers are fixedly mounted on the ends of the adjustable spoiler shafts, and one end of the adjustable spoiler shaft away from the retractable spoilers penetrates the anti-blocking linkage seat and is rotatably connected to the side wall of the anti-blocking linkage seat;

[0026] At least one group of arc-shaped flip plates is arranged between the inner positioning seat and the anti-blocking linkage seat, one side of the arc-shaped flip plate is fixedly connected to the adjustable spoiler shaft, and the other side of the arc-shaped flip plate is fixedly connected to at least one group of inner hinge blocks, and the inner hinge blocks are slidably embedded in the inner limit grooves.

[0027] Preferably, the dynamic tubular reactor for preparing fluazifop-butyl also includes:

[0028] An auxiliary cooling component, which is sleeved on the dynamic reaction tube and is used to assist in cooling the raw materials in the dynamic reaction chamber;

[0029] At least one set of anti-leakage components, which are installed in the reaction feed port and the reaction discharge port, and are used to prevent leakage from the reaction feed port and the reaction discharge port, and eliminate the water hammer effect caused by the flow of liquid raw materials in the dynamic reaction chamber.

[0030] Preferably, the reaction drive mechanism further comprises:

[0031] A cooling adjustment unit, the cooling adjustment unit is arranged on the equipment base, and the cooling adjustment unit is used to adjust the position of the auxiliary cooling assembly;

[0032] The cooling and regulating unit includes:

[0033] A cooling adjustment shaft, wherein the cooling adjustment shaft is rotatably mounted on the equipment base;

[0034] An adjusting threaded sleeve is threadedly sleeved on the outer wall of the cooling adjusting shaft, and the adjusting threaded sleeve is connected to the auxiliary cooling assembly;

[0035] An intermittent drive unit is connected to the reaction drive shaft and is installed on the equipment base. The intermittent drive unit is used for intermittent linkage driving of the cooling adjustment shaft.

[0036] Preferably, the auxiliary cooling assembly comprises:

[0037] A component support seat, wherein the component support seat is slidably mounted in the equipment base, and one side of the component support seat is detachably connected to the side wall of the adjusting threaded sleeve;

[0038] A medium guide pipe is fixedly mounted on the component support seat, and is used to guide the cooling medium. One end of the medium guide pipe is provided with a medium injection port, and the other end is provided with a medium return port.

[0039] Preferably, the intermittent driving unit comprises:

[0040] A first gear, the first gear is rotatably mounted on the device base, and the first gear is fixedly connected to the outer wall of the reaction drive shaft;

[0041] A second gear is arranged on one side of the first gear, the second gear is rotatably connected to the device base, and the second gear is meshed with the first gear for transmission, and a limiting groove is provided on a side wall of the second gear;

[0042] A swing link, wherein the swing link is rotatably mounted on the equipment base, one end of the swing link is slidably connected to the limit groove, and the other end of the swing link is hinged to the limit connection seat;

[0043] A rack limit seat fixedly connected to the limit connecting seat;

[0044] A swing rack, wherein the swing rack is slidably mounted in the rack limit seat, one end of the swing rack is hinged to the side wall of the second gear, the other end of the swing rack is meshedly connected to the third gear, and the side wall of the third gear is fixedly connected to the end of the cooling adjustment shaft;

[0045] A lifting locking seat is slidably installed on the equipment base, the upper end of the lifting locking seat is rotationally connected to the end of the swing connecting rod, and the lower end of the lifting locking seat is fixedly installed with a gear locking tooth, which is used to lock the third gear.

[0046] Preferably, the anti-leakage component comprises:

[0047] An anti-leakage seat, wherein the anti-leakage seat is fixedly mounted on the side wall of the dynamic reaction tube, and a slow-flow protection seat is fixedly connected to the bottom of the anti-leakage seat, and at least one group of fluid delay plates is arranged in the slow-flow protection seat;

[0048] An anti-impact linkage part, which is arranged in the anti-leakage seat;

[0049] A gas filter box is detachably mounted on the top of the anti-leakage seat, and the gas filter box is used to filter the gas released by the anti-leakage seat.

[0050] Preferably, the anti-shock linkage part comprises:

[0051] An anti-impact swing seat, wherein the anti-impact swing seat is movably arranged in the anti-leakage seat, and the upper part of the anti-impact swing seat is hinged with a linkage guide rod through a universal ball, and the linkage guide rod is fixedly installed in the anti-leakage seat;

[0052] A reciprocating piston plate is slidably arranged in the anti-leakage seat, and the reciprocating piston plate is also slidably sleeved on the outside of the linkage guide rod, and a double-sided gear seat is fixedly arranged on the reciprocating piston plate;

[0053] At least one group of anti-impact linkage rods, one end of which is hinged to the anti-impact swing seat, and the other end is fixedly mounted with lifting teeth, which mesh with the double-sided tooth seat for transmission.

[0054] On the other hand, the present invention also provides a process for preparing fluazifop-butyl, which comprises:

[0055] Step S10, alkaline hydrolysis and acidification reaction, using 2,4-difluoronitrobenzene as a starting material, 2,4-difluoronitrobenzene is subjected to alkaline hydrolysis reaction to obtain an intermediate 5-fluoro-2-nitrophenol;

[0056] Step S20, etherification reaction, adding a certain amount of DMF to the etherification kettle, starting stirring, opening the manhole, adding potassium carbonate and potassium iodide into the etherification kettle, slowly dropping a solution containing the intermediate 5-fluoro-2-nitrophenol and DMF at room temperature under nitrogen protection, and then dropping methyl chloroacetate, keeping the temperature for 4 hours after the addition, sampling and testing until the alkaline hydrolyzate is less than 0.5%, cooling to room temperature, centrifuging, and drying to obtain an etherified product, which is the intermediate 5-fluoro-2-nitrophenoxyacetic acid methyl ester;

[0057] Step S30, a reduction reaction, DMF, intermediate 5-fluoro-2-nitrophenoxyacetic acid methyl ester and Raney nickel (10% added each time) are added to the reduction kettle in sequence, the manhole is closed, and 10Kg / cm 2 Nitrogen was flushed and discharged 3 times, and then filled with hydrogen, maintaining the pressure at 7Kg / cm 2 , stir the reduction kettle, heat the reduction kettle to 60℃, and keep the reaction at 60-70℃, maintaining the hydrogen pressure at 7Kg / cm 2 , repeatedly filling with hydrogen until the pressure no longer decreases, keeping warm for 2 hours, the reaction is completed, and a reduced product is obtained, which is the intermediate 7-fluoro-2H-1,4-benzoxazine-3(4H)-one;

[0058] Step S40, nitration reaction, using a dynamic reaction tube to nitrate the intermediate 7-fluoro-2H-1,4-benzoxazine-3(4H)-one to obtain the intermediate 7-fluoro-6-nitro-2H-1,4-benzoxazine-3(4H)-one;

[0059] Step S50, secondary reduction reaction, DMF, intermediate 7-fluoro-6-nitro-2H-1,4-benzoxazine-3(4H)-one and Raney nickel (10% added each time) are sequentially added into the nitro reduction kettle, the manhole is closed, and 10Kg / cm 2 Nitrogen was flushed and discharged 3 times, and hydrogen was filled in to maintain the pressure at 7Kg / cm 2 , stir thoroughly, heat to 60℃, and keep the temperature at 60-70℃ for reaction, maintaining the hydrogen pressure at 7Kg / cm 2 , repeatedly filling with hydrogen until the pressure no longer drops, keeping warm and stirring for 2 hours, the reaction is completed, and the intermediate 7-fluoro-6-amino-2H-1,4-benzoxazin-3(4H)-one is obtained;

[0060] Step S60, propynylation reaction, DMF is added to the propylation kettle, the propylation kettle is stirred, the intermediate 7-fluoro-6-amino-2H-1,4-benzoxazine-3(4H)-one, catalyst and potassium hydroxide are added to the propylation kettle, and the propylation kettle is stirred for 0.5 hour after the addition is completed. The nitrogen valve is opened to replace the nitrogen, and the temperature is maintained. A certain amount of chloropropyne is added dropwise within 2 hours. After the addition is completed, the reaction is stirred and kept warm for 8 hours. Sampling is performed to detect that the nitro reduction product is less than 1.0%, stirring of the water washing kettle is turned on, distilled water is added, and frozen brine is turned on, and the reaction is cooled to 0-5°C and maintained at 0-5°C. The reaction liquid in the propylation kettle is slowly transferred to the water washing kettle. After the transfer is completed, the brine is pressed out, the temperature is naturally raised and stirred for 1 hour, and the centrifugation is performed. The wet product is rinsed with water and vacuum dried at 80°C to obtain the intermediate 7-fluoro-6-amino-4-(2-propargyl)2H-1,4-benzoxazine-3(4H)-one;

[0061] Step S70, condensation reaction, add acetic acid to the condensation kettle, start stirring the condensation kettle, open the manhole, add the intermediate 7-fluoro-6-amino-4-(2-propargyl)2H-1,4-benzoxazine-3(4H)-one and tetrahydrophthalic anhydride to the condensation kettle in sequence, heat the condensation kettle for reaction for 4 hours, take samples until the propyne compound is ≤1%, cool the condensation kettle to 50-60°C and keep it warm for 1 hour, cool it naturally and continue stirring for 2 hours, cool it to 20-25°C, stir it for 1 hour, centrifuge it, apply the filtrate three times, add new acetic acid to the calibrated high-level tank scale when the mother liquor is applied, add a certain amount of dichloroethane to the crystallization kettle, add the above filter cake to the crystallization kettle, heat it to reflux for 0.5 hours, cool it to room temperature for 4 hours, centrifuge it, apply the mother liquor, and vacuum dry the filter cake at 80°C to obtain the product fluazifop-propylamine.

