Preparation method of fluopyrabactam

Abstract

The invention provides a method for preparing fluopyrabamide. The method is applied to fluopyrabamide production equipment. The production equipment comprises: a continuous condensation reaction device for providing a product produced by a continuous condensation reaction, and a continuous batching device and a first raw material supply device respectively connected with the continuous condensation reaction device. The continuous batching device is used to transport a 3', 4', 5'-trifluoro-2-aminobiphenyl solution into the continuous condensation reaction device. The first raw material supply device is used to continuously transport pyridine and 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride into the continuous condensation reaction device. A continuous condensation reaction occurs in the continuous condensation reaction device to generate a crude product. The production equipment also comprises a continuous post-processing device for continuously post-processing the crude product to obtain a reaction product. The problems of low reaction efficiency and low product quality caused by batch reactions in the prior art are solved.

Description

Technical Field

[0001] The invention relates to the technical field of fluopyrabamide preparation, and in particular to a method for preparing fluopyrabamide. Background Art

[0002] At present, the main production process of flupyraclostrobin is to use 3,4,5-trifluoro-2'-nitrobiphenyl and 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride as raw materials and condense them to obtain qualified products.

[0003] In the prior art, in the process of producing flupyraclostrobin, a batch condensation reaction is generally carried out using a reactor, which requires a large amount of manual operation and material transfer. In addition, the raw material 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride is extremely active in chemical properties and is easily deteriorated when exposed to the air for a long time. The batch condensation reaction in the prior art will affect the quality of the final product. Summary of the invention

[0004] The main purpose of the present invention is to provide a method for preparing fluopyraclostrobin, so as to solve the problem in the prior art that the quality of the final product is affected by batch reaction.

[0005] In order to achieve the above object, according to one aspect of the present invention, a fluopyrabamide production device is provided, the production device comprising: a continuous condensation reaction device, the continuous condensation reaction device is used to provide a continuous condensation reaction site for preparing fluopyrabamide;

[0006] A continuous dosing device, which is connected to the continuous condensation reaction device to continuously provide 3',4',5'-trifluoro-2-aminobiphenyl solution as a first reaction raw material to the continuous condensation reaction device;

[0007] a first raw material supply device, the first raw material supply device being connected to the continuous condensation reaction device to continuously supply pyridine and 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride as a second reaction raw material to the continuous condensation reaction device;

[0008] A continuous post-processing device, which is connected to the continuous condensation reaction device to continuously post-process the crude product obtained by the continuous condensation reaction device to obtain a reaction product;

[0009] The first reaction raw material and the second reaction raw material undergo continuous condensation reaction in the continuous condensation reaction site to obtain a crude product.

[0010] Furthermore, the continuous post-processing device comprises:

[0011] A continuous acidification unit, which is connected to the continuous condensation reaction device to continuously acidify the crude product to obtain an acid-washed product system;

[0012] The continuous alkalization unit is connected with the continuous acidification unit to continuously perform alkali washing on the acid-washing product system to obtain the alkali-washing product system.

[0013] Furthermore, the continuous post-processing device also includes:

[0014] A continuous water washing unit, the continuous water washing unit is connected to the continuous alkalization unit to continuously wash the alkali-washed product system with water to obtain a water-washed product system;

[0015] A continuous crystallization unit, the continuous crystallization unit is connected to the continuous water washing unit to continuously crystallize the water washing product system to obtain a crystallization product system;

[0016] A continuous filtration unit, the continuous filtration unit is connected to the continuous crystallization unit to continuously filter the crystallization product system to obtain a filtration product system;

[0017] A drying unit is connected to the continuous filtering unit to dry the filtered product system to obtain a reaction product.

[0018] Furthermore, the continuous batching device comprises:

[0019] Continuous batching tank;

[0020] A continuous solid feeder, which is connected to the continuous batching tank to continuously transport the 3',4',5'-trifluoro-2-aminobiphenyl solid stored in the continuous solid feeder to the continuous batching tank;

[0021] A solvent storage tank, the solvent storage tank is connected to the continuous batching tank through a first pipeline, so that the solvent in the solvent storage tank is continuously transported from the first pipeline to the continuous batching tank, and continuously mixed with the 3',4',5'-trifluoro-2-aminobiphenyl solid in the continuous batching tank to obtain a 3',4',5'-trifluoro-2-aminobiphenyl solution;

[0022] The inlet of the liquid storage tank is connected with the continuous batching tank to accommodate the 3',4',5'-trifluoro-2-aminobiphenyl solution delivered from the continuous batching tank; and the outlet of the liquid storage tank is connected with the continuous condensation reaction device.

[0023] Furthermore, the continuous batching device also includes:

[0024] A first liquid flow meter, which is disposed on the first pipeline to detect the real-time flow of the liquid flowing through the first pipeline and generate a corresponding detection result;

[0025] The solvent feed pump is arranged on the first pipeline and is connected to the first liquid flow meter to control the flow rate of the solvent in the solvent storage tank entering the continuous dosing tank according to the detection result of the first liquid flow meter.

[0026] Furthermore, the continuous batching device also includes:

[0027] The first heat exchanger has a relatively independent first heat exchange channel and a second heat exchange channel. The first heat exchange channel is used to circulate a preheating medium. One port of the second heat exchange channel is connected to the outlet of the liquid storage tank to perform heat exchange on the 3', 4', 5'-trifluoro-2-aminobiphenyl solution flowing out of the liquid storage tank to increase the temperature of the 3', 4', 5'-trifluoro-2-aminobiphenyl solution.

[0028] Furthermore, the first raw material supply device comprises:

[0029] a first continuous mixing tank, the first continuous mixing tank being connected to the continuous condensation reaction device and another port of the second heat exchange channel respectively;

[0030] A first raw material tank, in which pyridine is stored, and the first raw material tank is connected to the first continuous mixing tank to transport pyridine into the first continuous mixing tank;

[0031] a second raw material tank, wherein 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride is stored in the second raw material tank, and the second raw material tank is connected to the first continuous mixing tank to continuously transport 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride into the first continuous mixing tank;

[0032] Wherein, pyridine, 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride and the 3',4',5'-trifluoro-2-aminobiphenyl solution after heat exchange in the first heat exchanger are continuously mixed in the first continuous mixing tank to obtain a mixed product system, and the mixed product system is transported to a continuous condensation reaction device to carry out a continuous condensation reaction to obtain a crude product.

[0033] Further, the continuous acidification unit comprises:

[0034] a second heat exchanger, the second heat exchanger having relatively independent third and fourth heat exchange channels, the third heat exchange channel being used for circulating cooling medium, and one port of the fourth heat exchange channel being connected to the continuous condensation reaction device to perform heat exchange on the crude product from the continuous condensation reaction device to reduce the temperature of the crude product;

[0035] A second continuous mixing tank, the second continuous mixing tank is connected to another port of the fourth heat exchange channel, and the crude product after heat exchange in the second heat exchanger enters the second continuous mixing tank; the outlet of the second continuous mixing tank is connected to the continuous alkalization unit;

[0036] An acid liquid storage tank stores acid liquid, and the acid liquid storage tank is connected to the second continuous mixing tank for continuously conveying acid liquid to the second continuous mixing tank, so as to continuously acidify the crude product in the second continuous mixing tank after heat exchange in the second heat exchanger, so as to obtain a pickling product system.

[0037] Furthermore, the pipeline connecting the outlet of the second continuous mixing tank and the continuous alkalization unit is also provided with:

[0038] The first continuous liquid separation component has a first heavy phase outlet and a first light phase outlet. The pickling product system enters the first continuous liquid separation component for continuous liquid separation to obtain a first heavy phase and a first light phase. The first light phase outlet is connected to the continuous alkalization unit.

[0039] The first heavy phase collecting tank is communicated with the first heavy phase outlet and is used for collecting the first heavy phase.

[0040] Furthermore, the pickling product system is continuously separated by the first continuous separation component to obtain a first heavy phase and a first light phase, and the continuous alkalization unit includes:

[0041] a third continuous mixing tank, wherein the inlet of the third continuous mixing tank is connected to the continuous acidification unit through a third pipeline, the first light phase enters the third continuous mixing tank from the third pipeline, and the outlet of the third continuous mixing tank is connected to the continuous water washing unit;

[0042] An alkali liquid storage tank stores alkali liquid, and the alkali liquid storage tank is connected to the inlet of the third continuous mixing tank through a fourth pipeline, and is used to continuously transport alkali liquid to the third continuous mixing tank to continuously alkali wash the first light phase in the acid storage tank to obtain an alkali washing product system.

[0043] Furthermore, the pipeline between the outlet of the third continuous mixing tank and the continuous water washing unit is also provided with:

[0044] The second continuous liquid separation component has a second heavy phase outlet and a second light phase outlet. The alkali washing product system enters the second continuous liquid separation component for continuous liquid separation to obtain a second heavy phase and a second light phase. The second light phase outlet is connected to the continuous water washing unit.

[0045] The second heavy phase collecting tank is communicated with the second heavy phase outlet and is used for collecting the second heavy phase.

[0046] Furthermore, the alkali washing product system is separated by the second continuous separation component to obtain a second heavy phase and a second light phase, and the continuous water washing unit includes:

[0047] a fourth continuous mixing tank, wherein the inlet of the fourth continuous mixing tank is connected to the continuous alkalization unit through a fifth pipeline, the second light phase enters the fourth continuous mixing tank from the fifth pipeline, and the outlet of the fourth continuous mixing tank is connected to the continuous crystallization unit;

[0048] A water storage tank stores water, and the outlet of the water storage tank is connected to the inlet of the fourth continuous mixing tank, and is used to continuously transport water to the fourth continuous mixing tank to continuously wash the second light phase in the fourth continuous mixing tank to obtain a water-washed product system.

[0049] Furthermore, the pipeline between the outlet of the fourth continuous mixing tank and the continuous crystallization unit is also provided with:

[0050] A third continuous liquid separation component has a third heavy phase outlet and a third light phase outlet. The water-washed product system enters the third continuous liquid separation component for continuous liquid separation to obtain a third heavy phase and a third light phase. The third light phase outlet is connected to the continuous crystallization unit;

[0051] The third heavy phase collecting tank is connected with the third heavy phase outlet and is used for collecting the third heavy phase.

