Continuous production equipment and production method of 3, 4, 5-trifluorobromobenzene

Abstract

The invention provides continuous production equipment and a production method of 3, 4, 5-trifluorobromobenzene, the continuous production equipment comprises a continuous feeding device, the continuous feeding device is used for continuously supplying a first reaction raw material and a second reaction raw material, the first reaction raw material is o-dichlorobenzene, and the second reaction raw material is chlorosulfonic acid; an inlet of the continuous sulfonation reaction tank is communicated with an outlet of the continuous feeding device, and the continuous sulfonation reaction tank is used for providing a reaction place for a continuous sulfonation reaction of the first reaction raw material and the second reaction raw material so as to obtain a continuous sulfonation product; an inlet of the continuous post-treatment device is communicated with an outlet of the continuous sulfonation reaction tank, so that continuous post-treatment is performed on the continuous sulfonation product, 3, 4, 5-trifluorobromobenzene is obtained, and the problems caused by batch reaction in the prior art are solved.

Description

Technical Field

[0001] The invention relates to the technical field of trifluorobromobenzene production, and in particular to a continuous production device and a production method for 3,4,5-trifluorobromobenzene. Background Art

[0002] 3,4,5-Trifluorobromobenzene is an important pesticide intermediate, mainly used in the synthesis of the succinate dehydrogenase inhibitor fungicide fluopicolide.

[0003] The existing production of 3,4,5-trifluorobromobenzene generally uses a reactor for batch reaction, which requires a lot of manual operation, such as manual material transfer, which not only takes a long reaction time but also has low production efficiency. At the same time, the mass transfer and heat transfer effects are poor during the batch reaction, the utilization rate of raw materials is low, and there are many by-products, resulting in an unstable final yield of 3,4,5-trifluorobromobenzene. Summary of the invention

[0004] The main purpose of the present invention is to provide a continuous production device and a production method for 3,4,5-trifluorobromobenzene, so as to solve the problems of low production efficiency caused by batch reaction, poor mass and heat transfer effect, low raw material utilization rate and a large number of by-products in the prior art.

[0005] In order to achieve the above object, according to one aspect of the present invention, a continuous production device of 3,4,5-trifluorobromobenzene is provided, comprising: a continuous feeding device, the continuous feeding device is used to continuously supply a first reaction raw material and a second reaction raw material, the first reaction raw material is o-dichlorobenzene, and the second reaction raw material is chlorosulfonic acid;

[0006] A continuous sulfonation reaction tank, the inlet of which is connected to the outlet of the continuous feeding device, for providing a reaction place for the first reaction raw material and the second reaction raw material to carry out a continuous sulfonation reaction to obtain a continuous sulfonation product;

[0007] The inlet of the continuous post-treatment device is connected with the outlet of the continuous sulfonation reaction tank to continuously post-treat the continuous sulfonation product and obtain 3,4,5-trifluorobromobenzene.

[0008] Further, the continuous feeding device comprises: a first raw material tank, the outlet of the first raw material tank is connected to the inlet of the continuous sulfonation reaction tank, so as to continuously transport the first reaction raw material stored therein to the continuous sulfonation reaction tank;

[0009] The second raw material tank has an outlet connected to the inlet of the continuous sulfonation reaction tank, so as to continuously transport the second reaction raw material stored in the second raw material tank to the continuous sulfonation reaction tank.

[0010] Further, the continuous post-treatment device comprises: a continuous nitration unit, the inlet of the continuous nitration unit is connected to the outlet of the continuous sulfonation reaction tank to continuously nitrate the continuous sulfonation product and obtain a continuous nitration product;

[0011] A continuous esterification unit, wherein the inlet of the continuous esterification unit is connected to the outlet of the continuous nitration unit to continuously esterify the continuous nitration product and obtain a continuous esterification product;

[0012] A continuous chlorine-based fluorination unit, wherein the inlet of the continuous chlorine-based fluorination unit is connected to the outlet of the continuous esterification unit to continuously chlorine-based fluorination the continuous esterification product and obtain a continuous chlorine-based fluorination product;

[0013] A continuous bromination unit, wherein the inlet of the continuous bromination unit is connected to the outlet of the continuous chloro-fluorination unit to continuously bromine the continuous chloro-fluorination product and obtain a continuous bromination product;

[0014] A continuous diazotization unit, wherein the inlet of the continuous diazotization unit is connected to the outlet of the continuous bromination unit to continuously diazotize the continuous bromination products and obtain continuous diazotization products;

[0015] The inlet of the continuous fluorination unit is connected to the outlet of the continuous diazotization unit to continuously fluorinate the continuous diazotization product and obtain 3,4,5-trifluorobromobenzene.