[0062] The present invention also provides a method for alkaline hydrolysis of 2,4-difluoronitrobenzene, which specifically comprises:

[0063] Step S101, adding distilled water to the alkali preparation kettle, adding potassium hydroxide into the alkali preparation kettle while stirring, preparing a potassium hydroxide solution and cooling it to room temperature for use;

[0064] Step S102, adding 2,4-difluoronitrobenzene and distilled water into the alkaline hydrolysis kettle, heating the alkaline hydrolysis kettle, and then dropping potassium hydroxide solution into the alkaline hydrolysis kettle. After the dropping is completed, the alkaline hydrolysis kettle is kept warm for 1 hour, sampling is performed until 2,4-difluoronitrobenzene is less than 0.5%, distilled water is added, and the material is transferred to the acidification kettle while it is hot;

[0065] Step S103, open the acidification kettle for circulating water cooling, keep the temperature while adding hydrochloric acid dropwise to a pH value of 2-3, let it stand for 0.5 hour, separate the lower organic phase and transfer it to a water washing kettle, transfer the upper water to a wastewater treatment kettle, add distilled water to the water washing kettle and stir for 0.5 hour, let it stand, separate the lower organic phase for high vacuum distillation, use the upper water jacket to the acidification kettle, and distill out the alkaline hydrolyzate under high vacuum. The alkaline hydrolyzate is the intermediate 5-fluoro-2-nitrophenol. Note that the temperature of the receiving port is not lower than 40°C to prevent solidification at the discharge port. Add a certain amount of DMF to dissolve the evaporated material.

[0066] The intermediate 7-fluoro-2H-1,4-benzoxazine-3(4H)-one is subjected to a nitration reaction using a dynamic reaction tube, specifically comprising:

[0067] Step S201, check the dynamic reaction tube and its ancillary equipment, confirm that they are dry and clean, and the valve is in a closed state, take dichloromethane, and transfer it to the dichloromethane metering tank through the dichloromethane intermediate tank for standby, and transfer sulfuric acid to the sulfuric acid metering tank through the sulfuric acid intermediate tank for standby, add concentrated sulfuric acid and 7-fluoro-2H-1,4-benzoxazine-3(4H)-one into the dissolving kettle, stir and dissolve, pass chilled water to cool to below 10°C, and then transfer to the dynamic reaction tube.

[0068] Step S202, after 7-fluoro-2H-1,4-benzoxazine-3(4H)-one, nitric acid, and dichloromethane are injected into the reaction feed port through the metering feeding pipe, the driving motor is turned on, the driving motor starts to drive the reaction driving shaft to rotate, and the reaction driving shaft rotates to drive the stirring mounting seat, the nitration stirring rod, and the nitration hammer ball to stir and mix the raw materials for nitration reaction;

[0069] Step S203, the rotation of the reaction drive shaft can also drive the anti-blocking linkage seat to rotate. The rotation of the anti-blocking linkage seat drives the retractable spoiler to disturb the raw material fluid. At the same time, the inner positioning seat and the inner limit groove limit the inner hinge block, so that the inner hinge block drives the arc-shaped flip plate, the adjustable spoiler shaft and the retractable spoiler to rotate, thereby enhancing the spoiler effect.

[0070] Step S204, the forward and reverse rotation of the reaction drive shaft can drive the first gear to rotate, the rotation of the first gear drives the rotation of the second gear, the rotation of the second gear can drive the limiting groove to rotate, the limiting groove drives the swing connecting rod to swing, the swing connecting rod drives the limiting connecting seat and the rack limiting seat to guide and limit the swing rack, and at the same time, the rotation of the second gear drives the swing rack to swing, and the end of the swing rack away from the second gear intermittently meshes with the third gear, so that the third gear drives the cooling adjustment shaft to rotate, and the rotation of the cooling adjustment shaft drives the adjusting threaded sleeve and the component supporting seat to reciprocate along the equipment base, thereby realizing the adjustment of the cooling position of the medium guide tube, and by controlling the feed amount and the circulation amount of the cooling medium in the dynamic reaction tube, the reaction temperature of the dynamic reaction tube is kept below 10°C.

[0071] Step S205, the material discharged from the dynamic reaction tube enters the nitration material buffer tank for sampling and analysis, and the reaction is determined to be complete when the raw material content is less than 0.5%.

[0072] Step S206, the reaction liquid in the nitration material buffer tank overflows into the oleic acid separation tank for separation, the upper organic phase overflows into the dichloromethane removal intermediate tank, and then goes to the dichloromethane recovery kettle to recover dichloromethane, the lower acid phase flows into the hydrolysis kettle, the material is centrifuged, and dried at 80° C. to obtain the intermediate 7-fluoro-6-nitro-2H-1,4-benzoxazine-3(4H)-one.

[0073] Compared with the prior art, the embodiments of the present application have the following beneficial effects:

[0074] In the embodiment of the present invention, an anti-blocking protection part and a reaction driving mechanism are provided. The technical means of the coordinated cooperation between the reaction driving mechanism and the anti-blocking protection part can break the dynamic balance of the fluid in the nitration reaction, thereby improving the nitration preparation efficiency of the propargyl fluazifop intermediate and avoiding leakage of the reaction feed port and the reaction discharge port. The anti-blocking protection part can also be automatically retracted and released after the reaction, thereby facilitating the discharge of the propargyl fluazifop intermediate and avoiding blockage.

[0075] In the embodiment of the present invention, an anti-blocking protection part is provided, and the anti-blocking protection part is composed of an inner positioning seat, an anti-blocking linkage seat, and a retractable spoiler. The inner positioning seat, the anti-blocking linkage seat, and the retractable spoiler cooperate with each other to automatically flip and adjust the position and angle of the retractable spoiler during the nitration reaction, thereby disturbing the flow of raw materials while avoiding blockage or adsorption of intermediates during discharge. Compared with the prior art, the disturbance effect is better, and at the same time, the disturbance range can be automatically expanded when the water hammer effect occurs in the flow of raw materials, thereby protecting the reaction feed port and the reaction discharge port to avoid leakage of the reaction feed port and the reaction discharge port.

[0076] In the embodiment of the present invention, the setting of the auxiliary cooling component ensures the cooling temperature required for the nitration reaction, thereby avoiding the problem of low efficiency in intermediate preparation due to overheating, and the anti-leakage component can cooperate with the anti-blocking protection part to avoid leakage at the reaction feed port and the reaction discharge port while effectively eliminating the water hammer effect caused by the flow of liquid raw materials in the dynamic reaction chamber.

[0077] In an embodiment of the present invention, an intermittent driving part is provided, and the intermittent driving part is composed of a first gear, a second gear, a third gear, a swing connecting rod, a swing rack and a lifting locking seat. The first gear, the second gear, the third gear, the swing connecting rod and the swing rack are linked together to intermittently drive the third gear and the cooling adjustment shaft to rotate when the reaction drive shaft rotates, thereby achieving the purpose of flexibly adjusting the position of the auxiliary cooling component, which can not only ensure the cooling efficiency of the auxiliary cooling component, but also reduce the energy consumption generated by cooling. BRIEF DESCRIPTION OF THE DRAWINGS

[0078] Figure 1 The present invention provides a schematic structural diagram of a dynamic tubular reactor for preparing fluazifop-butyl.

[0079] Figure 2 The present invention provides an axonometric diagram of a dynamic tubular reactor for preparing fluazifop-butyl.

[0080] Figure 3 It is a structural schematic diagram of the dynamic reaction mechanism provided by the present invention.

[0081] Figure 4 It is a three-dimensional structural schematic diagram of the dynamic reaction mechanism provided by the present invention.

[0082] Figure 5 It is a side view of the dynamic reaction mechanism provided by the present invention.

[0083] Figure 6 yes Figure 5 AA section view.

[0084] Figure 7 It is a schematic diagram of the connection structure between the anti-blocking protection part and the nitrification stirring part provided by the present invention.

[0085] Figure 8 It is a structural schematic diagram of the anti-blocking protection part provided by the present invention.

[0086] Fig. 9 It is a side view of the anti-blocking protection part provided by the present invention.

[0087] Fig.10 It is a structural schematic diagram of the reaction drive mechanism provided by the present invention.

[0088] Fig.11 It is an axonometric diagram of the reaction drive mechanism provided by the present invention.

[0089] Fig.12 It is a structural schematic diagram of the anti-leakage component provided by the present invention.

[0090] Fig.13 It is a bottom view of the anti-leakage component provided by the present invention.

[0091] Fig.14 It is a front view of the anti-leakage component provided by the present invention.

[0092] Fig.15 yes Fig.14 BB section view.

[0093] In the figure: 1-equipment base, 2-dynamic reaction mechanism, 21-dynamic reaction tube, 211-metering feeding tube, 212-reaction feed port, 213-reaction discharge port, 214-dynamic reaction chamber, 22-anti-blocking protection part, 221-inner positioning seat, 222-anti-blocking linkage seat, 223-inner limit groove, 224-inner hinge block, 225-arc flip plate, 226-adjustable spoiler shaft, 227-retractable spoiler plate, 23-nitrification stirring part, 231-stirring mounting seat, 232-nitrification stirring rod, 233-nitrification hammer ball, 3-anti-leakage component, 31-slow flow protection seat, 32-fluid delay plate, 33-anti-impact linkage part, 331-anti-impact swing seat, 332-swinging extension groove, 333-linkage guide rod, 334 -Anti-impact linkage rod, 335-reciprocating piston plate, 336-double-sided gear seat, 337-lifting teeth, 34-anti-leakage seat, 35-gas filter box, 4-reaction drive mechanism, 41-drive motor, 42-reaction drive shaft, 43-cooling adjustment part, 431-cooling adjustment shaft, 432-adjusting threaded sleeve, 44-intermittent drive part, 441-first gear, 442-second gear, 443-limiting groove, 444-swing connecting rod, 445-swing rack, 446-limiting connecting seat, 447-rack limiting seat, 448-third gear, 449-lifting locking seat, 450-gear locking teeth, 5-auxiliary cooling assembly, 51-assembly support seat, 52-medium guide pipe, 53-medium injection port, 54-medium reflux port. DETAILED DESCRIPTION

[0094] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by technicians in the technical field of this application; the terms used in the specification of the application herein are only for the purpose of describing specific embodiments and are not intended to limit this application; the terms "including" and "having" and any variations thereof in the specification and claims of this application and the above-mentioned drawings are intended to cover non-exclusive inclusions. The terms "first", "second", etc. in the specification and claims of this application or the above-mentioned drawings are used to distinguish different objects, not to describe a specific order.