[0052] Further, the water-washed product system is continuously separated by a third continuous separation component to obtain a third heavy phase and a third light phase, and the continuous crystallization unit includes:

[0053] A continuous crystallization tank, the inlet of which is connected to a continuous water washing unit, is used to continuously crystallize the third light phase to obtain a crystallization product system.

[0054] Further, the continuous filtration unit comprises:

[0055] A continuous filtration tank, the inlet of which is connected to a continuous crystallization unit, so as to continuously filter the crystallization product system to obtain a filtration product system.

[0056] Furthermore, the drying unit comprises:

[0057] A continuous drying tank, the inlet of which is connected to the continuous filtering unit, is used to continuously dry the filtered product system to obtain a reaction product.

[0058] According to another aspect of the present invention, a method for preparing fluopyrabendazim is provided. The method is applied to the above production equipment to prepare fluopyrabendazim. The method comprises:

[0059] Controlling the continuous dosing device to continuously deliver the 3',4',5'-trifluoro-2-aminobiphenyl solution to the continuous condensation reaction device, and controlling the first raw material supply device to continuously deliver pyridine and 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride to the continuous condensation reaction device, and the 3',4',5'-trifluoro-2-aminobiphenyl solution and pyridine and 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride are continuously reacted in the continuous condensation reaction device to obtain a crude product;

[0060] The crude product is input into a continuous post-processing device, so as to control the continuous post-processing device to continuously post-process the crude product system to obtain a reaction product.

[0061] Furthermore, the preparation method also includes:

[0062] The crude product is transported to a continuous acidification unit for continuous acidification to obtain an acid washing product system;

[0063] The acid-washed product system is transported to a continuous alkalization unit for continuous alkalization to obtain an alkali-washed product system;

[0064] The alkali-washed product system is transported to a continuous water-washing unit for continuous water-washing to obtain a water-washed product system;

[0065] The water-washed product system is transported to a continuous crystallization unit for continuous crystallization to obtain a crystallized product system;

[0066] The crystallization product system is transported to a continuous filtration unit for continuous filtration to obtain a filtration product system;

[0067] The filtered product system is transported to a drying unit for continuous drying to obtain a reaction product.

[0068] Furthermore, the preparation method also includes:

[0069] Controlling the continuous solid feeder and the solvent storage tank to continuously deliver 3', 4', 5'-trifluoro-2-aminobiphenyl solid and solvent to the continuous batching tank at a first preset flow rate, and continuously batching in the continuous batching tank under the first preset condition to obtain a 3', 4', 5'-trifluoro-2-aminobiphenyl solution, and delivering the 3', 4', 5'-trifluoro-2-aminobiphenyl solution to the liquid storage tank;

[0070] Among them, the first preset condition is that the reaction temperature of continuous batching is 30°C to 50°C, the reaction time of continuous batching is 10min to 90min, the amount of solvent is 1g / 1-5ml, and the solvent is any one or more of toluene, xylene, ethyl acetate, and dichloroethane.

[0071] Furthermore, the preparation method also includes:

[0072] Controlling the 3',4',5'-trifluoro-2-aminobiphenyl solution after heat exchange in the first heat exchanger, the pyridine in the first raw material tank, and the 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride in the second raw material tank to be respectively transported to the first continuous mixing tank, and continuously mixed under the second preset condition to obtain a mixed product system;

[0073] The mixed product system is transported to a continuous condensation reaction device at a first preset flow rate, and a continuous condensation reaction occurs under a third preset condition to obtain a continuous condensation reaction system;

[0074] Among them, the second preset condition is that the first mixing temperature is 50°C to 80°C, the first continuous mixing time is 1min to 10min, and the third preset condition is that the condensation reaction time in the continuous condensation reaction device is 30min to 180min.

[0075] Furthermore, the preparation method also includes:

[0076] Controlling the acid in the acid storage tank and the crude product in the continuous condensation reaction device to be transported to the second continuous mixing tank at a second preset flow rate, and acidifying under a fourth preset condition to obtain an acid washing product system;

[0077] wherein the flow rate of the acid solution is 12 to 20 g / min; and / or,

[0078] The acid is any one of hydrochloric acid, sulfuric acid and acetic acid; and / or,

[0079] The concentration of the acid solution is 5% to 15%;

[0080] The fourth preset condition is that the acidification temperature is 40° C. to 80° C., and the acidification residence time is 10 min to 60 min.

[0081] Furthermore, the preparation method also includes:

[0082] Controlling the pickling product system to be transported to the first continuous liquid separation component at a first feed rate, and performing continuous liquid separation at a first liquid separation temperature to obtain a first heavy phase and a first light phase;

[0083] The first liquid separation temperature is 40°C to 80°C.

[0084] Furthermore, the preparation method also includes:

[0085] Controlling the alkali liquid in the alkali liquid storage tank to enter the third continuous mixing tank at a second feed rate, conveying the first light phase to the third continuous mixing tank at a second feed rate, and continuously alkali-washing with the alkali liquid under a fifth preset condition to obtain an alkali-washed product system;

[0086] Wherein, the alkali solution is any one of sodium carbonate, sodium bicarbonate, ammonium bicarbonate or a combination of several thereof; and / or,

[0087] The concentration of lye is 5% to 25%;

[0088] The fifth preset condition is that the alkali washing time is 10 minutes to 60 minutes, and the alkali washing temperature is 40° C. to 80° C.; and / or,

[0089] Controlling the alkali washing product system to be transported to the second continuous liquid separation component at a third feed rate, and performing continuous liquid separation under a sixth preset condition to obtain a second heavy phase and a second light phase;

[0090] Among them, the sixth preset condition is that the alkaline washing separation temperature is 40°C to 80°C.

[0091] Furthermore, the preparation method also includes:

[0092] Controlling the second light phase and the water in the water storage tank to be continuously transported to the fourth continuous mixing tank at a fourth feed rate, and continuously washing with water under a seventh preset condition to obtain a water-washed product system;

[0093] The second light phase is obtained by continuously separating the alkali-washed product system through the second continuous separation component, and the seventh preset condition is that the continuous water washing time is 10 minutes to 60 minutes, and the continuous water washing temperature is 40° C. to 80° C.;

[0094] Controlling the water-wash product system to be transported to the third continuous liquid separation component at a fifth feed amount, and continuously liquid separation under an eighth preset condition to obtain a third heavy phase and a third light phase;

[0095] Among them, the eighth preset condition is that the water washing and liquid separation temperature is 40°C to 80°C.

[0096] Furthermore, the preparation method also includes:

[0097] Controlling the third light phase to be transported to the continuous crystallization tank at a sixth feed amount, and performing continuous crystallization under a ninth preset condition to obtain a crystallization product system;

[0098] The third light phase is a water-washed product system obtained by continuous separation by a third continuous separation component, and the ninth preset condition is that the continuous crystallization temperature is -10°C to 20°C, and the continuous crystallization time is 30min to 180min; and / or,

[0099] Controlling the crystallization product system to enter the continuous filtration tank at a sixth feed amount for continuous filtration to obtain a filtration product system;

[0100] Wherein, the continuous filtration temperature is -10°C to 20°C; and / or,

[0101] Controlling the filtration product system to be transported to a continuous drying tank for continuous drying to obtain a reaction product;

[0102] The drying temperature is 40°C to 60°C, and the drying time is 30min to 90min.

[0103] By applying the technical solution of the present invention, during use, the first reaction raw material is continuously transported from the continuous batching device to the continuous condensation reaction device 601. The first reaction raw material in this embodiment is a 3', 4', 5'-trifluoro-2-aminobiphenyl solution. At the same time, the first raw material supply device continuously provides the second reaction raw material to the continuous condensation reaction device 601. The second reaction raw material is pyridine and 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride. The first reaction raw material and the second reaction raw material undergo a continuous condensation reaction in the continuous condensation reaction device 601 to obtain a crude product. The crude product is then continuously transported to a continuous post-processing device for continuous post-processing. After continuous post-processing by the continuous post-processing device, a reaction product is obtained, i.e., the flupyraclostrobin in the present application.

[0104] Compared with the traditional batch reactor, the production equipment provided by the present application is a continuous process, and its overall working volume is much smaller than that of the traditional batch reactor. At the same time, in the whole reaction process, the control of the reaction temperature is more accurate, so that the cycle heat energy consumption can be reduced, the selectivity of the reaction can be improved, and the reaction temperature can be accurately controlled, so that the reaction is more stable. At the same time, in the production equipment provided by the present application, the first reaction raw material and the second reaction raw material can be continuously input, and the obtained reaction product can be continuously discharged, which is conducive to reducing the generation of by-products, providing the selectivity of the reaction, and the material utilization rate of the whole process is relatively high, reducing the loss in different reaction processes, compared with the intermittent reaction, the reaction time can be significantly shortened, and the production equipment in the present application is continuous, so the contact interface of the liquid-liquid two phases in each device is large, so the reaction rate is increased. On this basis, the above-mentioned continuous device is adopted, and automation is also realized between each reaction device and the reaction unit, and the reaction conditions are relatively more stable, so the product quality obtained is more stable and uniform, and at the same time, the automated continuous process reduces manual intervention, reduces labor intensity and operating risks, can achieve more stable product quality, and helps to reduce the variation caused by inaccurate control of reaction conditions between batches. BRIEF DESCRIPTION OF THE DRAWINGS

[0105] The drawings constituting a part of the present application are used to provide a further understanding of the present invention. The exemplary embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation of the present invention. In the drawings:

[0106] Figure 1The process flow chart of the production of fluopyraclostrobin according to the embodiment of the present application is shown.