[0016] Furthermore, the continuous nitration unit comprises: a continuous water washing component, the inlet of which is connected to the continuous sulfonation reaction tank to continuously wash the continuous sulfonation product with water to obtain a continuous water washing product;

[0017] a first continuous liquid separation component, wherein the inlet of the first continuous liquid separation component is connected to the outlet of the continuous water washing component, so as to continuously separate the continuous water washing product system and obtain a first organic phase;

[0018] A continuous nitration component, which is used to provide a continuous nitration reaction site, and the inlet end of the continuous nitration component is connected to the outlet end of the first continuous liquid separation component;

[0019] The first acid storage tank, the outlet of the first acid storage tank is connected with the inlet end of the continuous nitration component to transport the first acid solution into the continuous nitration component and mix it with the first organic phase in the continuous nitration component to obtain a continuous nitration product; the outlet of the continuous nitration component is connected with the continuous esterification unit.

[0020] Further, the continuous esterification unit comprises: a third raw material tank, wherein the third raw material tank is used to store a quenching agent;

[0021] A first continuous quenching component, wherein the inlet of the first continuous quenching component is connected to the outlet of the third raw material tank and the outlet of the continuous nitration unit, respectively, so as to continuously quench the continuous nitration product with a quenching agent to obtain a continuous quenching product;

[0022] a first continuous filtering component, wherein the inlet of the first continuous filtering component is connected to the outlet of the first continuous quenching component to continuously filter the continuous quenching product to obtain a continuous filtering product;

[0023] A first continuous dosing component, wherein the inlet of the first continuous dosing component is connected to the outlet of the first continuous filtering component to provide a continuous dosing reaction site for the continuous filtering product;

[0024] a first solvent storage tank, wherein the outlet of the first solvent storage tank is connected to the first continuous dosing component, so as to continuously dosing with the continuously filtered product in the first continuous dosing component and obtain a first continuous dosing product, and the first continuous dosing product is transported to the first liquid storage tank connected to the outlet end of the first continuous dosing component for temporary storage;

[0025] A continuous esterification component, wherein the outlet of the first liquid storage tank is connected to the inlet of the continuous esterification component to transport the first continuous batching product into the continuous esterification component;

[0026] The first solid feeder has an outlet connected to the inlet of the continuous esterification component to transport the first solid additive into the continuous esterification component so that the first solid additive is mixed with the first continuous batching product to carry out continuous esterification to obtain a continuous esterification product. The outlet of the continuous esterification component is connected to the continuous chlorine-based fluorination unit.

[0027] Further, the continuous chlorine-based fluorination unit comprises: a second continuous filtering component, the inlet of the second continuous filtering component is connected to the continuous esterification unit to continuously filter the continuous esterification product to obtain a second continuous filtered product;

[0028] a first continuous concentrating component, wherein the inlet of the first continuous concentrating component is connected to the outlet of the second continuous filtering component to continuously concentrate the second continuous filtering product to obtain a first continuous concentrated product;

[0029] A second continuous dosing component, the inlet of which is connected to the outlet of the first continuous concentration component to provide a continuous dosing reaction site for the first continuous concentration product;

[0030] a dimethylformamide storage tank, wherein the outlet of the dimethylformamide storage tank is connected to the second continuous batching component, so that the dimethylformamide stored in the dimethylformamide storage tank is transported to the second continuous batching component and mixed with the first continuous concentrated product in the second continuous batching component to continuously batch to obtain a second continuous batching product, and the second continuous batching product is transported to a second liquid storage tank connected to the outlet of the second continuous batching component for storage;

[0031] A continuous chlorine-based fluorination component, the inlet of which is connected to the outlet of the second liquid storage tank to provide a continuous fluorination reaction site;

[0032] A second solid feeder, the outlet of which is connected to the continuous chlorine-based fluorination component, is used to transport the fluorinating agent and continuously mix it with the second continuous batching product to obtain a continuous chlorine-based fluorination product. The outlet of the continuous chlorine-based fluorination component is connected to the continuous bromination unit.

[0033] Further, the continuous bromination unit comprises: a second continuous concentrating component, the inlet of the second continuous concentrating component is connected to the outlet of the continuous chlorine-based fluorination unit to continuously concentrate the continuous chlorine-based fluorination product to obtain a second continuous concentrated product;

[0034] A continuous hydrolysis reaction component, the inlet of which is connected to the outlet of the second continuous concentration component to provide a continuous hydrolysis reaction site;

[0035] A water storage component, wherein the outlet of the water storage component is connected to the inlet of the continuous hydrolysis reaction component to transport water and mix it with the second continuous concentrated product in the continuous hydrolysis reaction component to perform continuous hydrolysis to obtain a continuous hydrolyzed product;