[0095] The blade-type spoilers of the existing reactor cannot automatically adjust their retraction and extension according to the degree of reaction, which affects the discharge of the reaction products. At the same time, leakage is prone to occur at the flow channel inlet and the flow channel outlet due to changes in the flow rate and pressure of the reaction fluid. In view of the above problems, we propose a dynamic tubular reactor and process for preparing fluazifop-butyl. In short, the dynamic tubular reactor for preparing fluazifop-butyl consists of an equipment base 1, a dynamic reaction mechanism 2, and a reaction driving mechanism 4, and the dynamic reaction mechanism 2 includes a dynamic reaction tube 21, at least one group of anti-blocking protection parts 22, The nitration stirring part 23, the reaction drive mechanism 4 includes a drive motor 41 and a reaction drive shaft 42; in the embodiment of the present invention, an anti-blocking protection part 22 and a reaction drive mechanism 4 are provided, and the technical means of the reaction drive mechanism 4 and the anti-blocking protection part 22 in coordination can break the dynamic balance of the fluid in the nitration reaction, thereby improving the nitration preparation efficiency of the propargyl fluazifop intermediate, and avoiding leakage of the reaction feed port 212 and the reaction discharge port 213, and the anti-blocking protection part 22 can also be automatically retracted after the reaction, so as to facilitate the discharge of the propargyl fluazifop intermediate and avoid blockage. It effectively overcomes the problem that the existing reactor blade-type spoiler cannot automatically adjust the retraction and release according to the degree of reaction, affecting the discharge of the reaction product, and at the same time, the flow channel inlet and the flow channel outlet are prone to leakage due to changes in the flow rate and pressure of the reaction fluid.

[0096] The embodiment of the present invention provides a dynamic tubular reactor for preparing fluazifop-butyl, such as Figure 1-Figure 2 As shown, the dynamic tubular reactor for preparing fluazifop-butyl comprises:

[0097] The equipment base 1 may be a rectangular base or an "L"-shaped stand structure;

[0098] A dynamic reaction mechanism 2 fixedly mounted on the equipment base 1;

[0099] A reaction drive mechanism 4, wherein the reaction drive mechanism 4 is disposed on the device base 1, and the reaction drive mechanism 4 is used to drive the dynamic reaction mechanism 2;

[0100] like Figure 3-Figure 6 As shown, the dynamic reaction mechanism 2 includes:

[0101] A dynamic reaction tube 21 is provided with a dynamic reaction chamber 214, and a reaction feed port 212 and a reaction discharge port 213 are respectively provided on both sides of the dynamic reaction chamber 214. A metering feeding pipe 211 is fixedly installed at one end of the reaction feed port 212, and the metering feeding pipe 211 is used to inject the reaction raw materials for preparing fluazifop-butyl into the reaction feed port 212.

[0102] It should be noted that, in the embodiment of the present invention, the dynamic reaction tube 21 can be a circular tube structure with a hollow interior, and the dynamic reaction tube 21 can be made of stainless steel. At the same time, the dynamic reaction tube 21 is lined with enamel to prevent the acidic raw materials (sulfuric acid, hydrochloric acid or nitric acid) from corroding the dynamic reaction tube 21 during the nitration reaction. The bottom of the dynamic reaction tube 21 is fixedly mounted on the bottom surface of the equipment base 1 by fastening bolts or snaps, and the reaction feed port 212 and the reaction discharge port 213 can both be conical or truncated cone structures. The number of metering feeding tubes 211 is at least three groups, and the multiple groups of metering feeding tubes 211 are respectively connected to a dichloromethane metering tank, a nitric acid metering tank, and a 7-fluoro-2H-1,4-benzoxazine-3(4H)-one metering tank.

[0103] At the same time, in the embodiment of the present invention, the dynamic reaction tube 21 is used for nitration reaction to synthesize the intermediate 7-fluoro-6-nitro-2H-1,4-benzoxazine-3(4H)-one of fluazifop-butyl. The required raw materials can be 7-fluoro-2H-1,4-benzoxazine-3(4H)-one, nitric acid, and dichloromethane. The diameter of the dynamic reaction tube 21 is D=1.5 cm, the length is L=40 m, and the online amount of nitration material is V=11 L.

[0104] At least one group of anti-blocking protection parts 22, the anti-blocking protection parts 22 are arranged in the reaction feed port 212 and the reaction discharge port 213, and the anti-blocking protection parts 22 are used to protect the reaction feed port 212 and the reaction discharge port 213 and prevent the reaction feed port 212 and the reaction discharge port 213 from leaking;

[0105] At least one group of nitrification stirring parts 23, wherein the nitrification stirring parts 23 are arranged in the dynamic reaction chamber 214, and the nitrification stirring parts 23 are used to stir and mix the reaction raw materials for preparing fluazifop-butyl;

[0106] Among them, Figure 10-11 As shown, the reaction drive mechanism 4 includes:

[0107] A driving motor 41, wherein the driving motor 41 is fixedly mounted on the device base 1, and the driving motor 41 may be a forward and reverse servo motor, and the driving motor 41 is fixedly mounted on the device base 1 via a clamp or a bracket;

[0108] A reaction drive shaft 42 is fixedly connected to the output end of the drive motor 41, and one end of the reaction drive shaft 42 away from the drive motor 41 passes through the equipment base 1 and the side wall of the dynamic reaction tube 21, extends into the dynamic reaction chamber 214, and is respectively connected to the anti-blocking protection part 22 and the nitrification stirring part 23.

[0109] In this embodiment, one end of the reaction drive shaft 42 is fixedly connected to the output end of the drive motor 41 by interference fit, and the reaction drive shaft 42 is rotatably connected to the equipment base 1 and the side wall of the dynamic reaction tube 21 by a bearing and a sealing flange.

[0110] In the embodiment of the present invention, an anti-blocking protection part 22 and a reaction driving mechanism 4 are provided. The technical means of the coordinated cooperation between the reaction driving mechanism 4 and the anti-blocking protection part 22 can break the dynamic balance of the fluid in the nitration reaction, thereby improving the nitration preparation efficiency of the propargyl fluazifop intermediate and avoiding leakage of the reaction feed port 212 and the reaction discharge port 213. The anti-blocking protection part 22 can also be automatically retracted and released after the reaction, thereby facilitating the discharge of the propargyl fluazifop intermediate and avoiding blockage.

[0111] In a further preferred embodiment of the present invention, Figure 7 As shown, the nitrification stirring unit 23 includes:

[0112] A stirring mounting seat 231, wherein the stirring mounting seat 231 is fixedly mounted on the outer wall of the reaction drive shaft 42;

[0113] at least one set of nitrification stirring rods 232, wherein the outer wall of the nitrification stirring rods 232 is provided with a flow disturbance auger, and

[0114] The nitrification hammer ball 233 is detachably mounted on the end of the nitrification stirring rod 232 .

[0115] In this embodiment, the stirring mounting seat 231 is symmetrically or linearly arranged on the outer wall of the reaction drive shaft 42. The stirring mounting seat 231 is fixedly mounted on the outer wall of the reaction drive shaft 42 by mortise and tenon or plug-in, and the nitrating stirring rod 232 can be arranged on the side wall of the stirring mounting seat 231 in a counterclockwise circumferential tilt. The nitrating stirring rod 232 can be a round rod, a square rod, an arc rod or an "L"-shaped rod structure, and the nitrating stirring rod 232 can be made of ceramic or alloy material resistant to strong acid corrosion. The nitrating stirring rod 232 is fixedly connected to the stirring mounting seat 231 by welding or mortise and tenon. The material of the nitrating hammer ball 233 is consistent with that of the nitrating stirring rod 232. The setting of the nitrifying hammer ball 233 can hammer and turbulent the reaction raw materials, and at the same time, the turbulent auger sleeved on the outer wall of the nitrifying stirring rod can ensure the stirring and mixing efficiency of the raw materials.

[0116] In a further preferred embodiment of the present invention, Figure 8-Figure 9 As shown, the anti-blocking protection part 22 includes:

[0117] An inner positioning seat 221, wherein the inner positioning seat 221 is rotatably sleeved on the outer wall of the reaction drive shaft 42, and one end of the inner positioning seat 221 is detachably connected to the inner wall of the dynamic reaction tube 21;

[0118] At least one set of inner limiting grooves 223, wherein the inner limiting grooves 223 are provided on the inner positioning seat 221;

[0119] It should be noted that the inner positioning seat 221 can be a round seat or annular structure with a hollow interior. The inner positioning seat 221 is rotatably connected to the reaction drive shaft 42 and the anti-blocking linkage seat 222 through an O-ring, and the inner positioning seat 221 is arranged on the outer wall of the reaction drive shaft 42 through a roller or a bearing sleeve. The inner positioning seat 221 is fixedly connected to the inner wall of the dynamic reaction tube 21 by snapping or plugging. The inner limit groove 223 can be an arc groove, a "U"-shaped groove or a "Y"-shaped groove structure. The inner limit grooves 223 are circumferentially arranged on the outer wall of the inner positioning seat 221, and the number of the inner limit grooves 223 can be 3-6 groups. The inner wall of the inner limit groove 223 is polished. The arrangement of the inner limit groove 223 and the inner positioning seat 221 can guide and limit the retractable spoiler 227 when it is flipped to adjust the opening angle, thereby ensuring the accuracy and efficiency of the opening angle adjustment of the retractable spoiler 227.

[0120] The anti-blocking linkage seat 222 is rotatably sleeved on the outer wall of the inner positioning seat 221, and the anti-blocking linkage seat 222 is fixedly connected to the outer wall of the reaction drive shaft 42;

[0121] In this embodiment, the anti-blocking linkage seat 222 may be a round seat or a circular ring structure with a hollow interior, and the anti-blocking linkage seat 222 is welded or riveted to the outer wall of the reaction drive shaft 42 .

[0122] At least one set of retractable spoilers 227, wherein the retractable spoilers 227 are fixedly mounted on the ends of the adjustable spoiler shafts 226, and one end of the adjustable spoiler shafts 226 away from the retractable spoilers 227 passes through the anti-blocking linkage seat 222 and is rotatably connected to the side wall of the anti-blocking linkage seat 222;

[0123] It should be noted that the number of retractable spoilers 227 and arc-shaped flip plates 225 is consistent with the number of inner limit grooves 223. The shape of the retractable spoiler 227 can be a spiral, curved, or fan-shaped plate structure. The retractable spoiler 227 and the arc-shaped flip plate 225 are riveted or welded.