[0107] The above drawings include the following reference numerals:

[0108] 101, continuous solid feeder; 201, solvent storage tank; 202, first raw material tank; 203, second raw material tank; 204, acid storage tank; 205, alkali storage tank; 206, water storage tank; 301, liquid storage tank; 401, first heat exchanger; 402, third heat exchanger; 403, fourth heat exchanger; 404, second heat exchanger; 405, fifth heat exchanger; 406, sixth heat exchanger; 407, seventh heat exchanger; 501, first continuous mixing tank; 601, continuous condensation reaction device; 701, continuous batching tank; 801, first heavy phase collecting tank; 802, second heavy phase collecting tank; 803, third heavy phase collecting tank; 901, second continuous mixing tank; 902, third continuous mixing tank; 903, fourth Continuous mixing tank; 1001, continuous crystallization tank; 1101, first continuous liquid separation component; 1102, second continuous liquid separation component; 1103, third continuous liquid separation component; 1201, solvent feed pump; 1202, raw material feed pump; 1203, pyridine feed pump; 1204, liquid feed pump; 1205, acid feed pump; 1206, alkali feed pump; 1207, water feed pump; 1301, first liquid flow meter; 1302, second liquid flow meter; 1303, third liquid flow meter; 1304, fourth liquid flow meter; 1305, fifth liquid flow meter; 1306, sixth liquid flow meter; 1307, seventh liquid flow meter; 1401, continuous filtering tank; 1501, continuous drying tank. DETAILED DESCRIPTION

[0109] It should be noted that, in the absence of conflict, the embodiments and features in the embodiments of the present application can be combined with each other. The present invention will be described in detail below with reference to the accompanying drawings and in combination with the embodiments.

[0110] At present, the main production process of flupyraclostrobin is to use 3,4,5-trifluoro-2'-nitrobiphenyl and 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride as raw materials and condense them to obtain qualified products.

[0111] In the prior art, in the process of producing flupyraclostrobin, a batch condensation reaction is generally carried out using a reactor, which requires a large amount of manual operation and material transfer. In addition, the raw material 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride is extremely active in chemical properties and is easily deteriorated when exposed to the air for a long time. The batch condensation reaction in the prior art will affect the quality of the final product.

[0112] Therefore, the purpose of this application is to provide a continuous production device and preparation method of fluopyrabamide in view of the above problems, so as to solve the problem in the prior art that the quality of the final product is affected by batch reactions.

[0113] The present application first provides a continuous production device for fluopyrabamide, the continuous production device comprising: a continuous condensation reaction device 601, the continuous condensation reaction device 601 is used to provide a continuous condensation reaction site for preparing fluopyrabamide;

[0114] A continuous dosing device, which is connected to the continuous condensation reaction device 601 to continuously provide 3', 4', 5'-trifluoro-2-aminobiphenyl solution as a first reaction raw material to the continuous condensation reaction device 601;

[0115] A first raw material supply device, the first raw material supply device is connected to the continuous condensation reaction device 601 to continuously supply pyridine and 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride as a second reaction raw material to the continuous condensation reaction device 601;

[0116] A continuous post-processing device, which is connected to the continuous condensation reaction device 601 to continuously post-process the crude product obtained by the continuous condensation reaction device 601 to obtain a reaction product;

[0117] The first reaction raw material and the second reaction raw material undergo continuous condensation reaction in the continuous condensation reaction site to obtain a crude product.

[0118] Applying the technical solution of the present invention, during use, such as Figure 1 As shown, a first reaction raw material is continuously transported from a continuous dosing device to a continuous condensation reaction device 601. The first reaction raw material in this embodiment is a 3', 4', 5'-trifluoro-2-aminobiphenyl solution. At the same time, a second reaction raw material is continuously provided in the first raw material supply device to the continuous condensation reaction device 601. The second reaction raw material is pyridine and 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride. The first reaction raw material and the second reaction raw material undergo a continuous condensation reaction in the continuous condensation reaction device 601 to obtain a crude product. The crude product is then continuously transported to a continuous post-treatment device for continuous post-treatment. After continuous post-treatment by the continuous post-treatment device, a reaction product is obtained, i.e., the flupyraclostrobin in the present application.

[0119] Compared with the traditional batch reactor, the production equipment provided by the present application is a continuous process, and its overall working volume is much smaller than that of the traditional batch reactor. At the same time, in the whole reaction process, the control of the reaction temperature is more accurate, so that the cycle heat energy consumption can be reduced, the selectivity of the reaction can be improved, and the reaction temperature can be accurately controlled, so that the reaction is more stable. At the same time, in the production equipment provided by the present application, the first reaction raw material and the second reaction raw material can be continuously input, and the obtained reaction product can be continuously discharged, which is conducive to reducing the generation of by-products, providing the selectivity of the reaction, and the material utilization rate of the whole process is relatively high, reducing the loss in different reaction processes, compared with the intermittent reaction, the reaction time can be significantly shortened, and the production equipment in the present application is continuous, so the contact interface of the liquid-liquid two phases in each device is large, so the reaction rate is increased. On this basis, the above-mentioned continuous device is adopted, and automation is also realized between each reaction device and the reaction unit, and the reaction conditions are relatively more stable, so the product quality obtained is more stable and uniform, and at the same time, the automated continuous process reduces manual intervention, reduces labor intensity and operating risks, can achieve more stable product quality, and helps to reduce the variation caused by inaccurate control of reaction conditions between batches.

[0120] Further, the continuous post-treatment device includes: a continuous acidification unit, which is connected to the continuous condensation reaction device 601 to continuously acidify the crude product to obtain an acid-washed product system;

[0121] A continuous alkalization unit, the continuous alkalization unit is connected to the continuous acidification unit to continuously alkali wash the acid-washed product system to obtain an alkali-washed product system;

[0122] A continuous water washing unit, the continuous water washing unit is connected to the continuous alkalization unit to continuously wash the alkali-washed product system with water to obtain a water-washed product system;

[0123] A continuous crystallization unit, the continuous crystallization unit is connected to the continuous water washing unit to continuously crystallize the water washing product system to obtain a crystallization product system;

[0124] A continuous filtration unit, the continuous filtration unit is connected to the continuous crystallization unit to continuously filter the crystallization product system to obtain a filtration product system;

[0125] A drying unit is connected to the continuous filtering unit to dry the filtered product system to obtain a reaction product.

[0126] During use, the crude product in the continuous condensation reaction device is continuously transported to the continuous acidification unit, and the continuous acidification unit continuously acidifies the crude product to obtain a pickling product system, and the obtained pickling product system is continuously transported to the continuous alkalization unit, and the continuous alkalization unit continuously alkalizes and obtains an alkalization product system, and the alkalization product system is transported to the continuous water washing unit for continuous water washing to obtain a water washing product system, and the water washing product system is continuously transported to the continuous crystallization unit to obtain a crystallization product system, and the crystallization product system is continuously transported to the continuous filtration unit to continuously filter the crystallization product system to obtain a filtration product system, and the filtration product system is continuously transported to the drying unit for continuous drying to obtain a reaction product.

[0127] By providing a continuous acidification unit, a continuous alkalization unit, a continuous water washing unit, a continuous crystallization unit, a continuous filtration unit and a drying unit, uninterrupted processing of the product can be achieved. Compared with the existing technology, there is no need to wait for one batch of reactions to be completed before starting the next batch, which greatly speeds up the reaction rate. At the same time, it simplifies the traditional intermittent operation process such as material transfer, static separation and other operations, and the production efficiency is increased by more than 30%. The time consumption of the entire production process is shortened, and the production efficiency of flupyraclostrobin is improved.

[0128] The continuous batching device comprises: a continuous batching tank 701;

[0129] A continuous solid feeder 101, which is in communication with a continuous batching tank 701, so as to continuously deliver the 3', 4', 5'-trifluoro-2-aminobiphenyl solid stored therein to the continuous batching tank 701;

[0130] The solvent storage tank 201 is connected to the continuous batching tank 701 through a first pipeline, so that the solvent in the solvent storage tank 201 is continuously transported from the first pipeline to the continuous batching tank 701, and is continuously mixed with the 3',4',5'-trifluoro-2-aminobiphenyl solid in the continuous batching tank 701 to obtain a 3',4',5'-trifluoro-2-aminobiphenyl solution;

[0131] The liquid storage tank 301 has an inlet connected to the continuous batching tank 701 to accommodate the 3', 4', 5'-trifluoro-2-aminobiphenyl solution transported from the continuous batching tank 701; and the outlet of the liquid storage tank 301 is connected to the continuous condensation reaction device 601.

[0132] By providing the solvent storage tank 201 and the continuous solid feeder 101, it is possible to continuously transport the 3', 4', 5'-trifluoro-2-aminobiphenyl solid and the solvent to the continuous batching tank 701 for continuous batching. After the continuous batching in the continuous batching tank 701 forms a 3', 4', 5'-trifluoro-2-aminobiphenyl solution, the formed 3', 4', 5'-trifluoro-2-aminobiphenyl solution can be continuously transported to the liquid storage tank 301, and the liquid storage tank 301 then feeds the 3', 4', 5'-trifluoro-2-aminobiphenyl solid and the solvent to the continuous batching tank 701 for continuous batching. The benzene solution is continuously transported to the continuous condensation reaction device 601, and continuously condenses with pyridine and 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride in the continuous condensation reaction device 601 to continuously obtain the reaction product, i.e., flupyraclostrobin. This not only speeds up the reaction rate, but also reduces the difference caused by batch reactions, reduces the waste of raw materials and energy, and reduces production costs. The type of the continuous batching tank 701 is one or more of a continuous reactor, a continuous reaction house, and a continuous extraction house.

[0133] The continuous batching device further includes: a first liquid flow meter 1301, which is arranged on the first pipeline to detect the real-time flow of the liquid flowing through the first pipeline and generate a corresponding detection result;

[0134] The solvent feed pump 1201 is disposed on the first pipeline and is connected to the first liquid flow meter 1301 to control the flow of the solvent in the solvent storage tank 201 entering the continuous dosing tank 701 according to the detection result of the first liquid flow meter 1301 .

[0135] Specifically, the continuous dosing device also includes a first liquid flow meter 1301 arranged on the first pipeline, which is used to detect the real-time flow rate of the liquid flowing through the first pipeline and generate a corresponding detection result. A solvent feed pump 1201 is also provided on the first pipeline. The flow rate of the solvent in the solvent storage tank 201 entering the continuous dosing tank 701 can be controlled in real time according to the detection result of the first liquid flow meter 1301, so as to control the amount of the generated 3', 4', 5'-trifluoro-2-aminobiphenyl solution, and then control the amount of the generated fluopyram. By providing the first liquid flow meter 1301, the amount of the solvent can be well controlled, and the corresponding fluopyram can be produced according to actual needs.