[0036] a first continuous distillation component, wherein the inlet of the first continuous distillation component is connected to the outlet of the continuous hydrolysis reaction component to continuously distill the continuous hydrolysis product to obtain a continuous distillation product;

[0037] A continuous bromination reaction component, the inlet of which is connected to the outlet of the first continuous distillation component, providing a continuous bromination reaction site;

[0038] a third solid feeder, wherein the outlet of the third solid feeder is connected to the inlet of the continuous bromination reaction unit to convey the brominating agent;

[0039] The outlet of the second acid storage tank is connected to the inlet of the continuous bromination reaction component to transport the second acid solution and mix it with the brominating agent and the continuous distillation product to carry out continuous bromination to obtain a continuous bromination product. The outlet of the continuous bromination reaction component is connected to the continuous diazotization unit.

[0040] Further, the continuous diazotization unit comprises: a continuous extraction component, the inlet of the continuous extraction component is connected to the outlet of the continuous bromination unit to continuously extract the continuous bromination product to obtain a second organic phase;

[0041] a third solvent storage tank, wherein the outlet of the third solvent storage tank is connected to a third continuous dosing component to transport the third solvent therein, the outlet of the continuous extraction component is connected to the inlet of the third continuous dosing component to transport the second organic phase and continuously dosing with the third solvent to obtain a third continuous dosing product, and the third continuous dosing product is transported to a third liquid storage tank connected to the outlet end of the third continuous dosing component for storage;

[0042] A continuous reduction component, the inlet of which is connected to the outlet of the third liquid storage tank, so as to continuously reduce the third continuous batching product to obtain a continuous reduction product;

[0043] a third continuous concentrating component, whose inlet end is connected to the outlet of the continuous reducing component to continuously concentrate the continuous reduction product to obtain a third continuous concentrated product;

[0044] a fourth continuous dosing component, the inlet end of which is connected to the outlet of the third continuous concentrating component to accommodate the third continuous concentrated product;

[0045] A third acid storage tank, whose outlet end is connected to the inlet of the fourth continuous batching component, is used to transport the third acid solution into the fourth continuous batching component and mix it with the third continuous concentrated product to continuously batch and obtain a third continuous batching product;

[0046] a continuous diazo component, the inlet end of which is connected to the outlet of the fourth continuous batching component, and is used to accommodate the third continuous batching product;

[0047] The outlet of the nitrosylsulfuric acid storage component is connected to the inlet of the continuous diazo component to continuously transport nitrosylsulfuric acid into the continuous diazo component and mix it with the third continuous batching product in the continuous diazo component to perform continuous diazotization to obtain a continuous diazotization product. The outlet of the continuous diazo component is connected to the continuous fluorination unit.

[0048] Further, the continuous fluorination unit comprises: a second continuous quenching component, the inlet of which is connected to the outlet of the continuous diazotization unit;

[0049] a urea containing component, the outlet of which is connected to the inlet of the second continuous quenching component, so as to continuously deliver urea to the second continuous quenching component and mix urea with the continuous diazotization product in the second continuous quenching component to perform continuous quenching to obtain a second quenched product system;

[0050] a fluorination reaction component, the inlet of which is connected to the outlet of the second continuous quenching component to accommodate the second quenching product system;

[0051] A hydrofluoric acid storage component, the outlet of which is connected to the inlet of the fluorination reaction component to continuously transport the hydrofluoric acid and mix it with the second quenched product system in the fluorination reaction component to obtain a first fluorination product;

[0052] The inlet end of the second continuous distillation component is connected with the outlet end of the fluorination reaction component to continuously flow the first fluorination product to obtain 3,4,5-trifluorobromobenzene, and the 3,4,5-trifluorobromobenzene is transported to a product tank for storage.

[0053] According to another aspect of the present invention, a continuous production method of 3,4,5-trifluorobromobenzene is provided. The continuous production method is applied to the above-mentioned continuous production equipment, and the continuous production method comprises:

[0054] Controlling o-dichlorobenzene to be continuously fed in a first feed amount and chlorosulfonic acid to be continuously fed in a second feed amount to a continuous sulfonation reaction tank, and performing a continuous sulfonation reaction under a first preset condition to obtain a continuous sulfonation product;

[0055] Controlling the continuous sulfonation product to be continuously transported to a continuous post-treatment device for continuous post-treatment to obtain 3,4,5-trifluorobromobenzene;

[0056] Among them, the first preset condition is that the first reaction temperature is 50℃~80℃, the sulfonation reaction time is 120min~130min, the first feed amount is 10g / min~30g / min, and the second feed amount is 1g~3g of chlorosulfonic acid added to every 1g of o-dichlorobenzene.