[0124] At least one group of arc-shaped flip plates 225 are arranged between the inner positioning seat 221 and the anti-blocking linkage seat 222. One side of the arc-shaped flip plate 225 is fixedly connected to the adjustable spoiler shaft 226, and the other side of the arc-shaped flip plate 225 is fixedly connected with at least one group of inner hinge blocks 224, and the inner hinge blocks 224 are slidably embedded in the inner limit groove 223.

[0125] In this embodiment, the reaction drive shaft 42 is rotatably connected to the side wall of the anti-blocking linkage seat 222 via a sealed bearing or a bearing ring, and each set of the arc-shaped flip plates 225 is correspondingly installed with two sets of inner hinge blocks 224.

[0126] In the embodiment of the present invention, an anti-blocking protection part 22 is provided, and the anti-blocking protection part 22 is composed of an inner positioning seat 221, an anti-blocking linkage seat 222, and a retractable spoiler 227. The inner positioning seat 221, the anti-blocking linkage seat 222, and the retractable spoiler 227 cooperate with each other to automatically flip and adjust the position and angle of the retractable spoiler 227 during the nitration reaction, thereby disturbing the flow of raw materials while avoiding the blockage or adsorption of intermediates during discharge. Compared with the prior art, the disturbance effect is better, and at the same time, the disturbance range can be automatically expanded when the water hammer effect occurs in the flow of raw materials, thereby protecting the reaction feed port 212 and the reaction discharge port 213 to avoid leakage of the reaction feed port 212 and the reaction discharge port 213.

[0127] After 7-fluoro-2H-1,4-benzoxazine-3(4H)-one, nitric acid and dichloromethane are injected into the reaction feed port 212 through the metering feeding pipe 211, the driving motor 41 is turned on, and the driving motor 41 starts to drive the reaction driving shaft 42 to rotate, and the reaction driving shaft 42 rotates to drive the stirring mounting seat 231, the nitration stirring rod 232, and the nitration hammer ball 233 to stir and mix the raw materials for nitration reaction;

[0128] The rotation of the reaction drive shaft 42 can also drive the anti-blocking linkage seat 222 to rotate. The rotation of the anti-blocking linkage seat 222 drives the retractable spoiler 227 to disturb the raw material fluid. At the same time, the inner positioning seat 221 and the inner limit groove 223 limit the inner hinge block 224, so that the inner hinge block 224 drives the arc-shaped flip plate 225, the adjustable spoiler shaft 226 and the retractable spoiler 227 to rotate, thereby enhancing the spoiler effect.

[0129] In a further preferred embodiment of the present invention, Figure 1-2 As shown, the embodiment of the present invention also includes:

[0130] An auxiliary cooling component 5, the auxiliary cooling component 5 is sleeved on the dynamic reaction tube 21, and the auxiliary cooling component 5 is used to assist in cooling the raw materials in the dynamic reaction chamber 214;

[0131] At least one set of anti-leakage components 3, which are installed in the reaction feed port 212 and the reaction discharge port 213, and are used to prevent leakage from the reaction feed port 212 and the reaction discharge port 213, and eliminate the water hammer effect caused by the flow of liquid raw materials in the dynamic reaction chamber 214.

[0132] In this embodiment, the setting of the auxiliary cooling component 5 ensures the cooling temperature required for the nitration reaction, thereby avoiding the problem of low efficiency in intermediate preparation due to overheating, and the anti-leakage component 3 can cooperate with the anti-blocking protection part 22 to avoid leakage from the reaction feed port 212 and the reaction discharge port 213 while effectively eliminating the water hammer effect caused by the flow of liquid raw materials in the dynamic reaction chamber 214.

[0133] In a further preferred embodiment of the present invention, Figure 1-Figure 2 As shown, the reaction drive mechanism 4 also includes:

[0134] A cooling adjustment part 43, wherein the cooling adjustment part 43 is arranged on the equipment base 1, and the cooling adjustment part 43 is used to adjust the position of the auxiliary cooling component 5;

[0135] The cooling and regulating unit 43 includes:

[0136] A cooling adjustment shaft 431, wherein the cooling adjustment shaft 431 is rotatably mounted on the equipment base 1;

[0137] An adjusting threaded sleeve 432 threadably sleeved on the outer wall of the cooling adjusting shaft 431, the adjusting threaded sleeve 432 being connected to the auxiliary cooling assembly 5;

[0138] It should be noted that one end of the cooling adjustment shaft 431 is rotatably connected to the device base 1 via a bearing or a roller. The cooling adjustment shaft 431 can be a threaded rod or a ball screw, and the adjusting threaded sleeve 432 is slidably connected to the device base 1.

[0139] The intermittent driving part 44 is connected to the reaction driving shaft 42 . The intermittent driving part 44 is installed on the equipment base 1 . The intermittent driving part 44 is used for intermittent linkage driving the cooling adjustment shaft 431 .

[0140] In this embodiment, the auxiliary cooling component 5 includes:

[0141] A component support seat 51, wherein the component support seat 51 is slidably mounted in the device base 1, and one side of the component support seat 51 is detachably connected to the side wall of the adjusting threaded sleeve 432;

[0142] A medium guide pipe 52 is fixedly mounted on the component support seat 51 and is used to guide the cooling medium. A medium injection port 53 is provided at one end of the medium guide pipe 52 and a medium return port 54 is provided at the other end.

[0143] It should be noted that the component support seat 51 can be a round seat or a circular ring with a hollow interior. The component support seat 51 is detachably connected to the adjusting threaded sleeve 432 by means of a snap or a fastening bolt, and the medium guide pipe 52 can be a hard spiral tube structure. The medium guide pipe 52 is fixedly installed on the component support seat 51 by snap connection or riveting. The medium injection port 53 and the medium return port 54 are respectively connected to the medium circulation tank, and the cooling medium can be condensed water, glycerin or other fluid media that are easy to conduct heat. At the same time, in order to enhance the thermal insulation effect, the outside of the medium guide pipe 52 can be provided with an insulation cover.

[0144] In a further preferred embodiment of the present invention, Figure 10-11 As shown, the intermittent driving unit 44 includes:

[0145] A first gear 441, which is rotatably mounted on the device base 1, and is fixedly connected to the outer wall of the reaction drive shaft 42, and the first gear 441 is fixedly connected to the outer wall of the reaction drive shaft 42 by plugging or riveting;

[0146] A second gear 442 is disposed on one side of the first gear 441, the second gear 442 is rotatably connected to the device base 1, and the second gear 442 and the first gear 441 are meshed for transmission, and a limiting groove 443 is provided on a side wall of the second gear 442;

[0147] It should be noted that the inner side of the second gear 442 is rotatably connected to the equipment base 1 through a bearing or a roller, and a limiting groove 443 is provided on the outer side of the second gear 442. At least one group of protrusions is arranged in the limiting groove 443. The purpose of the protrusions is to drive the swing link 444, thereby indirectly and intermittently driving the cooling adjustment part 43.

[0148] A swing link 444, wherein the swing link 444 is rotatably mounted on the device base 1, one end of the swing link 444 is slidably connected to the limit groove 443, and the other end of the swing link 444 is hinged to the limit connection seat 446, the middle part of the swing link 444 is rotatably connected to the side wall of the device base 1 through a bearing or a rotating shaft, one end of the swing link 444 close to the limit groove 443 is slidably connected to the limit groove 443 through a hinge block, and the other end of the swing link 444 is hinged to the limit connection seat 446, and the limit connection seat 446 can be a rectangular seat or a "T"-shaped seat;

[0149] A rack limit seat 447 fixedly connected to the limit connection seat 446, wherein the gear limit seat is fixedly connected to the rack limit seat 447 by fastening bolts or welding, and the rack limit seat 447 may be a rectangular seat or a "T"-shaped seat with a hollow interior;

[0150] A swing rack 445, wherein the swing rack 445 is slidably mounted in the rack stop seat 447, wherein one end of the swing rack 445 is hinged to the side wall of the second gear 442, and the other end of the swing rack 445 is meshedly connected to the third gear 448, and the side wall of the third gear 448 is fixedly connected to the end of the cooling adjustment shaft 431;

[0151] The upper wall of the swing rack 445 is slidably connected to the rack limit seat 447, the swing rack 445 is hinged to the eccentric position of the side wall of the second gear 442, and the third gear 448 is rotatably connected to the equipment base 1 through a bearing or a roller, and the side wall of the third gear 448 is riveted or welded to the cooling adjustment shaft 431.

[0152] The lifting locking seat 449 is slidably installed on the equipment base 1, the upper end of the lifting locking seat 449 is rotationally connected to the end of the swing link 444, and the lower end of the lifting locking seat 449 is fixedly installed with a gear locking tooth 450, which is used to lock the third gear 448.

[0153] In this embodiment, the lifting locking seat 449 can be a rectangular seat or a rectangular frame with a hollow interior. The lifting locking seat 449 is slidably connected to the equipment base 1 through a slide groove or a slide rail. The lifting locking seat 449 and the gear locking tooth 450 are riveted or welded, and the gear locking tooth 450 and the third gear 448 are meshed for transmission.

[0154] In the embodiment of the present invention, an intermittent driving part 44 is provided, and the intermittent driving part 44 is composed of a first gear 441, a second gear 442, a third gear 448, a swing link 444, a swing rack 445 and a lifting locking seat 449. The first gear 441, the second gear 442, the third gear 448, the swing link 444, and the swing rack 445 cooperate with each other to intermittently drive the third gear 448 and the cooling adjustment shaft 431 to rotate when the reaction drive shaft 42 rotates, thereby achieving the purpose of flexibly adjusting the position of the auxiliary cooling component 5, which can not only ensure the cooling efficiency of the auxiliary cooling component 5, but also reduce the energy consumption generated by cooling.