[0136] The continuous dosing device also includes: a first heat exchanger 401, the first heat exchanger 401 has a relatively independent first heat exchange channel and a second heat exchange channel, the first heat exchange channel is used to circulate the preheating medium, and one port of the second heat exchange channel is connected to the outlet of the liquid storage tank 301, so as to exchange heat with the 3', 4', 5'-trifluoro-2-aminobiphenyl solution flowing out of the liquid storage tank 301, so as to increase the temperature of the 3', 4', 5'-trifluoro-2-aminobiphenyl solution.

[0137] By providing the first heat exchanger 401, the 3',4',5'-trifluoro-2-aminobiphenyl solution flowing out of the liquid storage tank 301 can be heat exchanged in advance to increase the temperature of the 3',4',5'-trifluoro-2-aminobiphenyl solution flowing out of the liquid storage tank 301 for heat exchange, thereby accelerating the reaction of the 3',4',5'-trifluoro-2-aminobiphenyl solution flowing out of the liquid storage tank 301 with pyridine and 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride. The rate of fluopyrabamide production can be increased by increasing the feed rate. A raw material feed pump 1202 and a second liquid flow meter 1302 are provided on the pipeline connecting the liquid storage tank 301 and the first heat exchanger 401 to detect the flow of the 3', 4', 5'-trifluoro-2-aminobiphenyl solution entering the first heat exchanger 401 in real time, and the valve opening of the raw material feed pump 1202 is controlled according to the detection result. The first heat exchanger 401 is one or more of a shell and tube heat exchanger, a spiral tube heat exchanger, and a plate heat exchanger.

[0138] The first raw material supply device comprises: a first continuous mixing tank 501, the first continuous mixing tank 501 is connected with the continuous condensation reaction device 601 and the other port of the second heat exchange channel respectively;

[0139] A first raw material tank 202, in which pyridine is stored, and the first raw material tank 202 is connected to the first continuous mixing tank 501 to transport pyridine into the first continuous mixing tank 501;

[0140] A second raw material tank 203, in which 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride is stored, and the second raw material tank 203 is connected to the first continuous mixing tank 501 to continuously transport 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride into the first continuous mixing tank 501;

[0141] Among them, pyridine, 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride and the 3',4',5'-trifluoro-2-aminobiphenyl solution after heat exchange in the first heat exchanger 401 are continuously mixed in the first continuous mixing tank 501 to obtain a mixed product system, and the mixed product system is transported to the continuous condensation reaction device 601 to carry out a continuous condensation reaction to obtain a crude product.

[0142] By providing the first raw material tank 202 and the second raw material tank 203, pyridine and 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride can be continuously transported into the first continuous mixing tank 501, so that the two can be timely subjected to continuous condensation reaction with the 3', 4', 5'-trifluoro-2-aminobiphenyl solution in the first continuous mixing tank 501 to continuously obtain a crude product. By continuously transporting 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride to the first continuous mixing tank 501 for continuous mixing, it is possible to avoid contact with air due to its active chemical properties. , and deterioration occurs; a third heat exchanger 402 is further provided between the first raw material tank 202 and the first continuous mixing tank 501, and a third liquid flow meter 1303 and a pyridine feeding pump 1203 are further provided on the pipeline between the first raw material tank 202 and the third heat exchanger 402. By controlling the valve opening of the pyridine feeding pump 1203 according to the detection result of the third liquid flow meter 1303, the amount of pyridine entering the third heat exchanger 402 can be controlled. By providing the third heat exchanger 402, the pyridine can be preliminarily heat exchanged to preliminarily increase the temperature of the pyridine, thereby accelerating the first continuous mixing tank 5 01, the other end of the third heat exchanger 402 is connected to the inlet end of the third heat exchanger 402; at the same time, a liquid feed pump 1204, a fourth liquid flow meter 1304 and a fourth heat exchanger 403 are sequentially provided on the pipeline between the second raw material tank 203 and the first continuous mixing tank 501, the fourth liquid flow meter 1304 is used to detect the flow rate of the liquid entering the fourth heat exchanger 403 in real time, and the liquid feed pump 1204 is used to control the flow of 3-(difluoromethyl)-1 ... -methyl-1H-pyrazole-4-carbonyl chloride, the fourth heat exchanger 403 is used to preliminarily increase the temperature of 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride to accelerate the mixing rate of pyridine and 3',4',5'-trifluoro-2-aminobiphenyl solution after heat exchange in the first continuous mixing tank 501, the first continuous mixing tank 501 is one or more of a dynamic tubular reactor, a continuous axe reactor, and a continuous tubular reactor, the third heat exchanger 402 and the fourth heat exchanger 403 are one or more of a shell and tube heat exchanger, a spiral tube heat exchanger, and a plate heat exchanger.

[0143] The continuous acidification unit includes: a second heat exchanger 404, the second heat exchanger 404 has a relatively independent third heat exchange channel and a fourth heat exchange channel, the third heat exchange channel is used to circulate cooling medium, and one port of the fourth heat exchange channel is connected to the continuous condensation reaction device 601 to perform heat exchange on the crude product from the continuous condensation reaction device 601 to reduce the temperature of the crude product;

[0144] The second continuous mixing tank 901 is connected to another port of the fourth heat exchange channel, and the crude product after heat exchange in the second heat exchanger 404 enters the second continuous mixing tank 901; the outlet of the second continuous mixing tank 901 is connected to the continuous alkalization unit;

[0145] The acid liquid storage tank 204 stores acid liquid, and the acid liquid storage tank 204 is connected to the second continuous mixing tank 901 for continuously conveying acid liquid to the second continuous mixing tank 901, so as to continuously acidify the crude product in the second continuous mixing tank 901 after heat exchange in the second heat exchanger 404, so as to obtain a pickling product system.

[0146] By providing a second heat exchanger 404, it is possible to achieve heat exchange of the crude product from the continuous condensation reaction device 601 to reduce the temperature of the crude product, which is beneficial to the subsequent acidification of the crude product. An acid feed pump 1205, a fifth liquid flow meter 1305 and a fifth heat exchanger 405 are provided in sequence between the acid storage tank 204 and the second continuous mixing tank 901. The fifth liquid flow meter 1305 is used to detect the flow of the acid in real time and control the valve opening of the acid feed pump 1205 according to the detection result. The fifth heat exchanger 405 is used to reduce the temperature of the acid because the pickling process is an exothermic process. The second heat exchanger 404 and the fifth heat exchanger 405 are one or more of a shell and tube heat exchanger, a spiral tube heat exchanger, and a plate heat exchanger. The second continuous mixing tank 901 is one or more of a dynamic tubular reactor, a continuous axe reactor, and a continuous tubular reactor.

[0147] The outlet of the second continuous mixing tank 901 is connected to the pipeline of the continuous alkalization unit and is also provided with:

[0148] The first continuous liquid separation component 1101 has a first heavy phase outlet and a first light phase outlet. The pickling product system enters the first continuous liquid separation component 1101 for continuous liquid separation to obtain a first heavy phase and a first light phase. The first light phase outlet is connected to the continuous alkalization unit.

[0149] The first heavy phase collecting tank 801 is connected to the first heavy phase outlet and is used to collect the first heavy phase.

[0150] By providing a first continuous liquid separation component 1101, it is possible to achieve continuous acidification of the pickling product system, and continuously obtain a first heavy phase and a first light phase. The first heavy phase enters the first heavy phase collection tank 801 through the first heavy phase outlet for storage, and the first light phase enters the continuous alkalization unit from the first light phase outlet for continuous alkalization. The type of the first continuous liquid separation component 1101 is one or more of a continuous centrifugal extractor, a continuous extraction column, and a static liquid separator.

[0151] Furthermore, the pickling product system is continuously separated by the first continuous separation component 1101 to obtain a first heavy phase and a first light phase, and the continuous alkalization unit includes:

[0152] A third continuous mixing tank 902, the inlet of the third continuous mixing tank 902 is connected to the continuous acidification unit through a third pipeline, the first light phase enters the third continuous mixing tank 902 from the third pipeline, and the outlet of the third continuous mixing tank 902 is connected to the continuous water washing unit;

[0153] An alkali liquid storage tank 205, wherein alkali liquid is stored in the alkali liquid storage tank 205, and the alkali liquid storage tank 205 is connected to the inlet of the third continuous mixing tank 902 through a fourth pipeline, and is used for continuously conveying alkali liquid into the third continuous mixing tank 902, so as to continuously alkali wash the first light phase in the alkali liquid storage tank 205, so as to obtain an alkali washing product system;

[0154] The pipeline between the outlet of the third continuous mixing tank 902 and the continuous water washing unit is also provided with:

[0155] The second continuous liquid separation component 1102 has a second heavy phase outlet and a second light phase outlet. The alkali washing product system enters the second continuous liquid separation component 1102 for continuous liquid separation to obtain a second heavy phase and a second light phase. The second light phase outlet is connected to the continuous water washing unit.

[0156] The second heavy phase collecting tank 802 is connected to the second heavy phase outlet and is used to collect the second heavy phase.

[0157] By providing an alkali liquid storage tank 205, it is possible to continuously input alkali liquid into the third continuous mixing tank 902, so as to continuously alkali wash the acid washing product system in the third continuous mixing tank 902, and continuously obtain an alkali washing product system, and continuously transport the alkali washing product system to the second continuous liquid separation component 1102 for continuous liquid separation, and obtain a second heavy phase and a second light phase, the second heavy phase continuously enters the second heavy phase collecting tank 802 from the second heavy phase outlet for storage, and the second light phase continuously enters the continuous water washing unit from the second light phase outlet for continuous water washing, and an alkali liquid feed pump 1206 for detecting alkali is also provided on the pipeline between the alkali liquid storage tank 205 and the third continuous mixing tank 902. The sixth liquid flow meter 1306 for measuring the liquid flow rate and the sixth heat exchanger 406 for increasing the temperature of the alkali liquid, the alkali liquid feed pump 1206 controls the valve opening of the alkali liquid feed pump 1206 according to the size of the sixth liquid flow meter 1306, the other port of the sixth heat exchanger 406 is connected to the inlet of the third continuous mixing tank 902, the sixth heat exchanger 406 is one or more of a shell and tube heat exchanger, a spiral tube heat exchanger, and a plate heat exchanger, the third continuous mixing tank 902 is one or more of a dynamic tubular reactor, a continuous axe reactor, and a continuous tubular reactor, and the second continuous liquid separation component 1102 is one or more of a continuous centrifugal extractor, a continuous extraction column, and a static liquid separator.