[0057] Furthermore, the continuous production method further comprises: controlling the continuous sulfonation product to be continuously transported to the continuous nitration unit for continuous esterification to obtain a continuous esterification product;

[0058] Controlling the continuous esterification product to be continuously delivered to the continuous chlorine-based fluorination unit for continuous chlorine-based fluorination to obtain a continuous chlorine-based fluorination product;

[0059] Controlling the continuous chloro-fluorination product to be continuously delivered to the continuous bromination unit for continuous bromination to obtain continuous bromination products;

[0060] Controlling the continuous bromination product to be continuously transported to the continuous diazotization unit to perform continuous diazotization and obtain continuous diazotization product;

[0061] The continuous diazotization product is controlled to be continuously transported to a continuous fluorination unit to perform continuous fluorination, and 3,4,5-trifluorobromobenzene is obtained.

[0062] Furthermore, the continuous production method further comprises: controlling the continuous sulfonation product to be delivered to the continuous water washing component at a third feed rate, continuously washing the continuous sulfonation product with water at a set water volume under a second preset condition, and obtaining a continuous water washing product;

[0063] Controlling the continuous water-washing product to enter the first continuous liquid separation component at a fourth feed rate to perform continuous liquid separation under a third preset condition, and obtaining a first organic phase;

[0064] Controlling the first organic phase to be delivered to the continuous nitration component at a fifth feed amount, and at the same time, controlling the first acid solution to be delivered to the continuous nitration component at a set acid solution amount, and performing continuous nitration under the action of the nitrating agent under a fourth preset condition to obtain a continuous nitration product;

[0065] The third feed rate is 15 g / min to 45 g / min, and the water volume is set to 0.5 ml to 1.5 ml of water per 1 g of the third feed rate; and / or

[0066] The second preset condition is that the water washing temperature is 5°C to 10°C and the water washing time is 10min to 30min; and / or,

[0067] The fourth feed rate is 20 g / min to 60 g / min; and / or,

[0068] The third preset condition is that the first continuous liquid separation temperature is 20°C to 40°C; and / or,

[0069] The first continuous separation time is 5min to 10min; and / or,

[0070] The fifth feed rate is 10 g / min to 15 g / min, and the amount of the acid solution is set to 30 g to 45 g of the first acid solution per 1 g of the third feed rate; and / or,

[0071] The nitrating agent is one or more of potassium nitrate, sodium nitrate and concentrated nitric acid; and / or,

[0072] The amount of the nitrating agent used is 0.8 g to 1.5 g per 1 g of the third feed amount; and / or,

[0073] The fourth preset condition is that the nitrification temperature is 0°C to 20°C and the nitrification time is 60min to 180min; and / or,

[0074] The first acid solution is concentrated sulfuric acid with a mass concentration of 81% to 98%.

[0075] Furthermore, the continuous production method further comprises: controlling the continuous nitration unit in the continuous post-treatment device to continuously nitrate the continuous sulfonation product to obtain a continuous nitration product, which is transported to the first continuous quenching component at a sixth feed amount, and continuously quenching the continuous nitration product under a fifth preset condition with a solvent having a set solvent amount, to obtain a continuous quenching product;

[0076] Controlling the continuous quenching product to be delivered to the first continuous filtering component at a seventh feed amount, and performing continuous filtering under a sixth preset condition to obtain a continuous filtering product;

[0077] Controlling the continuous filtration product to be delivered to the first continuous dosing component at an eighth feed rate, and controlling the first solvent in the first solvent storage tank to be delivered to the first continuous dosing component at a first set amount, performing continuous dosing under a sixth preset condition, and obtaining a first continuous dosing product;

[0078] Controlling the first continuous batching product to be delivered to the continuous esterification component at a feed rate of 30 g / min-80 g / min, and at the same time, controlling the first solid feeder to deliver the first solid additive to the continuous esterification component at a second set amount, and performing continuous esterification at a temperature of 40° C.-70° C. for an esterification time of 30 min-180 min to obtain a continuous esterification product;

[0079] Wherein, the sixth feed rate is 50 g / min to 120 g / min, and the amount of solvent is set to be 1 ml to 3 ml per 1 g of the sixth feed rate; and / or,

[0080] The solvent is one or more of tap water, purified water, and deionized water; and / or,

[0081] The fifth preset condition is that the temperature of the first continuous quenching is 5°C to 20°C, and the first continuous quenching time is 10min to 30min; and / or,

[0082] The seventh feed rate is 200 g / min to 420 g / min; and / or,

[0083] The sixth preset condition is that the first continuous filtration temperature is in the range of 10°C to 20°C, and the first continuous filtration time is 10min to 30min; and / or,

[0084] The eighth feed rate is 10 g / min to 15 g / min, the sixth preset condition is that the first continuous batching temperature is 20° C. to 50° C., the first continuous batching time is 10 min to 30 min, and the first set dosage is 2 ml to 5 ml of the first solvent added per 1 g of the eighth feed rate; and / or,

[0085] The second set dosage is 1.2 g to 3.5 g of the first solid additive added per 1 g of the first continuous batching product; and / or,

[0086] The first solid additive is any one or more of potassium carbonate, cesium carbonate and sodium carbonate.