[0155] During operation, the reaction drive shaft 42 can drive the first gear 441 to rotate by forward and reverse rotation, and the rotation of the first gear 441 drives the second gear 442 to rotate, and the rotation of the second gear 442 can drive the limiting groove 443 to rotate, and the limiting groove 443 drives the swing connecting rod 444 to swing, and the swing connecting rod 444 drives the limiting connecting seat 446 and the rack limiting seat 447 to guide and limit the swing rack 445, and at the same time, the rotation of the second gear 442 drives the swing rack 445 to swing, and the end of the swing rack 445 away from the second gear 442 intermittently engages with the third gear 448, so that the third gear 448 drives the cooling adjustment shaft 431 to rotate, and the rotation of the cooling adjustment shaft 431 drives the adjusting threaded sleeve 432 and the component supporting seat 51 to reciprocate along the equipment base 1, thereby realizing the adjustment of the cooling position of the medium guide tube 52, and by controlling the feed amount and the circulation amount of the cooling medium of the dynamic reaction tube 21, the reaction temperature of the dynamic reaction tube 21 is kept below 10°C.

[0156] In a further preferred embodiment of the present invention, Figure 12-Figure 15 As shown, the anti-leakage component 3 includes:

[0157] The anti-leakage seat 34 is fixedly mounted on the side wall of the dynamic reaction tube 21, and the bottom of the anti-leakage seat 34 is fixedly connected to a slow-flow protection seat 31, and at least one set of fluid delay plates 32 is arranged in the slow-flow protection seat 31;

[0158] The slow-flow protection seat 31 can be an hourglass-shaped structure, so as to prevent the fluid from stopping feeding and entering the anti-leakage seat 34, which has the effect of slowing down the flow and preventing overflow of the fluid. The fluid delay plate 32 is arranged in the slow-flow protection seat 31 in a counterclockwise circumferential direction, and the shape of the fluid delay plate 32 can be a rectangular, arc-shaped or fan-shaped structure.

[0159] An anti-impact linkage part 33, the anti-impact linkage part 33 is arranged in the anti-leakage seat 34;

[0160] The gas filter box 35 is detachably mounted on the top of the anti-leakage seat 34 , and the gas filter box 35 is used to filter the gas released by the anti-leakage seat 34 .

[0161] It should be noted that the anti-leakage seat 34 can be a circular seat or a rectangular seat with a hollow interior. The anti-leakage seat 34 is fixedly installed on the top of the side wall of the dynamic reaction tube 21 by means of a sealing flange and welding, and the anti-leakage seat 34 and the slow-flow protection seat 31 are fixedly connected by a snap. A gas filter box 35 is arranged on the top of the anti-leakage seat 34, so that when the fluid produces a water hammer effect to impact the anti-leakage seat 34 to discharge the gas, the gas can be filtered to prevent the discharged gas from polluting the external environment. The gas filter box 35 can be an activated carbon or organic vapor filter box. The gas filter box 35 is also connected to a one-way check solenoid valve to ensure the sealing of the dynamic reaction chamber 214 during normal reaction.

[0162] In this embodiment, the anti-shock linkage part 33 includes:

[0163] An anti-impact swing seat 331, wherein the anti-impact swing seat 331 is movably arranged in the anti-leakage seat 34, and a linkage guide rod 333 is hinged on the upper part of the anti-impact swing seat 331 through a universal ball, and the linkage guide rod 333 is fixedly installed in the anti-leakage seat 34;

[0164] It should be noted that the anti-impact swing seat 331 can be a conical plate, a frustum plate or a circular plate structure. In order to facilitate the passage of gas, the outer wall of the anti-impact swing seat 331 is circumferentially provided with multiple groups of swing flow grooves 332, and the swing flow grooves 332 can be arc grooves, circular grooves or rectangular groove structures.

[0165] A reciprocating piston plate 335 slidably disposed in the anti-leakage seat 34, the reciprocating piston plate 335 is also slidably sleeved on the outside of the linkage guide rod 333, and a double-sided gear seat 336 is fixedly disposed on the reciprocating piston plate 335;

[0166] In this embodiment, the double-sided tooth seat 336 is fixedly installed on the reciprocating piston plate 335 by means of bolts or snaps. Two groups of longitudinal racks are symmetrically arranged on the double-sided tooth seat 336. The double-sided tooth seat 336 is slidingly connected to the linkage guide rod 333 through a sliding groove or a sliding rail. The setting of the linkage guide rod 333 realizes the guiding and limiting of the anti-impact swing seat 331 and the reciprocating piston plate 335.

[0167] At least one group of anti-impact linkage rods 334, one end of the anti-impact linkage rod 334 is hinged to the anti-impact swing seat 331, and the other end is fixedly installed with a lifting tooth 337, the lifting tooth 337 is meshed with the double-sided tooth seat 336 for transmission, the lifting teeth 337 are arranged on both sides of the double-sided tooth seat 336, and can be staggered up and down, thereby ensuring that the two groups of the lifting teeth 337 alternately lift or press down the double-sided tooth seat 336.

[0168] It should be noted that the anti-impact linkage rod 334 can be divided into two groups, and the middle part of the anti-impact linkage rod 334 is slidably connected to the reciprocating piston plate 335. When the water hammer effect occurs, the fluid impacts the anti-impact swing seat 331, thereby causing the anti-impact swing seat 331 to swing. When the anti-impact swing seat 331 swings, it can drive the anti-impact linkage rod 334 to swing alternately. The anti-impact linkage rod 334 drives the lifting teeth 337 to move alternately, so that the lifting teeth 337 alternately lifts or presses down the double-sided tooth seat 336, thereby effectively eliminating the fluid water hammer effect.

[0169] On the other hand, an embodiment of the present invention further provides a process for preparing fluazifop-butyl, wherein the process for preparing fluazifop-butyl specifically comprises:

[0170] Step S10, alkaline hydrolysis and acidification reaction, using 2,4-difluoronitrobenzene as a starting material, 2,4-difluoronitrobenzene is subjected to alkaline hydrolysis reaction to obtain an intermediate 5-fluoro-2-nitrophenol.

[0171] Step S20, etherification reaction, add a certain amount of DMF to the etherification kettle, start stirring, open the manhole, put potassium carbonate and potassium iodide into the etherification kettle, slowly drop a solution containing the intermediate 5-fluoro-2-nitrophenol and DMF at room temperature under nitrogen protection, then drop methyl chloroacetate, keep warm and react for 4 hours after the addition, take samples and detect until the alkaline hydrolyzate is less than 0.5%, cool to room temperature, centrifuge, wash the filter cake with DMF, maintain the vacuum degree of the filtrate above -0.096Mpa, perform reduced pressure distillation, add distilled water to precipitate solids, centrifuge, wash the filter cake with water, and dry to obtain an etherified product, which is the intermediate 5-fluoro-2-nitrophenoxyacetic acid methyl ester.

[0172] Among them, the main reaction of etherification reaction is:

[0173]

[0174] Table 1 shows the main reaction raw material parameters of etherification reaction:

[0175] Table 1

[0176] name 5-Fluoro-2-nitrophenol Methyl chloroacetate Potassium carbonate 5-Fluoro-2-nitrophenoxyacetic acid methyl ester Potassium chloride Potassium bicarbonate Molecular formula C6H4FNO3 C3H5ClO2 K2CO3 C9H8FNO5 KCl KHCO3 Molecular weight 157.1 108.52 138.21 229.16 74.55 100.12 Input amount / t / a 905.77 619.36 788.81 content 98％ 99％ 99％ 100％ 100％ 100％ Reaction volume / t / a 883.12 603.87 769.09 Production volume / t / a 1262.44 410.69 551.56 Remaining amount / t / a 22.64 15.48 19.72

[0177] In this embodiment, during the etherification reaction, the conversion rate of 5-fluoro-2-nitrophenol was 97.5%, and the intermediate 5-fluoro-2-nitrophenoxyacetic acid methyl ester (content 98%) was obtained.

[0178] The side reactions of the etherification reaction are:

[0179]

[0180] Table 2 shows the parameters of the etherification reaction side reaction raw materials:

[0181] Table 2

[0182] name 3-Fluoro-4-nitrophenol Methyl chloroacetate Potassium carbonate Methyl 3-fluoro-4-nitrophenoxyacetate Potassium chloride Potassium bicarbonate Molecular formula C6H4FNO3 C3H5ClO2 K2CO3 C9H8FNO5 KCl KHCO3 Molecular weight 157.1 108.52 138.21 229.16 74.55 100.12 Input amount / t / a 18.12 12.64 16.10 content 100％ 99％ 99％ 100％ 100％ 100％ Reaction volume / t / a 17.66 12.32 15.70 Production volume / t / a 25.76 8.38 11.26 Remaining amount / t / a 0.45 0.32 0.40

[0183] Step S30, a reduction reaction, DMF, intermediate 5-fluoro-2-nitrophenoxyacetic acid methyl ester and Raney nickel (10% added each time) are added to the reduction kettle in sequence, the manhole is closed, and 10Kg / cm 2 Nitrogen was flushed and discharged 3 times, and then filled with hydrogen, maintaining the pressure at 7Kg / cm 2 , stir the reduction kettle, heat the reduction kettle to 60℃, and keep the reaction at 60-70℃, maintaining the hydrogen pressure at 7Kg / cm 2 , repeatedly fill with hydrogen until the pressure stops dropping, keep warm for 2 hours, and the reaction is complete;

[0184] The reduction kettle is then cooled to 40-45°C, depressurized, allowed to stand for 30 minutes, and filled with nitrogen. The reaction solution is pressed into the distillation kettle through a bottom tube and a pipeline filter to transfer the material to prevent the low-temperature product from precipitating and clogging the pipeline. After the material transfer is completed, the vacuum (-0.095Mpa) on the distillation kettle is turned on and stirred. The temperature is slowly increased and the pressure is reduced to recover the solvent DMF. After the solvent is recovered, the temperature is lowered, a certain amount of water is added to the residue, centrifuged, and dried at 80°C to obtain a reduced product, which is the intermediate 7-fluoro-2H-1,4-benzoxazine-3(4H)-one.

[0185] In step S30, the conversion rate of 5-fluoro-2-nitrophenoxyacetic acid methyl ester is 97%, and the intermediate 7-fluoro-2H-1,4-benzoxazin-3(4H)-one (content 98%) is obtained.