[0158] Further, the alkali washing product system is separated by the second continuous separation component 1102 to obtain a second heavy phase and a second light phase, and the continuous water washing unit includes:

[0159] A fourth continuous mixing tank 903, the inlet of the fourth continuous mixing tank 903 is connected to the continuous alkalization unit through a fifth pipeline, the second light phase enters the fourth continuous mixing tank 903 from the fifth pipeline, and the outlet of the fourth continuous mixing tank 903 is connected to the continuous crystallization unit;

[0160] A water storage tank 206, in which water is stored, and the outlet of the water storage tank 206 is connected to the inlet of the fourth continuous mixing tank 903, and is used to continuously transport water to the fourth continuous mixing tank 903, so as to continuously wash the second light phase in the fourth continuous mixing tank 903 with water, so as to obtain a water-washed product system;

[0161] The pipeline between the outlet of the fourth continuous mixing tank 903 and the continuous crystallization unit is also provided with:

[0162] The third continuous liquid separation component 1103 has a third heavy phase outlet and a third light phase outlet. The water-washed product system enters the third continuous liquid separation component 1103 for continuous liquid separation to obtain a third heavy phase and a third light phase. The third light phase outlet is connected to the continuous crystallization unit;

[0163] The third heavy phase collecting tank 803 is connected to the third heavy phase outlet and is used for collecting the third heavy phase.

[0164] By providing a water storage tank 206, it is possible to continuously input water into the fourth continuous mixing tank 903, so as to continuously wash the alkali washing product system in the fourth continuous mixing tank 903 with water, and continuously obtain a washed product system, the type of water is one or more of tap water and purified water, the washed product system is continuously transported to the third continuous liquid separation component 1103 for continuous liquid separation, and a third heavy phase and a third light phase are obtained, the third heavy phase continuously enters the third heavy phase collecting tank 803 from the third heavy phase outlet for storage, and the third light phase continuously enters the continuous separation component 1103 from the third light phase outlet for storage. The crystal unit performs continuous crystallization, and a water feed pump 1207, a seventh liquid flow meter 1307 for detecting the flow rate of water, and a seventh heat exchanger 407 for increasing the water temperature are further provided on the pipeline between the water storage tank 206 and the fourth continuous mixing tank 903. The other end of the seventh heat exchanger 407 is connected to the fourth continuous mixing tank 903. The seventh heat exchanger 407 is one or more of a shell-and-tube heat exchanger, a spiral tube heat exchanger, and a plate heat exchanger. The type of the third continuous liquid separation component 1103 is one or more of a continuous centrifugal extractor, a continuous extraction column, and a static liquid separator.

[0165] Further, the water-washed product system is continuously separated by the third continuous separation component 1103 to obtain a third heavy phase and a third light phase, and the continuous crystallization unit includes: a continuous crystallization tank 1001, and the inlet of the continuous crystallization tank 1001 is connected to the continuous water-washing unit to continuously crystallize the third light phase to obtain a crystallization product system;

[0166] The continuous filtration unit comprises: a continuous filtration tank 1401, the inlet of the continuous filtration tank 1401 is connected to the continuous crystallization unit to continuously filter the crystallization product system to obtain a filtration product system;

[0167] The drying unit includes: a continuous drying tank 1501, the inlet of the continuous drying tank 1501 is connected to the continuous filtering unit to continuously dry the filtered product system to obtain a reaction product.

[0168] By providing a continuous crystallization tank 1001, a continuous filtration tank 1401 and a continuous drying tank 1501, the third light phase, the crystallization product system and the filtration product system can be continuously processed, the reaction rate of preparing fluopyrabamide is increased, and the product quality of the produced fluopyrabamide is improved, wherein the type of the continuous crystallization tank 1001 is one or more of a horizontal flow reactor and a dynamic tubular reactor, and the type of the continuous filtration tank 1401 is one or more of a horizontal screw centrifuge and a rotary table filter.

[0169] Example 1

[0170] The present application embodiment provides a fluopyraclostrobin production device, such as Figure 1 As shown, the production equipment includes: controlling the continuous solid feeder 101 to continuously deliver 3', 4', 5'-trifluoro-2-aminobiphenyl solid to the continuous batching tank 701, and at the same time, controlling the solvent storage tank 201 to continuously deliver the solvent to the continuous batching tank 701, so that the two are continuously batched in the continuous batching tank 701 to form a 3', 4', 5'-trifluoro-2-aminobiphenyl solution, and then continuously delivering the 3', 4', 5'-trifluoro-2-aminobiphenyl solution to the liquid storage tank 301 for insulation, and then delivering it to the first heat exchanger 401 for heat exchange to increase the temperature of the 3', 4', 5'-trifluoro-2-aminobiphenyl solution, and delivering it to the first continuous mixing tank 501, At the same time, the pyridine in the first raw material tank 202 and the 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride in the second raw material tank 203 are controlled to be continuously transported to the first continuous mixing tank 501 for continuous mixing, and the mixed product system after mixing is continuously transported to the continuous condensation reaction device 601 for continuous condensation reaction to obtain a crude product, and the crude product is continuously transported to the second heat exchanger 404 for heat exchange to reduce the temperature of the crude product, and the crude product after the temperature is reduced is transported to the second continuous mixing tank 901, and at the same time, the acid in the acid storage tank 204 is controlled to be continuously transported to the second continuous mixing tank 901 to continuously acid wash the crude product, and obtain the acid washing product system. , the acid washing product system is continuously transported to the first continuous liquid separation component 1101 for continuous liquid separation, and a first heavy phase and a first light phase are obtained. The first heavy phase is collected by the first heavy phase collecting tank 801, and the first light phase enters the third continuous mixing tank 902. At the same time, the alkali solution storage tank 205 is controlled to continuously transport alkali solution to the third continuous mixing tank 902 to continuously alkali wash the first light phase and obtain an alkali washing product system, and the alkali washing product system is continuously transported to the second continuous liquid separation component 1102 for continuous liquid separation, and a second heavy phase and a second light phase are obtained. The second heavy phase is collected by the second heavy phase collecting tank 802, and the second light phase enters the fourth continuous mixing tank 903, and the water storage tank 206 is controlled to continuously transport alkali solution to the fourth continuous mixing tank 903, to continuously wash the second light phase in the fourth continuous mixing tank 903 with water, and obtain a water-washed product system; the water-washed product system is continuously transported to the third continuous liquid separation component 1103 for continuous liquid separation, and a third heavy phase and a third light phase are obtained; the third heavy phase is continuously collected by the third heavy phase collecting tank 803; the third light phase enters the continuous crystallization tank 1001 for continuous crystallization, and a crystallization product system is obtained; the crystallization product system is continuously transported to the continuous filtering tank 1401, and the crystallization product system is continuously filtered to obtain a filtered product system; the filtered product system is continuously transported to the continuous drying tank 1501 for continuous drying to obtain a reaction product, i.e., flupyracodymid.

[0171] The present application also provides a method for preparing fluopyrabendazole, which uses the above production equipment to prepare fluopyrabendazole, and the preparation method comprises:

[0172] Controlling the continuous batching device to continuously deliver the 3',4',5'-trifluoro-2-aminobiphenyl solution to the continuous condensation reaction device, and controlling the first raw material supply device to continuously deliver pyridine and 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride to the continuous condensation reaction device, and the 3',4',5'-trifluoro-2-aminobiphenyl solution and pyridine and 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride are continuously reacted in the continuous condensation reaction device to obtain a crude product;

[0173] Controlling the continuous solid feeder and the solvent storage tank to continuously deliver 3', 4', 5'-trifluoro-2-aminobiphenyl solid and solvent to the continuous batching tank at a first preset flow rate, and continuously batching in the continuous batching tank under the first preset condition to obtain a 3', 4', 5'-trifluoro-2-aminobiphenyl solution, and delivering the 3', 4', 5'-trifluoro-2-aminobiphenyl solution to the liquid storage tank;

[0174] Among them, the first preset condition is that the reaction temperature of continuous batching is 30°C to 50°C, the reaction time of continuous batching is 10min to 90min, the amount of solvent is 1g / 1-5ml, and the solvent is any one or more of toluene, xylene, ethyl acetate, and dichloroethane.

[0175] Controlling the 3',4',5'-trifluoro-2-aminobiphenyl solution after heat exchange in the first heat exchanger, the pyridine in the first raw material tank, and the 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride in the second raw material tank to be respectively transported to the first continuous mixing tank, and continuously mixed under the second preset condition to obtain a mixed product system;

[0176] The mixed product system is transported to a continuous condensation reaction device at a first preset flow rate, and a continuous condensation reaction occurs under a third preset condition to obtain a continuous condensation reaction system;

[0177] Among them, the second preset condition is that the first mixing temperature is 50°C to 80°C, the first continuous mixing time is 1min to 10min, and the third preset condition is that the condensation reaction time in the continuous condensation reaction device is 30min to 180min.

[0178] The crude product is input into a continuous post-processing device, and the continuous post-processing device is controlled to continuously post-process the crude product system to obtain a reaction product;

[0179] The crude product is transported to a continuous acidification unit for continuous acidification to obtain an acid washing product system;

[0180] Controlling the acid in the acid storage tank and the crude product in the continuous condensation reaction device to be transported to the second continuous mixing tank at a second preset flow rate, and acidifying under a fourth preset condition to obtain an acid washing product system;

[0181] wherein the flow rate of the acid solution is 12 to 20 g / min; and / or,

[0182] The type of the acid is any one of hydrochloric acid, sulfuric acid and acetic acid; and / or the concentration of the acid is 5% to 15%;

[0183] The fourth preset condition is that the acidification temperature is 40° C. to 80° C., and the acidification residence time is 10 min to 60 min.

[0184] The pickling product system is controlled to be transported to the first continuous liquid separation component at a first feed rate, and is continuously separated at a first liquid separation temperature to obtain a first heavy phase and a first light phase; wherein the first liquid separation temperature is 40°C to 80°C.