[0087] Furthermore, the method further comprises: controlling the continuous esterification unit in the continuous post-treatment device to continuously esterify the continuous nitration product to obtain a continuous esterification product, and conveying the continuous esterification product to the second continuous filtering component at a feed rate of 50 g / min to 150 g / min, and continuously filtering under the conditions of a filtration temperature of 10° C. to 30° C. and a filtration time of 10 min to 30 min, and obtaining a second continuous filtration product;

[0088] Controlling the second continuous filtration product to be transported to the first continuous concentration component at a feed rate of 30 g / min to 80 g / min, and continuously concentrating under the conditions of a first concentration temperature of 40° C. to 60° C., a first concentration pressure of -0.06 MPa to -0.1 MPa, and a first concentration time of 30 min to 60 min, to obtain a first continuous concentrated product;

[0089] The first continuous concentrated product is controlled to be delivered to the second continuous batching component at a feed rate of 10 g / min to 15 g / min, and the second solvent in the dimethylformamide storage tank is controlled to be continuously batched at a temperature of 20° C. to 40° C. and a batching time of 10 min to 30 min at a third set amount to obtain a second continuous batching product;

[0090] Controlling the second continuous batching product to be delivered to the continuous chlorine-based fluorination component at a feed rate of 25 g / min to 80 g / min, and controlling the second solid feeder to continuously deliver the fluorinating agent to the continuous chlorine-based fluorination component at a fourth set amount, and continuously mixing under the condition of a fifth set amount of the catalyst to obtain a continuous chlorine-based fluorination product;

[0091] Wherein, the type of the second solvent is one or more of N,N-dimethylformamide and N,N-dimethylacetamide; and / or,

[0092] The type of fluorinating agent is one or more of potassium fluoride, sodium fluoride, and boron trifluoride; and / or,

[0093] The type of catalyst is one or more of tetraphenylphosphonium bromide and 4-bromobenzyltriphenylphosphonium bromide; and / or,

[0094] The third set dosage is 2 mL to 5 mL of dimethylformamide added per 1 g of the first continuous concentrated product; and / or,

[0095] The fourth set dosage is 0.15 g to 0.3 g of the fluorinating agent added per 1 g of the second continuous batching product; and / or,

[0096] The fifth set dosage is 0.1 g to 0.5 g of the catalyst added per 1 g of the second continuous batching product.

[0097] Furthermore, the method further comprises: controlling the continuous chlorine-based fluorination unit in the continuous post-treatment device to continuously chlorine-based fluorination the continuous esterification product to obtain a continuous chlorine-based fluorination product at a feed rate of 40 g / min to 100 g / min to be transported to a second continuous concentration component, and continuously concentrated at a concentration temperature of 90° C. to 140° C., a concentration pressure of -0.06 MPa to 0-0.1 MPa, and a concentration time of 30 min to 60 min to obtain a second continuous concentrated product;

[0098] Controlling the second continuous concentrated product to be delivered to the continuous hydrolysis reaction component at a feed rate of 20 g / min to 50 g / min, and controlling the water storage component to deliver a sixth set amount of water to the continuous hydrolysis reaction component, and performing continuous hydrolysis at a hydrolysis temperature of 10° C. to 50° C. and a hydrolysis time of 60 min to 180 min to obtain a continuous hydrolysis product;

[0099] Controlling the continuous hydrolysis product to be transported to the first continuous distillation component at a feed rate of 40 g / min to 100 g / min, and continuously distilling at a distillation temperature of 100° C. to 180° C. and a distillation pressure of -0.08 MPa to -0.1 MPa to obtain a continuous distillation product;

[0100] Controlling the continuous distillation product to be delivered to the continuous bromination reaction component at a feed rate of 3 g / min to 10 g / min, controlling the third solid feeder to continuously deliver the brominating agent to the continuous bromination reaction component at a seventh set amount, and controlling the second acid liquid in the second acid storage tank to be delivered to the continuous bromination reaction component at an eighth set amount, and performing continuous bromination under the conditions of a bromination temperature of 40° C. to 60° C. and a bromination time of 30 min to 90 min to obtain a continuous bromination product;

[0101] Wherein, the type of brominating agent is one or more of dibromohydantoin, bromine, and N-bromosuccinimide; and / or,

[0102] The sixth set dosage is 3 mL to 5 mL of water per 1 g of the second continuous concentrated product; and / or,

[0103] The seventh set dosage is that the dosage of the brominating agent added per 1 g of the second continuous concentrated product is 1 g to 2 g; and / or,

[0104] The eighth set dosage is 2-5 g of the second acid solution added per 1 g of the second continuous concentrated product; and / or,

[0105] The second acid solution is 81%~98% sulfuric acid.