[0186] The main reaction of a reduction reaction is:

[0187]

[0188] Table 3 shows the main reaction raw material parameters of the primary reduction reaction:

[0189] Table 3

[0190] name 5-Fluoro-2-nitrophenoxyacetic acid methyl ester hydrogen 7-Fluoro-2H-1,4-benzoxazin-3(4H)-one Methanol water Molecular formula C9H8FNO5 H2 C8H6FNO2 CH3OH H2O Molecular weight 229.16 2.02 167.14 32.04 18.02 Input amount / t / a 1288.20 33.72 content 98％ 99％ 100％ 100％ 100％ Reaction volume / t / a 1249.55 32.71 Production volume / t / a 893.15 171.21 192.59 Remaining amount / t / a 38.65 1.01

[0191] Step S40, nitration reaction, using the dynamic reaction tube 21 to carry out nitration reaction on the intermediate 7-fluoro-2H-1,4-benzoxazine-3(4H)-one to obtain the intermediate 7-fluoro-6-nitro-2H-1,4-benzoxazine-3(4H)-one.

[0192] Step S50, secondary reduction reaction, DMF, intermediate 7-fluoro-6-nitro-2H-1,4-benzoxazine-3(4H)-one and Raney nickel (10% added each time) are sequentially added into the nitro reduction kettle, the manhole is closed, and 10Kg / cm 2 Nitrogen was flushed and discharged 3 times, and hydrogen was filled in to maintain the pressure at 7Kg / cm 2 , stir thoroughly, heat to 60℃, and keep the temperature at 60-70℃ for reaction, maintaining the hydrogen pressure at 7Kg / cm 2 , repeatedly fill with hydrogen until the pressure stops dropping, keep warm and stir for 2 hours, and the reaction is complete.

[0193] The mixture was cooled to 40-45°C, depressurized, allowed to stand for 30 minutes, and filled with nitrogen. The reaction solution was pressed into the distillation kettle through the bottom tube and the pipeline filter to prevent the low-temperature product from precipitating and clogging the pipeline. After the material transfer was completed, the vacuum (-0.095Mpa) on the distillation kettle was turned on and stirred. The temperature was slowly increased and the pressure was reduced to recover the solvent DMF. After the solvent was recovered, the temperature was lowered, a certain amount of water was added to the residue, and the mixture was centrifuged. The filter cake was washed with water, centrifuged, and dried at 80°C to obtain the intermediate 7-fluoro-6-amino-2H-1,4-benzoxazine-3(4H)-one.

[0194] It should be noted that the conversion rate of 7-fluoro-6-nitro-2H-1,4-benzoxazine-3(4H)-one in the secondary reduction reaction was 96%, and the intermediate 7-fluoro-6-amino-2H-1,4-benzoxazine-3(4H)-one (content 98%) was obtained.

[0195] In this embodiment, the main reaction of the secondary reduction reaction is:

[0196]

[0197] Table 4 shows the main reaction raw material parameters of the secondary reduction reaction:

[0198] Table 4

[0199]

[0200]

[0201] Step S60, propynylation reaction, DMF is added to the propylation kettle, the propylation kettle is started to stir, the intermediate 7-fluoro-6-amino-2H-1,4-benzoxazine-3(4H)-one, catalyst and potassium hydroxide are added to the propylation kettle, and the propylation kettle is stirred for 0.5 hour after the addition is completed. The nitrogen valve is opened to replace the nitrogen, and the temperature is maintained. A certain amount of chloropropyne is added dropwise within 2 hours. After the dropwise addition is completed, the reaction is stirred and kept warm for 8 hours. Sampling is detected to detect that the nitro reduction product is less than 1.0%, the stirring of the water washing kettle is started, distilled water is added, and the frozen brine is turned on, and the reaction is cooled to 0-5°C and maintained at 0-5°C. The reaction liquid in the propylation kettle is slowly transferred to the water washing kettle. After the transfer is completed, the brine is pressed out, the temperature is naturally raised and stirred for 1 hour, centrifuged, the wet product is rinsed with water, and vacuum dried at 80°C to obtain the intermediate 7-fluoro-6-amino-4-(2-propargyl)2H-1,4-benzoxazine-3(4H)-one.

[0202] It should be noted that, in this embodiment, the conversion rate of 7-fluoro-6-amino-2H-1,4-benzoxazine-3(4H)-one is 95.5%, and the intermediate 7-fluoro-6-amino-4-(2-propargyl)2H-1,4-benzoxazine-3(4H)-one (content 93%) is obtained.

[0203] The main reaction of propynylation is:

[0204]

[0205] Table 5 shows the main reaction raw material parameters of propynylation reaction:

[0206] Table 5

[0207]

[0208] Step S70, condensation reaction, add acetic acid to the condensation kettle, start stirring the condensation kettle, open the manhole, add the intermediate 7-fluoro-6-amino-4-(2-propargyl)2H-1,4-benzoxazine-3(4H)-one and tetrahydrophthalic anhydride to the condensation kettle in sequence, heat the condensation kettle for reaction for 4 hours, take samples until the propyne compound is ≤1%, cool the condensation kettle to 50-60°C and keep it warm for 1 hour, cool it naturally and continue stirring for 2 hours, cool it to 20-25°C, stir it for 1 hour, centrifuge it, apply the filtrate three times, add new acetic acid to the calibrated high-level tank scale when the mother liquor is applied, add a certain amount of dichloroethane to the crystallization kettle, add the above filter cake to the crystallization kettle, heat it to reflux for 0.5 hours, cool it to room temperature for 4 hours, centrifuge it, apply the mother liquor, and vacuum dry the filter cake at 80°C to obtain the product fluazifop-propylamine.

[0209] In this example, the conversion rate of 7-fluoro-6-amino-4-(2-propargyl)2H-1,4-benzoxazin-3(4H)-one was 95%, and the product fluazifop (content 98%) was obtained.

[0210] In this embodiment, the main reaction of the condensation reaction is:

[0211]

[0212] Table 6 shows the main reaction raw material parameters of the condensation reaction:

[0213] Table 6

[0214]

[0215] It should be noted that the process reaction flow for preparing fluazifop-butyl is as follows:

[0216]

[0217] In an embodiment of the present invention, the method for alkaline hydrolysis of 2,4-difluoronitrobenzene specifically comprises:

[0218] Step S101, adding distilled water to the alkali preparation kettle, adding potassium hydroxide into the alkali preparation kettle while stirring, preparing a potassium hydroxide solution, cooling it to room temperature for use.

[0219] Step S102, 2,4-difluoronitrobenzene and distilled water are added to the alkaline hydrolysis kettle, the alkaline hydrolysis kettle is heated, and then potassium hydroxide solution is added dropwise to the alkaline hydrolysis kettle. After the addition is completed, the alkaline hydrolysis kettle is kept warm for 1 hour, sampling is performed until 2,4-difluoronitrobenzene is less than 0.5%, distilled water is added, and the material is transferred to the acidification kettle while it is hot.

[0220] Step S103, open the acidification kettle for circulating water cooling, keep the temperature while adding hydrochloric acid dropwise to a pH value of 2-3, let it stand for 0.5 hour, separate the lower organic phase and transfer it to a water washing kettle, transfer the upper water to a wastewater treatment kettle, add distilled water to the water washing kettle and stir for 0.5 hour, let it stand, separate the lower organic phase for high vacuum distillation, use the upper water jacket to the acidification kettle, and distill out the alkaline hydrolyzate under high vacuum. The alkaline hydrolyzate is the intermediate 5-fluoro-2-nitrophenol. Note that the temperature of the receiving port is not lower than 40°C to prevent solidification at the discharge port. Add a certain amount of DMF to dissolve the evaporated material.

[0221] In this embodiment, the main reaction of the alkaline hydrolysis reaction of 2,4-difluoronitrobenzene is:

[0222]

[0223] Table 7 shows the main reaction raw material parameters of alkaline hydrolysis reaction:

[0224] Table 7

[0225]

[0226]

[0227] On the other hand, an embodiment of the present invention further provides a method for performing a nitration reaction on an intermediate 7-fluoro-2H-1,4-benzoxazine-3(4H)-one using a dynamic reaction tube 21, wherein the nitration reaction on the intermediate 7-fluoro-2H-1,4-benzoxazine-3(4H)-one using a dynamic reaction tube 21 specifically comprises:

[0228] Step S201, check the dynamic reaction tube 21 and its ancillary equipment, confirm that they are dry and clean, and the valve is in a closed state, take dichloromethane, and transfer it to the dichloromethane metering tank through the dichloromethane intermediate tank for standby, and transfer sulfuric acid to the sulfuric acid metering tank through the sulfuric acid intermediate tank for standby, add concentrated sulfuric acid and 7-fluoro-2H-1,4-benzoxazine-3(4H)-one into the dissolving kettle, stir and dissolve, pass chilled water to cool to below 10°C, and then transfer to the dynamic reaction tube 21.

[0229] Step S202, when 7-fluoro-2H-1,4-benzoxazine-3(4H)-one, nitric acid and dichloromethane are injected into the reaction feed port 212 through the metering feeding pipe 211, the driving motor 41 is turned on, and the driving motor 41 starts to drive the reaction driving shaft 42 to rotate. The reaction driving shaft 42 rotates to drive the stirring mounting seat 231, the nitration stirring rod 232, and the nitration hammer ball 233 to stir and mix the raw materials for nitration reaction.

[0230] The nitration reaction is as follows:

[0231] The main reaction is as follows, and Table 8 shows the main reaction raw material parameters:

[0232]

[0233] Table 8

[0234] name 7-Fluoro-2H-1,4-benzoxazin-3(4H)-one Nitric acid 7-Fluoro-6-nitro-2H-1,4-benzoxazin-3(4H)-one water Molecular formula C8H7FN2O3 HNO3 C8H7FN2O3 H2O Molecular weight 167.14 63.01 212.13 18.02 Input amount / t / a 884.03 328.04 content 98％ 98％ 100％ 100％ Reaction volume / t / a 853.09 321.61 Production volume / t / a 1061.07 90.14 Remaining amount / t / a 30.94 6.43

[0235] Table 9 shows the side reaction raw material parameters:

[0236]

[0237] Table 9

[0238]

[0239] In step S203, the rotation of the reaction drive shaft 42 can also drive the anti-blocking linkage seat 222 to rotate. The rotation of the anti-blocking linkage seat 222 drives the retractable spoiler 227 to disturb the raw material fluid. At the same time, the inner positioning seat 221 and the inner limit groove 223 limit the inner hinge block 224, so that the inner hinge block 224 drives the arc-shaped flip plate 225, the adjustable spoiler shaft 226 and the retractable spoiler 227 to rotate, thereby enhancing the spoiler effect.