[0185] The acid-washed product system is transported to a continuous alkalization unit for continuous alkalization to obtain an alkali-washed product system;

[0186] Controlling the alkali liquid in the alkali liquid storage tank to enter the third continuous mixing tank at a second feed rate, conveying the first light phase to the third continuous mixing tank at a second feed rate, and continuously alkali-washing with the alkali liquid under a fifth preset condition to obtain an alkali-washed product system;

[0187] Wherein, the alkali solution is any one of sodium carbonate, sodium bicarbonate, ammonium bicarbonate or a combination of several thereof; and / or,

[0188] The concentration of the alkali solution is 5% to 25%; the fifth preset condition is that the alkali washing time is 10 min to 60 min, and the alkali washing temperature is 40° C. to 80° C.; and / or,

[0189] The alkali washing product system is controlled to be transported to the second continuous liquid separation component at a third feed rate, and continuous liquid separation is performed under a sixth preset condition to obtain a second heavy phase and a second light phase; wherein the sixth preset condition is that the alkali washing liquid separation temperature is 40°C to 80°C.

[0190] The alkali-washed product system is transported to a continuous water-washing unit for continuous water-washing to obtain a water-washed product system;

[0191] Controlling the second light phase and the water in the water storage tank to be continuously transported to the fourth continuous mixing tank at a fourth feed rate, and continuously washing with water under a seventh preset condition to obtain a water-washed product system;

[0192] The second light phase is obtained by continuously separating the alkali-washed product system through the second continuous separation component, and the seventh preset condition is that the continuous water washing time is 10 minutes to 60 minutes, and the continuous water washing temperature is 40° C. to 80° C.;

[0193] The water-wash product system is controlled to be transported to the third continuous liquid separation component at the fifth feed rate, and is continuously separated under the eighth preset condition to obtain a third heavy phase and a third light phase; wherein the eighth preset condition is that the water-wash separation temperature is 40° C. to 80° C.

[0194] The water-washed product system is transported to a continuous crystallization unit for continuous crystallization to obtain a crystallized product system;

[0195] The crystallization product system is transported to a continuous filtration unit for continuous filtration to obtain a filtration product system;

[0196] The filtered product system is transported to a drying unit for continuous drying to obtain a reaction product.

[0197] Controlling the third light phase to be transported to the continuous crystallization tank at a sixth feed amount, and performing continuous crystallization under a ninth preset condition to obtain a crystallization product system;

[0198] The third light phase is a water-washed product system obtained by continuous separation by a third continuous separation component, and the ninth preset condition is that the continuous crystallization temperature is -10°C to 20°C, and the continuous crystallization time is 30min to 180min; and / or,

[0199] Controlling the crystallization product system to enter the continuous filtration tank at the sixth feed amount for continuous filtration to obtain a filtration product system; wherein the continuous filtration temperature is -10°C to 20°C; and / or,

[0200] Controlling the filtration product system to be transported to a continuous drying tank for continuous drying to obtain a reaction product;

[0201] The drying temperature is 40°C to 60°C, and the drying time is 30min to 90min.

[0202] The embodiments of the present application can more accurately control each process, including temperature, pressure and flow rate, by limiting the process conditions in each part, which helps to improve the quality of the generated fluopyraclostrobin. At the same time, in the continuous production process, the utilization rate of materials is higher, which reduces the material loss that may occur in batch reactions. Automated continuous production reduces manual intervention and reduces safety accidents caused by human errors. At the same time, continuous production is easier to scale up to meet the growth of market demand, reduces the generation of chemical waste, and helps to reduce the impact on the environment. Because each step in this process has limited reaction conditions, the quality of the produced products can be made more stable and reliable. By adjusting the parameters of each device, it can flexibly adapt to the production needs of different products.

[0203] Example 2

[0204]

[0205] 3',4',5'-trifluoro-2-aminobiphenyl is fed into the continuous batching tank 701 at a feeding rate of 10.0 g / min using the continuous solid feeder 101, and toluene is fed into the continuous batching tank 701 at a feeding rate of 26.0 g / min from the solvent storage tank 201, and the mixture is kept mixed at 50° C. for 20 min to obtain a raw material system containing 3',4',5'-trifluoro-2-aminobiphenyl, and the raw material system is temporarily stored in the liquid storage tank 301 at a feeding rate of 36.0 g / min, and kept warm at 50° C.;

[0206] The feed liquid in the liquid storage tank 301 was fed at a rate of 10.0 g / min, and pyridine was fed at a rate of 1.8 g / min, and 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride was fed at a rate of 2.5 g / min, respectively, and preheated through the corresponding 50° C. heat exchanger, and then entered the first continuous mixing tank 501 through the mixer, and stayed at 55° C. for 90 min; the system containing the condensation product (i.e., the crude product in the above embodiment) was fed at a rate of 14.3 g / min. The organic phase after separation by the first continuous liquid separation part 1101 is passed into the third continuous mixing tank 902 at a feed rate of 11.2 g / min, and sodium bicarbonate is fed into the second continuous mixing tank 901 at a feed rate of 20.0 g / min, and acidified at 70°C for 30 min; the obtained system is fed into the first continuous liquid separation part 1101 for separation at a feed rate of 34.3 g / min; the organic phase after separation by the first continuous liquid separation part 1101 is passed into the third continuous mixing tank 902 at a feed rate of 11.2 g / min, and sodium bicarbonate is fed into the second continuous mixing tank 901 at a feed rate of 20.0 g / min. The feed rate of 10.1 g / min was passed into the third continuous mixing tank 902, and the alkali washing was carried out at 70°C for 30 min; the obtained system was fed into the second continuous liquid separation part 1102 for liquid separation at a feed rate of 31.2 g / min; the organic phase after liquid separation by the second continuous liquid separation part 1102 was fed into the fourth continuous mixing tank 903 at a feed rate of 10.1 g / min, and purified water was fed into the fourth continuous mixing tank 903 at a feed rate of 20 g / min, and the alkali washing was carried out at 70°C for 30 min; the obtained system was fed into the second continuous liquid separation part 1102 for liquid separation at a feed rate of 31.2 g / min; the organic phase after liquid separation by the second continuous liquid separation part 1102 was fed into the fourth continuous mixing tank 903 at a feed rate of 10.1 g / min, and the ...; the purified water was fed into the g / min into the third continuous liquid separation component 1103 for separation; after separation by the third continuous liquid separation component 1103, the organic phase enters the continuous crystallization tank 1001 at a feed rate of 9.6 g / min and stays at 10°C for 60 min; the precipitated solid overflows into the continuous filtration tank 1401 at a feed rate of 4.75 g / min, the temperature of the continuous filtration tank 1401 is set to 50°C, and fluopyram is obtained after staying for 30 min; the yield of fluopyram is measured to be 92%.

[0207] Example 3

[0208] 3',4',5'-trifluoro-2-aminobiphenyl is fed into the continuous batching tank 701 at a feeding rate of 15.0 g / min using the continuous solid feeder 101, and toluene is fed into the continuous batching tank 701 at a feeding rate of 39.0 g / min from the solvent storage tank 201, and the mixture is kept at 50° C. for 20 min, and the raw material system containing 3',4',5'-trifluoro-2-aminobiphenyl is fed into the liquid storage tank 301 at a feeding rate of 54.0 g / min for temporary storage and kept at 50° C.;

[0209] The feed liquid in the liquid storage tank 301 was fed at a rate of 15.0 g / min, and pyridine was fed at a rate of 2.7 g / min, and 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride was fed at a rate of 2.5 g / min. The feed liquid was preheated through the corresponding 50°C heat exchanger and then passed through the mixer to enter the first continuous mixing tank 501, where it remained at 55°C for 60 min. The system containing the condensation product (i.e., the crude product) was fed to the second continuous mixing tank 501 at a rate of 21.5 g / min. The continuous mixing tank 901 was filled with 5% hydrochloric acid aqueous solution at a feeding rate of 30.0 g / min, and acidified at 70°C for 30 min; the obtained system was fed into the first continuous liquid separation part 1101 for liquid separation at a feeding rate of 51.5 g / min; the organic phase after liquid separation in the first continuous liquid separation part 1101 was fed into the third continuous mixing tank 902 at a feeding rate of 16.8 g / min, and sodium bicarbonate was fed into the third continuous mixing tank 902 at a feeding rate of 30.0 g / min. The obtained system was fed into the third continuous mixing tank 902 and washed with alkali at 70°C for 30 minutes; the obtained system was fed into the second continuous liquid separation part 1102 for separation at a feed rate of 46.8 g / min; the organic phase after separation by the second continuous liquid separation part 1102 was fed into the fourth continuous mixing tank 903 at a feed rate of 15.2 g / min, and purified water was fed into the fourth continuous mixing tank 903 at a feed rate of 30 g / min, and washed with water at 70°C for 30 minutes; the obtained system was fed into the second continuous liquid separation part 1102 at a feed rate of 45.2 g / min The organic phase enters the continuous crystallization tank 1001 at a feed rate of 14.4 g / min for separation by the third continuous liquid separation part 1103; after separation by the third continuous liquid separation part 1103, the organic phase enters the continuous crystallization tank 1001 at a feed rate of 14.4 g / min and stays at 10°C for 60 min; the precipitated solid overflows into the continuous filtration tank 1401 at a feed rate of 7.05 g / min, the temperature of the continuous filtration tank 1401 is set to 50°C, and after staying for 30 min, fluopyrabendazole is obtained; the yield of fluopyrabendazole is measured to be 91.06%.

[0210] Example 4

[0211] The condensation reaction time was screened and tested on the basis of Example 2 and reduced to 30 min. Other reaction conditions remained unchanged, and the yield of fluopyrabendazole was measured to be 81.6%.

[0212] Example 5

[0213] The condensation reaction time was screened and tested on the basis of Example 2, and the reaction time was extended to 180 min. Other reaction conditions remained unchanged, and the yield of fluopyrabendazole was measured to be 89.9%.

[0214] Example 6

[0215] Based on the reaction conditions of Example 2, pyridine was replaced with triethylamine and N,N-diisopropylethylamine for base type screening test. The yield of flupyraclostrobin was 88.7% using triethylamine, and the yield of flupyraclostrobin was 85.4% using N,N-diisopropylethylamine. The type of base has a certain influence on the reaction, and pyridine is preferred.