[0106] Furthermore, the method further comprises: controlling the continuous bromination unit in the post-treatment device to continuously bromine the continuous chloro-fluorinated product to obtain the continuous bromination product, continuously conveying the continuous bromination product to the continuous extraction component at a feed rate of 15 g / min to 30 g / min, and continuously extracting at a temperature of 30° C. to 50° C. and a time of 15 min to 45 min to obtain a second organic phase;

[0107] The second organic phase is controlled to be fed at a rate of 5 g / min to 15 g / min, and the third solvent in the third solvent storage tank is continuously delivered to the third continuous batching component at a ninth set amount, and the batching is continuously performed at a temperature of 20° C. to 40° C. and a time of 10 min to 30 min to obtain a third continuous batching product;

[0108] Control the third continuous batching product to be delivered to the continuous reduction component at a feed rate of 40 g / min to 90 g / min, and carry out continuous reduction under the conditions of the reducing agent being the tenth set amount, the reduction temperature being 40° C. to 80° C., the pressure being 0.3 MPa to 1.0 MPa, and the time being 30 to 60 min to obtain a continuous reduction product;

[0109] Controlling the continuous reduction product to be transported to the third continuous concentration component at a feed rate of 40 g / min to 90 g / min, and continuously concentrating at a concentration temperature of 40° C. to 60° C. and a concentration pressure of -0.06 MPa to 0-0.1 MPa to obtain a third continuous concentrated product;

[0110] The third continuous concentrated product is controlled to be fed at a rate of 10 g / min to 15 g / min, and the third acid solution in the third acid storage tank is transported to the fourth continuous batching component at an eleventh set dosage, and the batching is continuously performed under the conditions of a reaction temperature of 0° C. to 20° C. and a residence time of 10 min to 20 min to obtain a third continuous batching product;

[0111] Controlling the third continuous batching product to be delivered to the continuous diazo component at a feed rate of 30 g / min to 75 g / min, and controlling the nitrosylsulfuric acid storage component to be delivered to the continuous diazo component at a twelfth set amount, so that the third continuous batching product is mixed with the nitrosylsulfuric acid, and a continuous diazotization reaction is carried out under the conditions of a reaction temperature of -20°C to 0°C and a reaction residence time of 30 min to 90 min to obtain a continuous diazotization product;

[0112] Wherein, the third solvent is one or more of ethanol, methanol, and isopropanol; and / or,

[0113] The type of reducing agent is one or more of Raney nickel, palladium carbon, and aluminum-nickel alloy catalyst; and / or,

[0114] The third acid solution is concentrated sulfuric acid with a concentration of 30% to 70%, and the concentration of nitrosylsulfuric acid is 30% to 50%; and / or,

[0115] The ninth set dosage is that the dosage of the third solvent added to 1g of the second organic phase is 3mL~5mL; and / or,

[0116] The tenth set dosage is that the dosage of the reducing agent added per 1g of the third continuous batching product is 0.05g~0.2g; and / or,

[0117] The eleventh setting amount is that the amount of the third acid solution added to 1g of the third continuous concentrated product is 5g-10g; and / or,

[0118] The twelfth set dosage is that the dosage of nitrosylsulfuric acid added per 1g of the third continuous batching product is 3g~5g.

[0119] Furthermore, the method further includes: controlling the continuous diazotization unit in the post-treatment device to continuously diazotize the continuous bromination product to obtain a continuous diazotization product at a feed rate of 150 / min~250 / min to be transported to the second continuous quenching component, and at the same time controlling the urea containing component to continuously transport the urea to the second continuous quenching component at a twelfth set amount, and continuously quenching at a quenching temperature of 10~20°C and a quenching residence time of 10min~30min to obtain a second quenching product system;

[0120] Controlling the second quenched product system to be delivered to the fluorination reaction component at a feed rate of 300 g / min to 600 g / min, and controlling the hydrofluoric acid storage component to continuously deliver hydrofluoric acid to the fluorination reaction component at a thirteenth set amount, and performing a continuous fluorination reaction under the conditions of a first catalyst, a reaction temperature of 40° C. to 80° C., and a reaction residence time of 30 min to 90 min to obtain a first fluorination product;

[0121] Controlling the first fluorination product to be delivered to the second continuous distillation component at a dosage of 200 g / min to 500 g / min, and continuously distilling at a second distillation temperature of 40° C. to 60° C. and a second distillation pressure of -0.08 MPa to -0.1 MPa to obtain 3,4,5-trifluorobromobenzene;