[0240] Step S204, the reaction drive shaft 42 can drive the first gear 441 to rotate by forward and reverse rotation, the first gear 441 drives the second gear 442 to rotate by rotation, the second gear 442 drives the limiting groove 443 to rotate, the limiting groove 443 drives the swing link 444 to swing, the swing link 444 drives the limiting connection seat 446 and the rack limiting seat 447 to guide and limit the swing rack 445, and at the same time, the second gear 442 drives the swing rack 445 to swing by rotation, and the end of the swing rack 445 away from the second gear 442 intermittently meshes with the third gear 448, so that the third gear 448 drives the cooling adjustment shaft 431 to rotate, and the cooling adjustment shaft 431 drives the adjusting threaded sleeve 432 and the component support seat 51 to reciprocate along the equipment base 1, thereby realizing the adjustment of the cooling position of the medium guide tube 52, and by controlling the feed amount and the circulation amount of the cooling medium of the dynamic reaction tube 21, the reaction temperature of the dynamic reaction tube 21 is kept below 10°C.

[0241] Step S205, the material discharged from the dynamic reaction tube 21 enters the nitration material buffer tank for sampling and analysis, and the reaction is determined to be complete when the raw material content is less than 0.5%.

[0242] In the embodiment of the present invention, it is ensured that the 7-fluoro-2H-1,4-benzoxazin-3(4H)-one in the reaction liquid at the outlet of the dynamic tubular reactor is less than 0.5%.

[0243] Step S206, the reaction liquid in the nitration material buffer tank overflows into the oleic acid separation tank for separation, the upper organic phase overflows into the dichloromethane removal intermediate tank, and then goes to the dichloromethane recovery kettle to recover dichloromethane; the lower acid phase flows into the hydrolysis kettle, the material is centrifuged, the filter cake is slurried once with water and sodium bicarbonate, the pH is adjusted to 7-9, stirred for 30 minutes, and dried at 80°C to obtain the intermediate 7-fluoro-6-nitro-2H-1,4-benzoxazine-3(4H)-one (content 97%).

[0244] In summary, the present invention provides a dynamic tubular reactor and process for preparing fluazifop-butyl. In the embodiment of the present invention, an anti-blocking protection part 22 and a reaction driving mechanism 4 are provided. The technical means of the coordinated cooperation between the reaction driving mechanism 4 and the anti-blocking protection part 22 can break the dynamic balance of the fluid in the nitration reaction, thereby improving the nitration preparation efficiency of the fluazifop-butyl intermediate, and avoiding leakage of the reaction feed port 212 and the reaction discharge port 213. The anti-blocking protection part 22 can also be automatically retracted and released after the reaction, thereby facilitating the discharge of the fluazifop-butyl intermediate and avoiding blockage.

[0245] It should be noted that, for the above-mentioned embodiments, for the sake of simplicity, they are all described as a series of action combinations, but those skilled in the art should know that the present invention is not limited by the described order of actions, because according to the present invention, some steps may be performed in other orders or simultaneously. Secondly, those skilled in the art should also know that the embodiments described in the specification are all preferred embodiments, and the actions and modules involved are not necessarily required by the present invention.

Claims

1. A dynamic tubular reactor for preparing fluazifop-butyl, the dynamic tubular reactor for preparing fluazifop-butyl comprising: Equipment base; A dynamic reaction mechanism fixedly mounted on a base of the device; A reaction drive mechanism, the reaction drive mechanism is arranged on the device base, and the reaction drive mechanism is used to drive the dynamic reaction mechanism; It is characterized in that the dynamic reaction mechanism comprises: A dynamic reaction tube, wherein a dynamic reaction chamber is provided in the dynamic reaction tube, a reaction feed port and a reaction discharge port are respectively provided on both sides of the dynamic reaction chamber, a metering feeding pipe is fixedly installed at one end of the reaction feed port, and the metering feeding pipe is used to inject the reaction raw materials for preparing fluazifop-butyl into the reaction feed port; At least one group of anti-blocking protection parts, the anti-blocking protection parts are arranged in the reaction feed port and the reaction discharge port, and the anti-blocking protection parts are used to protect the reaction feed port and the reaction discharge port and prevent leakage of the reaction feed port and the reaction discharge port; At least one nitration stirring section, wherein the nitration stirring section is arranged in the dynamic reaction chamber and is used for stirring and mixing the reaction raw materials for preparing fluazifop-butyl; Wherein, the reaction drive mechanism comprises: A driving motor, wherein the driving motor is fixedly mounted on the device base; A reaction drive shaft is fixedly connected to the output end of the drive motor, and one end of the reaction drive shaft away from the drive motor passes through the equipment base and the side wall of the dynamic reaction tube, extends into the dynamic reaction chamber, and is respectively connected to the anti-blocking protection part and the nitrification stirring part.

2. The dynamic tubular reactor for preparing fluazifop-butyl according to claim 1, characterized in that: The nitrification stirring unit comprises: A stirring mounting seat, the stirring mounting seat is fixedly mounted on the outer wall of the reaction drive shaft; at least one set of nitrification stirring rods, wherein the outer wall of the nitrification stirring rods is provided with a flow disturbance auger, and A nitration hammer ball detachably mounted on the end of the nitration stirring rod.

3. The dynamic tubular reactor for preparing fluazifop-butyl according to claim 1, characterized in that: The anti-blocking protection part comprises: An inner positioning seat, the inner positioning seat is rotatably sleeved on the outer wall of the reaction drive shaft, and one end of the inner positioning seat is detachably connected to the inner wall of the dynamic reaction tube; At least one set of inner limiting grooves, wherein the inner limiting grooves are arranged on the inner positioning seat; An anti-blocking linkage seat is rotatably sleeved on the outer wall of the inner positioning seat, and the anti-blocking linkage seat is fixedly connected to the outer wall of the reaction drive shaft; At least one set of retractable spoilers, wherein the retractable spoilers are fixedly mounted on the ends of the adjustable spoiler shafts, and one end of the adjustable spoiler shaft away from the retractable spoilers penetrates the anti-blocking linkage seat and is rotatably connected to the side wall of the anti-blocking linkage seat; At least one group of arc-shaped flip plates is arranged between the inner positioning seat and the anti-blocking linkage seat, one side of the arc-shaped flip plate is fixedly connected to the adjustable spoiler shaft, and the other side of the arc-shaped flip plate is fixedly connected to at least one group of inner hinge blocks, and the inner hinge blocks are slidably embedded in the inner limit grooves.

4. The dynamic tubular reactor for preparing fluazifop-butyl as claimed in claim 3, characterized in that: Also includes: An auxiliary cooling component, which is sleeved on the dynamic reaction tube and is used to assist in cooling the raw materials in the dynamic reaction chamber; At least one set of anti-leakage components, which are installed in the reaction feed port and the reaction discharge port, and are used to prevent leakage from the reaction feed port and the reaction discharge port, and eliminate the water hammer effect caused by the flow of liquid raw materials in the dynamic reaction chamber.

5. The dynamic tubular reactor for preparing fluazifop-butyl as claimed in claim 4, characterized in that: The reaction drive mechanism also includes: A cooling adjustment unit, the cooling adjustment unit is arranged on the equipment base, and the cooling adjustment unit is used to adjust the position of the auxiliary cooling assembly; The cooling and regulating unit includes: A cooling adjustment shaft, wherein the cooling adjustment shaft is rotatably mounted on the equipment base; An adjusting threaded sleeve is threadedly sleeved on the outer wall of the cooling adjusting shaft, and the adjusting threaded sleeve is connected to the auxiliary cooling assembly; An intermittent drive unit, the intermittent drive unit is connected to the reaction drive shaft, the intermittent drive unit is installed on the equipment base, and the intermittent drive unit is used to intermittently drive the cooling adjustment shaft; The anti-leakage component comprises: An anti-leakage seat, wherein the anti-leakage seat is fixedly mounted on the side wall of the dynamic reaction tube, and a slow-flow protection seat is fixedly connected to the bottom of the anti-leakage seat, and at least one group of fluid delay plates is arranged in the slow-flow protection seat; An anti-impact linkage part, which is arranged in the anti-leakage seat; A gas filter box detachably mounted on the top of the anti-leakage seat, the gas filter box being used to filter the gas released by the anti-leakage seat; The anti-shock linkage unit comprises: An anti-impact swing seat, wherein the anti-impact swing seat is movably arranged in the anti-leakage seat, and the upper part of the anti-impact swing seat is hinged with a linkage guide rod through a universal ball, and the linkage guide rod is fixedly installed in the anti-leakage seat; A reciprocating piston plate is slidably arranged in the anti-leakage seat, and the reciprocating piston plate is also slidably sleeved on the outside of the linkage guide rod, and a double-sided gear seat is fixedly arranged on the reciprocating piston plate; At least one group of anti-impact linkage rods, one end of which is hinged to the anti-impact swing seat, and the other end is fixedly mounted with lifting teeth, which mesh with the double-sided tooth seat for transmission.

6. The dynamic tubular reactor for preparing fluazifop-butyl as claimed in claim 5, characterized in that: The auxiliary cooling assembly comprises: A component support seat, wherein the component support seat is slidably mounted in the equipment base, and one side of the component support seat is detachably connected to the side wall of the adjusting threaded sleeve; A medium guide pipe is fixedly mounted on the component support seat, and is used to guide the cooling medium. One end of the medium guide pipe is provided with a medium injection port, and the other end is provided with a medium return port.