[0216] It should be noted that the terms used herein are only for describing specific embodiments and are not intended to limit the exemplary embodiments according to the present application. As used herein, unless the context clearly indicates otherwise, the singular form is also intended to include the plural form. In addition, it should be understood that when the terms "comprise" and / or "include" are used in this specification, it indicates the presence of features, steps, operations, devices, components and / or combinations thereof.

[0217] Unless otherwise specifically stated, the relative arrangement of the parts and steps described in these embodiments, numerical expressions and numerical values ​​do not limit the scope of the present invention. At the same time, it should be understood that, for ease of description, the sizes of the various parts shown in the accompanying drawings are not drawn according to the actual proportional relationship. The technology, method and equipment known to ordinary technicians in the relevant field may not be discussed in detail, but in appropriate cases, the technology, method and equipment should be regarded as a part of the authorization specification. In all examples shown and discussed here, any specific value should be interpreted as being merely exemplary, rather than as a limitation. Therefore, other examples of exemplary embodiments may have different values. It should be noted that similar reference numerals and letters represent similar items in the following drawings, so once a certain item is defined in an accompanying drawing, it does not need to be further discussed in subsequent drawings.

[0218] In the description of the present invention, it is necessary to understand that the directions or positional relationships indicated by directional words such as "front, back, up, down, left, right", "lateral, vertical, perpendicular, horizontal" and "top, bottom" are usually based on the directions or positional relationships shown in the drawings. They are only for the convenience of describing the present invention and simplifying the description. Unless otherwise specified, these directional words do not indicate or imply that the devices or elements referred to must have a specific direction or be constructed and operated in a specific direction. Therefore, they cannot be understood as limiting the scope of protection of the present invention. The directional words "inside and outside" refer to the inside and outside relative to the contours of each component itself.

[0219] For ease of description, spatially relative terms such as "above", "above", "on the upper surface of", "above", etc. may be used here to describe the spatial positional relationship between a device or feature and other devices or features as shown in the figure. It should be understood that spatially relative terms are intended to include different orientations of the device in use or operation in addition to the orientation described in the figure. For example, if the device in the accompanying drawings is inverted, the device described as "above other devices or structures" or "above other devices or structures" will be positioned as "below other devices or structures" or "below other devices or structures". Thus, the exemplary term "above" can include both "above" and "below". The device can also be positioned in other different ways (rotated 90 degrees or in other orientations), and the spatially relative descriptions used here are interpreted accordingly.

[0220] In addition, it should be noted that the use of terms such as "first" and "second" to limit components is only for the convenience of distinguishing the corresponding components. If not otherwise stated, the above terms have no special meaning and therefore cannot be understood as limiting the scope of protection of the present invention.

[0221] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A method for preparing fluopyraclostrobin, characterized in that: The method for preparing fluopyrabamide is applied to a fluopyrabamide production device, and is characterized in that the fluopyrabamide production device comprises: A continuous condensation reaction device (601), wherein the continuous condensation reaction device (601) is used to provide a continuous condensation reaction site for preparing fluopyraclostrobin; A continuous dosing device, the continuous dosing device being connected to the continuous condensation reaction device (601) to continuously provide the 3',4',5'-trifluoro-2-aminobiphenyl solution as a first reaction raw material to the continuous condensation reaction device (601); a first raw material supply device, the first raw material supply device being connected to the continuous condensation reaction device (601) to continuously supply pyridine and 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride as second reaction raw materials to the continuous condensation reaction device (601); A continuous post-processing device, the continuous post-processing device being connected to the continuous condensation reaction device (601) to continuously post-process the crude product obtained by the continuous condensation reaction device (601) to obtain a reaction product; The first reaction raw material and the second reaction raw material undergo a continuous condensation reaction in the continuous condensation reaction site to obtain the crude product; The preparation method comprises: controlling the continuous batching device to continuously deliver the 3',4',5'-trifluoro-2-aminobiphenyl solution to the continuous condensation reaction device, and controlling the first raw material supply device to continuously deliver the pyridine and the 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride to the continuous condensation reaction device, wherein the 3',4',5'-trifluoro-2-aminobiphenyl solution reacts with the pyridine and the 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride in the continuous condensation reaction device to obtain a crude product; The crude product is input into the continuous post-processing device to control the continuous post-processing device to continuously post-process the crude product system to obtain a reaction product.

2. The method for preparing fluopyraclostrobin according to claim 1, characterized in that: The continuous post-processing device comprises: A continuous acidification unit, the continuous acidification unit being connected to the continuous condensation reaction device (601) to continuously acidify the crude product to obtain an acid-washed product system; A continuous alkalization unit is connected to the continuous acidification unit to continuously perform alkali washing on the acid-washed product system to obtain an alkali-washed product system.

3. The method for preparing fluopyraclostrobin according to claim 2, characterized in that: The continuous post-processing device also includes: A continuous water washing unit, wherein the continuous water washing unit is connected to the continuous alkalization unit to continuously wash the alkali-washed product system with water to obtain a water-washed product system; a continuous crystallization unit, the continuous crystallization unit being connected to the continuous water washing unit to continuously crystallize the water washing product system to obtain a crystallization product system; a continuous filtration unit, the continuous filtration unit being connected to the continuous crystallization unit to continuously filter the crystallization product system to obtain a filtration product system; A drying unit is connected to the continuous filtering unit to dry the filtered product system to obtain the reaction product.

4. The method for preparing fluopyraclostrobin according to claim 2, characterized in that: The continuous batching device comprises: Continuous batching tank (701); A continuous solid feeder (101), the continuous solid feeder (101) being in communication with the continuous batching tank (701) so as to continuously deliver the 3',4',5'-trifluoro-2-aminobiphenyl solid stored therein to the continuous batching tank (701); A solvent storage tank (201), wherein the solvent storage tank (201) is connected to the continuous dosing tank (701) via a first pipeline, so that the solvent in the solvent storage tank (201) is continuously transported from the first pipeline to the continuous dosing tank (701), and continuously mixed with the 3',4',5'-trifluoro-2-aminobiphenyl solid in the continuous dosing tank (701), so as to obtain the 3',4',5'-trifluoro-2-aminobiphenyl solution; A liquid storage tank (301), wherein the inlet of the liquid storage tank (301) is connected to the continuous batching tank (701) to accommodate the 3',4',5'-trifluoro-2-aminobiphenyl solution transported from the continuous batching tank (701); and the outlet of the liquid storage tank (301) is connected to the continuous condensation reaction device (601).

5. The method for preparing fluopyraclostrobin according to claim 4, characterized in that: The continuous batching device also includes: A first liquid flow meter (1301), the first liquid flow meter (1301) being arranged on the first pipeline to detect the real-time flow rate of the liquid flowing through the first pipeline and to generate a corresponding detection result; A solvent feed pump (1201), wherein the solvent feed pump (1201) is disposed on the first pipeline, and the solvent feed pump (1201) is connected to the first liquid flow meter (1301) to control the flow rate of the solvent in the solvent storage tank (201) entering the continuous dosing tank (701) according to the detection result of the first liquid flow meter (1301).

6. The method for preparing fluopyraclostrobin according to claim 4, characterized in that: The continuous batching device also includes: A first heat exchanger (401), wherein the first heat exchanger (401) has a relatively independent first heat exchange channel and a second heat exchange channel, wherein the first heat exchange channel is used for circulating a preheating medium, and a port of the second heat exchange channel is connected to the outlet of the liquid storage tank (301) for performing heat exchange on the 3', 4', 5'-trifluoro-2-aminobiphenyl solution flowing out of the liquid storage tank (301) to increase the temperature of the 3', 4', 5'-trifluoro-2-aminobiphenyl solution.

7. The method for preparing fluopyraclostrobin according to claim 6, characterized in that: The first raw material supply device comprises: A first continuous mixing tank (501), the first continuous mixing tank (501) being connected to the continuous condensation reaction device (601) and another port of the second heat exchange channel respectively; a first raw material tank (202), wherein pyridine is stored in the first raw material tank (202), and the first raw material tank (202) is connected to the first continuous mixing tank (501) so as to transport the pyridine into the first continuous mixing tank (501); a second raw material tank (203), wherein 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride is stored in the second raw material tank (203), and the second raw material tank (203) is connected to the first continuous mixing tank (501) so as to continuously transport the 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride into the first continuous mixing tank (501); The pyridine, the 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride and the 3',4',5'-trifluoro-2-aminobiphenyl solution after heat exchange in the first heat exchanger (401) are continuously mixed in the first continuous mixing tank (501) to obtain a mixed product system, and the mixed product system is transported to the continuous condensation reaction device (601) to carry out the continuous condensation reaction to obtain the crude product.

8. The method for preparing fluopyraclostrobin according to claim 7, characterized in that: The continuous acidification unit comprises: a second heat exchanger (404), wherein the second heat exchanger (404) has a relatively independent third heat exchange channel and a fourth heat exchange channel, wherein the third heat exchange channel is used to circulate a cooling medium, and a port of the fourth heat exchange channel is connected to the continuous condensation reaction device (601) to perform heat exchange on the crude product from the continuous condensation reaction device (601) to reduce the temperature of the crude product; a second continuous mixing tank (901), wherein the second continuous mixing tank (901) is connected to another port of the fourth heat exchange channel, and the crude product after heat exchange in the second heat exchanger (404) enters the second continuous mixing tank (901); an outlet of the second continuous mixing tank (901) is connected to the continuous alkalization unit; An acid liquid storage tank (204), wherein acid liquid is stored in the acid liquid storage tank (204), and the acid liquid storage tank (204) is connected to the second continuous mixing tank (901) and is used to continuously transport acid liquid to the second continuous mixing tank (901) so as to continuously acidify the crude product in the second continuous mixing tank (901) after heat exchange in the second heat exchanger (404), so as to obtain the pickling product system.