[0122] Wherein, the quenching temperature is 10°C to 20°C, and the concentration of hydrofluoric acid is 30% to 50%; and / or,

[0123] The first catalyst is one or more of cuprous oxide, cupric sulfate, and cupric oxide; and / or,

[0124] The amount of the first catalyst used is 0.005 g to 0.02 g per 1 g of the second quenched product system; and / or,

[0125] The twelfth set dosage is that the dosage of urea contained in 1g of the continuous diazotization product is 0.8g~1.6g; and / or,

[0126] The thirteenth setting dosage is that the amount of hydrofluoric acid added to every 1g of the second quenching product is 0.03g~0.1g.

[0127] By applying the technical solution of the present invention, by changing the traditional batch reaction into a continuous reaction, frequent manual operation and material transfer are avoided, and the frequency of personnel contact during the operation of highly dangerous chemicals is reduced, thereby significantly improving the safety of the production process. During the reaction process, since the reactions of each part are continuous, the heat loss during the reaction process is reduced, the energy required for cooling and heating is reduced, and the standing time of the material during the reaction process is reduced, which effectively reduces the overall energy consumption. The continuous reaction reduces the use of solvents, reduces the generation of wastewater, waste gas and solid waste, and is beneficial to environmental protection and reduces production costs. In addition, the use of continuous reaction devices avoids the "cleaning-loading-reaction-unloading-cleaning" cycle of traditional kettle reactions, increases the continuous operation time of the equipment, and thus improves equipment utilization. Continuous production reduces manual intervention and reduces dependence on operating skills, while also reducing the number of employees and labor costs. In the continuous production process, the continuous flow of raw materials and products reduces the storage time of materials, reduces the risk of material deterioration, and optimizes material management. The continuous reaction device can also adjust the reaction speed and scale according to production needs, which improves the flexibility of the production system and can quickly respond to market changes. Continuous production reduces the size of the reaction equipment to a certain extent and reduces equipment investment costs. At the same time, the reduced amount of solvent in the post-treatment process also helps to reduce production costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0128] 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:

[0129] Figure 1 A flow chart showing a continuous production device according to an embodiment of the present application;

[0130] Figure 2 Schematic diagram of the baffle provided in the embodiment of the present application being located in the continuous nitrification component.

[0131] The above drawings include the following reference numerals:

[0132] 301, first raw material tank; 302, second raw material tank; 303, water storage tank; 304, first acid storage tank; 401, continuous sulfonation reaction tank; 402, continuous water washing unit; 601, first continuous liquid separation unit; 403, continuous nitration unit; 305, third raw material tank; 404, first continuous quenching unit; 701, first continuous filtering unit; 306, first solvent storage tank; 405, first continuous batching unit; 307, first liquid storage tank; 406, continuous esterification unit; 702, second continuous filtering unit; 801, first continuous concentration unit; 308, dimethylformamide storage tank; 309, second liquid storage tank; 304, first acid storage tank; 503, first solid feeder; 505, second solid feeder machine; 408, continuous chlorine-based fluorination unit; 802, second continuous concentration unit; 310, water storage unit; 409, continuous hydrolysis reaction unit; 901, first continuous distillation unit; 410, continuous bromination reaction unit; 506, third solid feeder; 311, second acid storage tank; 1101, continuous extraction unit; 312, third solvent storage tank; 407, second continuous batching unit; 411, third continuous batching unit; 313, third liquid storage tank; 1001, continuous reduction unit; 803, third continuous concentration unit; 412, fourth continuous batching unit; 314, third acid storage tank; 413, continuous diazo unit; 315, nitrosylsulfuric acid storage unit; 414, second continuous quenching unit; 316, Urea containing part; 415, fluorination reaction part; 902, second continuous distillation part; 318, product tank; 201, first liquid flow meter; 202, second liquid flow meter; 101, o-dichlorobenzene feed pump; 102, chlorosulfonic acid feed pump; 103, first water feed pump; 203, third liquid flow meter; 104, second sulfuric acid feed pump; 204, fourth liquid flow meter; 105, first liquid feed pump; 205, fifth liquid flow meter; 502, fourth solid feeder; 106, second liquid feed pump; 206, sixth liquid flow meter; 107, third liquid feed pump; 207, seventh liquid flow meter; 504, fifth solid feeder; 108, fourth liquid feed pump; 208, eighth liquid flow meter meter; 109, fifth liquid feed pump; 209, ninth liquid flow meter; 110, sixth liquid feed pump; 210, tenth liquid flow meter; 111, first sulfuric acid feed pump; 211, eleventh liquid flow meter; 112, ethanol feed pump; 212, twelfth liquid flow meter; 113, seventh liquid feed pump; 213, twelfth liquid flow meter; 114, third sulfuric acid feed pump; 214, thirteenth liquid flow meter; 115, nitrosylsulfuric acid feed pump; 215, fourteenth liquid flow meter; 116, urea solution feed pump; 216, fifteenth liquid flow meter; 117, hydrofluoric acid feed pump; 217, sixteenth liquid flow meter; 317, hydrofluoric acid storage component; 501, nitrating agent solid feeder;4031, baffle. ; DETAILED DESCRIPTION

[0133] 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.