7. The dynamic tubular reactor for preparing fluazifop-butyl as claimed in claim 5, characterized in that: The intermittent driving unit comprises: A first gear, the first gear is rotatably mounted on the device base, and the first gear is fixedly connected to the outer wall of the reaction drive shaft; A second gear is arranged on one side of the first gear, the second gear is rotatably connected to the device base, and the second gear is meshed with the first gear for transmission, and a limiting groove is provided on a side wall of the second gear; A swing link, wherein the swing link is rotatably mounted on the equipment base, one end of the swing link is slidably connected to the limit groove, and the other end of the swing link is hinged to the limit connection seat; A rack limit seat fixedly connected to the limit connecting seat; A swing rack, wherein the swing rack is slidably mounted in the rack limit seat, one end of the swing rack is hinged to the side wall of the second gear, the other end of the swing rack is meshedly connected to the third gear, and the side wall of the third gear is fixedly connected to the end of the cooling adjustment shaft; A lifting locking seat is slidably installed on the equipment base, the upper end of the lifting locking seat is rotationally connected to the end of the swing connecting rod, and the lower end of the lifting locking seat is fixedly installed with a gear locking tooth, which is used to lock the third gear.

8. A process for preparing fluazifop-butyl, implemented by using the dynamic tubular reactor for preparing fluazifop-butyl as claimed in any one of claims 1 to 7, characterized in that: It includes: Step S10, alkaline hydrolysis and acidification reaction, using 2,4-difluoronitrobenzene as a starting material, 2,4-difluoronitrobenzene is subjected to alkaline hydrolysis reaction to obtain an intermediate 5-fluoro-2-nitrophenol; Step S20, etherification reaction, adding a certain amount of DMF to the etherification kettle, starting stirring, opening the manhole, adding potassium carbonate and potassium iodide into the etherification kettle, slowly dropping a solution containing the intermediate 5-fluoro-2-nitrophenol and DMF at room temperature under nitrogen protection, and then dropping methyl chloroacetate, keeping the temperature for 4 hours after the addition, sampling and testing until the alkaline hydrolyzate is less than 0.5%, cooling to room temperature, centrifuging, and drying to obtain an etherified product, which is the intermediate 5-fluoro-2-nitrophenoxyacetic acid methyl ester; Step S30, a reduction reaction, DMF, intermediate 5-fluoro-2-nitrophenoxyacetic acid methyl ester and Raney nickel (10% added each time) are added to the reduction kettle in sequence, the manhole is closed, and 10Kg / cm 2 Nitrogen was flushed and discharged 3 times, and then filled with hydrogen, maintaining the pressure at 7Kg / cm 2 , stir the reduction kettle, heat the reduction kettle to 60℃, and keep the reaction at 60-70℃, maintaining the hydrogen pressure at 7Kg / cm 2 , repeatedly filling with hydrogen until the pressure no longer decreases, keeping warm for 2 hours, the reaction is completed, and a reduced product is obtained, which is the intermediate 7-fluoro-2H-1,4-benzoxazine-3(4H)-one; Step S40, nitration reaction, using a dynamic reaction tube to nitrate the intermediate 7-fluoro-2H-1,4-benzoxazine-3(4H)-one to obtain the intermediate 7-fluoro-6-nitro-2H-1,4-benzoxazine-3(4H)-one; Step S50, secondary reduction reaction, DMF, intermediate 7-fluoro-6-nitro-2H-1,4-benzoxazine-3(4H)-one and Raney nickel (10% added each time) are sequentially added into the nitro reduction kettle, the manhole is closed, and 10Kg / cm 2 Nitrogen was flushed and discharged 3 times, and hydrogen was filled in to maintain the pressure at 7Kg / cm 2 , stir thoroughly, heat to 60℃, and keep the temperature at 60-70℃ to react, maintaining the hydrogen pressure at 7Kg / cm 2 , repeatedly filling with hydrogen until the pressure no longer drops, keeping warm and stirring for 2 hours, the reaction is completed, and the intermediate 7-fluoro-6-amino-2H-1,4-benzoxazin-3(4H)-one is obtained; Step S60, propynylation reaction, DMF is added to the propylation kettle, the propylation kettle is stirred, the intermediate 7-fluoro-6-amino-2H-1,4-benzoxazine-3(4H)-one, catalyst and potassium hydroxide are added to the propylation kettle, and the propylation kettle is stirred for 0.5 hour after the addition is completed. The nitrogen valve is opened to replace the nitrogen, and the temperature is maintained. A certain amount of chloropropyne is added dropwise within 2 hours. After the addition is completed, the reaction is stirred and kept warm for 8 hours. Sampling is performed to detect that the nitro reduction product is less than 1.0%, stirring of the water washing kettle is turned on, distilled water is added, and frozen brine is turned on, and the reaction is cooled to 0-5°C and maintained at 0-5°C. The reaction liquid in the propylation kettle is slowly transferred to the water washing kettle. After the transfer is completed, the brine is pressed out, the temperature is naturally raised and stirred for 1 hour, and the centrifugation is performed. The wet product is rinsed with water and vacuum dried at 80°C to obtain the intermediate 7-fluoro-6-amino-4-(2-propargyl)2H-1,4-benzoxazine-3(4H)-one; Step S70, condensation reaction, add acetic acid to the condensation kettle, start stirring the condensation kettle, open the manhole, add the intermediate 7-fluoro-6-amino-4-(2-propargyl)2H-1,4-benzoxazine-3(4H)-one and tetrahydrophthalic anhydride to the condensation kettle in sequence, heat the condensation kettle for reaction for 4 hours, take samples until the propyne compound is ≤1%, cool the condensation kettle to 50-60°C and keep it warm for 1 hour, cool it naturally and continue stirring for 2 hours, cool it to 20-25°C, stir it for 1 hour, centrifuge it, apply the filtrate three times, add new acetic acid to the calibrated high-level tank scale when the mother liquor is applied, add a certain amount of dichloroethane to the crystallization kettle, add the above filter cake to the crystallization kettle, heat it to reflux for 0.5 hours, cool it to room temperature for 4 hours, centrifuge it, apply the mother liquor, and vacuum dry the filter cake at 80°C to obtain the product fluazifop-propylamine.

9. The process for preparing fluazifop-butyl as claimed in claim 8, characterized in that: The method for alkaline hydrolysis of 2,4-difluoronitrobenzene specifically comprises: Step S101, adding distilled water to the alkali preparation kettle, adding potassium hydroxide into the alkali preparation kettle while stirring, preparing a potassium hydroxide solution and cooling it to room temperature for use; Step S102, adding 2,4-difluoronitrobenzene and distilled water into the alkaline hydrolysis kettle, heating the alkaline hydrolysis kettle, and then dropping potassium hydroxide solution into the alkaline hydrolysis kettle. After the dropping is completed, the alkaline hydrolysis kettle is kept warm for 1 hour, sampling is performed until 2,4-difluoronitrobenzene is less than 0.5%, distilled water is added, and the material is transferred to the acidification kettle while it is hot; Step S103, open the acidification kettle for circulating water cooling, keep the temperature while adding hydrochloric acid dropwise to a pH value of 2-3, let it stand for 0.5 hour, separate the lower organic phase and transfer it to a water washing kettle, transfer the upper water to a wastewater treatment kettle, add distilled water to the water washing kettle and stir for 0.5 hour, let it stand, separate the lower organic phase for high vacuum distillation, use the upper water jacket to the acidification kettle, and distill out the alkaline hydrolyzate under high vacuum. The alkaline hydrolyzate is the intermediate 5-fluoro-2-nitrophenol. Note that the temperature of the receiving port is not lower than 40°C to prevent solidification at the discharge port. Add a certain amount of DMF to dissolve the evaporated material.

10. The process for preparing fluazifop-butyl as claimed in claim 8, characterized in that: A method for nitrating an intermediate 7-fluoro-2H-1,4-benzoxazine-3(4H)-one using a dynamic reaction tube specifically comprises: Step S201, check the dynamic reaction tube and its ancillary equipment to confirm that they are dry and clean, and the valve is in a closed state, take dichloromethane, and transfer it to the dichloromethane metering tank through the dichloromethane intermediate tank for standby, and transfer sulfuric acid to the sulfuric acid metering tank through the sulfuric acid intermediate tank for standby, add concentrated sulfuric acid and 7-fluoro-2H-1,4-benzoxazine-3(4H)-one to the dissolving kettle, stir and dissolve, pass chilled water to cool to below 10°C, and then transfer to the dynamic reaction tube; Step S202, after 7-fluoro-2H-1,4-benzoxazine-3(4H)-one, nitric acid, and dichloromethane are injected into the reaction feed port through the metering feeding pipe, the driving motor is turned on, the driving motor starts to drive the reaction driving shaft to rotate, and the reaction driving shaft rotates to drive the stirring mounting seat, the nitration stirring rod, and the nitration hammer ball to stir and mix the raw materials for nitration reaction; Step S203, the reaction drive shaft rotates and can also drive the anti-blocking linkage seat to rotate, and the anti-blocking linkage seat rotates to drive the retractable spoiler to disturb the raw material fluid. At the same time, the inner positioning seat and the inner limit groove limit the inner hinge block, so that the inner hinge block drives the arc-shaped flip plate, the adjustable spoiler shaft and the retractable spoiler to rotate, thereby enhancing the spoiler effect; Step S204, the reaction drive shaft can drive the first gear to rotate by forward and reverse rotation, the first gear rotation drives the second gear rotation, the second gear rotation can drive the limit groove rotation, the limit groove drives the swing connecting rod to swing, the swing connecting rod drives the limit connecting seat and the rack limit seat to guide and limit the swing rack, and at the same time, the second gear rotation drives the swing rack to swing, and the end of the swing rack away from the second gear intermittently meshes with the third gear, so that the third gear drives the cooling adjustment shaft to rotate, and the cooling adjustment shaft rotation drives the adjustment thread sleeve and the component support seat to reciprocate along the equipment base, thereby realizing the adjustment of the cooling position of the medium guide tube, and by controlling the feed amount and the circulation amount of the cooling medium of the dynamic reaction tube, the reaction temperature of the dynamic reaction tube is kept below 10°C; Step S205, the material discharged from the dynamic reaction tube enters the nitration material buffer tank for sampling and analysis, and the reaction is determined to be complete if the raw material content is less than 0.5%; Step S206: The reaction liquid in the nitration material buffer tank overflows into the oleic acid separation tank for separation, and the upper organic phase overflows into the desulfurization tank. After the chloromethane intermediate tank, the dichloromethane is recovered in the dichloromethane recovery kettle, and the lower acid phase flows into the hydrolysis kettle. The material is centrifuged and dried at 80℃. The intermediate 7-fluoro-6-nitro-2H-1,4-benzoxazin-3(4H)-one was obtained.

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