9. The method for preparing fluopyraclostrobin according to claim 8, characterized in that: The pipeline connecting the outlet of the second continuous mixing tank (901) and the continuous alkalization unit is also provided with: A first continuous liquid separation component (1101) has a first heavy phase outlet and a first light phase outlet, and the acid washing product system enters the first continuous liquid separation component (1101) for continuous liquid separation to obtain a first heavy phase and a first light phase; the first light phase outlet is connected to the continuous alkalization unit; A first heavy phase collecting tank (801), wherein the first heavy phase collecting tank (801) is connected to the first heavy phase outlet and is used to collect the first heavy phase.

10. The method for preparing fluopyraclostrobin according to claim 3, characterized in that: The pickling product system is continuously separated by a first continuous separation component (1101) to obtain a first heavy phase and a first light phase. The continuous alkalization unit comprises: A third continuous mixing tank (902), wherein the inlet of the third continuous mixing tank (902) is connected to the continuous acidification unit through a third pipeline, the first light phase enters the third continuous mixing tank (902) from the third pipeline, and the outlet of the third continuous mixing tank (902) is connected to the continuous water washing unit; An alkali liquid storage tank (205) is provided with alkali liquid stored therein. The alkali liquid storage tank (205) is connected to the inlet of the third continuous mixing tank (902) via a fourth pipeline, and is used for continuously conveying alkali liquid to the third continuous mixing tank (902) to continuously alkali wash the first light phase in the alkali liquid storage tank (205) to obtain the alkali washing product system.

11. The method for preparing fluopyraclostrobin according to claim 10, characterized in that: The pipeline between the outlet of the third continuous mixing tank (902) and the continuous water washing unit is also provided with: The second continuous liquid separation component (1102) has a second heavy phase outlet and a second light phase outlet. The alkali washing product system enters the second continuous liquid separation component (1102) for continuous liquid separation to obtain a second heavy phase and a second light phase. The second light phase outlet is connected to the continuous water washing unit. A second heavy phase collecting tank (802), wherein the second heavy phase collecting tank (802) is connected to the second heavy phase outlet and is used for collecting the second heavy phase.

12. The method for preparing fluopyraclostrobin according to claim 3, characterized in that: The alkali washing product system is separated by the second continuous separation component (1102) to obtain a second heavy phase and a second light phase. The continuous water washing unit comprises: a fourth continuous mixing tank (903), wherein the inlet of the fourth continuous mixing tank (903) is connected to the continuous alkalization unit via a fifth pipeline, the second light phase enters the fourth continuous mixing tank (903) from the fifth pipeline, and the outlet of the fourth continuous mixing tank (903) is connected to the continuous crystallization unit; A water storage tank (206), wherein water is stored in the water storage tank (206), and the outlet of the water storage tank (206) is connected to the inlet of the fourth continuous mixing tank (903), and is used to continuously transport water to the fourth continuous mixing tank (903) to continuously wash the second light phase in the fourth continuous mixing tank (903) with water to obtain the water-washed product system.

13. The method for preparing fluopyraclostrobin according to claim 12, characterized in that: The pipeline between the outlet of the fourth continuous mixing tank (903) and the continuous crystallization unit is also provided with: A third continuous liquid separation component (1103) has a third heavy phase outlet and a third light phase outlet, the water-washed product system enters the third continuous liquid separation component (1103) for continuous liquid separation to obtain a third heavy phase and a third light phase, and the third light phase outlet is connected to the continuous crystallization unit; A third heavy phase collecting tank (803), the third heavy phase collecting tank (803) is connected to the third heavy phase outlet, and is used to collect the third heavy phase.

14. The method for preparing fluopyraclostrobin according to claim 3, characterized in that: The water-washed product system is continuously separated by a third continuous separation component (1103) to obtain a third heavy phase and a third light phase. The continuous crystallization unit comprises: A continuous crystallization tank (1001), wherein the inlet of the continuous crystallization tank (1001) is connected to the continuous water washing unit to continuously crystallize the third light phase to obtain the crystallization product system.

15. The method for preparing fluopyraclostrobin according to claim 3, characterized in that: The continuous filtration unit comprises: A continuous filtration tank (1401), wherein the inlet of the continuous filtration tank (1401) is connected to the continuous crystallization unit to continuously filter the crystallization product system to obtain the filtered product system.

16. The method for preparing fluopyraclostrobin according to claim 3, characterized in that: The drying unit comprises: A continuous drying tank (1501), wherein the inlet of the continuous drying tank (1501) is connected to the continuous filtering unit so as to continuously dry the filtered product system to obtain the reaction product.

17. The method for preparing fluopyraclostrobin according to claim 16, characterized in that: The preparation method further comprises: The crude product is transported to a continuous acidification unit for continuous acidification to obtain an acid washing product system; The acid-washed product system is transported to a continuous alkalization unit for continuous alkalization to obtain an alkali-washed product system; The alkali-washed product system is transported to a continuous water-washing unit for continuous water-washing to obtain a water-washed product system; The water-washed product system is transported to a continuous crystallization unit for continuous crystallization to obtain a crystallized product system; transporting the crystallization product system to a continuous filtration unit for continuous filtration to obtain a filtration product system; The filtered product system is transported to a drying unit for continuous drying to obtain the reaction product.

18. The method for preparing fluopyraclostrobin according to claim 16, characterized in that: The preparation method further comprises: Controlling a continuous solid feeder and a solvent storage tank to continuously deliver 3', 4', 5'-trifluoro-2-aminobiphenyl solid and solvent to a continuous batching tank at a first preset flow rate, and continuously batching in the continuous batching tank under a first preset condition to obtain the 3', 4', 5'-trifluoro-2-aminobiphenyl solution, and delivering the 3', 4', 5'-trifluoro-2-aminobiphenyl solution to a liquid storage tank; Among them, the first preset condition is that the reaction temperature of continuous batching is 30°C to 50°C, the reaction time of continuous batching is 10min to 90min, the amount of the solvent is 1g / 1-5ml, and the solvent is any one or more of toluene, xylene, ethyl acetate, and dichloroethane.

19. The method for preparing fluopyraclostrobin according to claim 18, characterized in that: The preparation method further comprises: Controlling the 3',4',5'-trifluoro-2-aminobiphenyl solution, the pyridine in the first raw material tank, and the 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride in the second raw material tank after heat exchange in the first heat exchanger to be respectively transported to the first continuous mixing tank, and continuously mixed under the second preset condition to obtain a mixed product system; The mixed product system is transported to a continuous condensation reaction device at the first preset flow rate, and a continuous condensation reaction occurs under a third preset condition to obtain a continuous condensation reaction system; Among them, the second preset condition is that the first mixing temperature is 50°C to 80°C, and the first continuous mixing time is 1min to 10min, and the third preset condition is that the condensation reaction time in the continuous condensation reaction device is 30min to 180min.

20. The method for preparing fluopyraclostrobin according to claim 16, characterized in that: The preparation method further comprises: Controlling the acid in the acid storage tank and the crude product in the continuous condensation reaction device to be transported to the second continuous mixing tank at a second preset flow rate, and acidifying under a fourth preset condition to obtain an acid washing product system; Wherein, the flow rate of the acid solution is 12 to 20 g / min; and / or, The acid solution is any one of hydrochloric acid, sulfuric acid and acetic acid; and / or, The concentration of the acid solution is 5% to 15%; The fourth preset condition is that the acidification temperature is 40° C. to 80° C., and the acidification residence time is 10 min to 60 min.

21. The method for preparing fluopyraclostrobin according to claim 17, characterized in that: The preparation method further comprises: Controlling the pickling product system to be transported to a first continuous liquid separation component at a first feed rate, and performing continuous liquid separation at a first liquid separation temperature to obtain a first heavy phase and a first light phase; Wherein, the first liquid separation temperature is 40°C to 80°C.

22. The method for preparing fluopyraclostrobin according to claim 21, characterized in that: The preparation method further comprises: Controlling the alkali liquid in the alkali liquid storage tank to enter the third continuous mixing tank at a second feed rate, conveying the first light phase to the third continuous mixing tank at a second feed rate, and continuously alkali-washing with the alkali liquid under a fifth preset condition to obtain an alkali-washed product system; Wherein, the alkali solution is any one of sodium carbonate, sodium bicarbonate, ammonium bicarbonate or a combination of several thereof; and / or, The concentration of the alkali solution is 5% to 25%; The fifth preset condition is that the alkali washing time is 10 minutes to 60 minutes, and the alkali washing temperature is 40° C. to 80° C.; and / or, Controlling the alkali-wash product system to be transported to the second continuous liquid separation component at a third feed rate, and performing continuous liquid separation under a sixth preset condition to obtain a second heavy phase and a second light phase; Among them, the sixth preset condition is that the alkaline washing separation temperature is 40°C to 80°C.

23. The method for preparing fluopyraclostrobin according to claim 17, characterized in that: The preparation method further comprises: Controlling the second light phase and the water in the water storage tank to be continuously transported to the fourth continuous mixing tank at a fourth feed rate, and continuously washing with water under a seventh preset condition to obtain a water-washed product system; The second light phase is obtained by continuously separating the alkali-washed product system through the second continuous separation component, and the seventh preset condition is that the continuous water washing time is 10 minutes to 60 minutes, and the continuous water washing temperature is 40° C. to 80° C.; Controlling the water-wash product system to be transported to the third continuous liquid separation component at a fifth feed amount, and continuously liquid separation under an eighth preset condition to obtain a third heavy phase and a third light phase; Among them, the eighth preset condition is that the water washing and liquid separation temperature is 40°C to 80°C.

24. The method for preparing fluopyraclostrobin according to claim 17, characterized in that: The preparation method further comprises: Controlling the third light phase to be transported to the continuous crystallization tank at a sixth feed amount, and performing continuous crystallization under a ninth preset condition to obtain a crystallization product system; Wherein, the third light phase is obtained by continuous separation of the water-washed product system by the third continuous separation component, and the ninth preset condition is that the continuous crystallization temperature is -10°C to 20°C, and the continuous crystallization time is 30min to 180min; and / or, Controlling the crystallization product system to enter the continuous filtration tank with the sixth feed amount for continuous filtration to obtain a filtration product system; Wherein, the continuous filtration temperature is -10°C to 20°C; and / or, Controlling the filtered product system to be transported to a continuous drying tank for continuous drying to obtain the reaction product; The drying temperature is 40°C to 60°C, and the drying time is 30min to 90min.

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