[0134] 3,4,5-Trifluorobromobenzene is an important pesticide intermediate, mainly used in the synthesis of the succinate dehydrogenase inhibitor fungicide fluopicolide.

[0135] The existing production of 3,4,5-trifluorobromobenzene generally uses a reactor for batch reaction, which requires a lot of manual operation, such as manual material transfer, which not only takes a long reaction time but also has low production efficiency. At the same time, the mass transfer and heat transfer effects are poor during the batch reaction, the utilization rate of raw materials is low, and there are many by-products, resulting in an unstable final yield of 3,4,5-trifluorobromobenzene.

[0136] Therefore, the purpose of this application is to provide a continuous production device and production method for 3,4,5-trifluorobromobenzene in view of the above problems.

[0137] First, the present application embodiment provides a 3,4,5-trifluorobromobenzene continuous production device, comprising:

[0138] A continuous feeding device, the continuous feeding device is used to continuously supply a first reaction raw material and a second reaction raw material, the first reaction raw material is o-dichlorobenzene, and the second reaction raw material is chlorosulfonic acid;

[0139] A continuous sulfonation reaction tank 401, the inlet of which is connected to the outlet of the continuous feeding device, for providing a reaction place for the first reaction raw material and the second reaction raw material to perform a continuous sulfonation reaction to obtain a continuous sulfonation product;

[0140] A continuous post-treatment device, the inlet of which is connected to the outlet of the continuous sulfonation reaction tank 401, so as to continuously post-treat the continuous sulfonation product and obtain 3,4,5-trifluorobromobenzene.

[0141] By continuously supplying o-dichlorobenzene and chlorosulfonic acid through a continuous feeding device and performing a continuous reaction in a continuous sulfonation reaction tank 401, the reaction time is significantly shortened, and the idle period of waiting for raw materials and interruption of the reaction in a batch reaction is avoided, thereby improving the efficiency of the entire production process. At the same time, the continuous reaction process makes the reaction conditions more stable. By accurately controlling the reaction temperature and the ratio of the reactants, the reaction yield and purity of 3,4,5-trifluorobromobenzene can be improved, while reducing the generation of by-products, thereby ensuring the stability of product quality. Exemplarily, the continuous sulfonation reaction tank 401 is one or more of a dynamic tubular reactor, a fully mixed flow reactor, and a plug flow reactor, so as to further improve the stability and efficiency of the continuous reaction.

[0142] The continuous sulfonation reaction tank 401 and the subsequent continuous post-treatment device avoid frequent manual operation and material transfer, reduce the frequency of human contact during the operation of highly dangerous chemicals, and thus significantly improve the safety of the production process. During the reaction process, the continuous reaction and post-treatment reduce heat loss, reduce the energy required for cooling and heating, and reduce the standing time of the material during the reaction process, effectively reducing the overall energy consumption. The continuous reaction reduces the use of solvents, reduces the generation of wastewater, waste gas and solid waste, is beneficial to environmental protection and reduces production costs. In addition, the use of the continuous reaction device avoids the "cleaning-loading-reaction-unloading-cleaning" of the traditional kettle reaction. The cycle process increases the continuous operation time of the equipment, thereby improving equipment utilization. Continuous production reduces manual intervention and reduces dependence on operating skills. It also reduces the number of employees and reduces labor costs. In the continuous production process, the continuous flow of raw materials and products reduces the storage time of materials, reduces the risk of material deterioration, and optimizes material management. The continuous reaction device can also adjust the reaction speed and scale according to production needs, which improves the flexibility of the production system and can respond quickly to market changes. Continuous production reduces the volume of reaction equipment to a certain extent and reduces equipment investment costs. At the same time, the reduced amount of solvent in the post-treatment process also helps to reduce production costs.

[0143] Furthermore, the continuous feeding device comprises:

[0144] A first raw material tank 301, wherein the outlet of the first raw material tank 301 is connected to the inlet of the continuous sulfonation reaction tank 401, so as to continuously transport the first reaction raw material stored therein to the continuous sulfonation reaction tank 401;

[0145] The second raw material tank 302 has an outlet connected to the inlet of the continuous sulfonation reaction tank 401 , so as to continuously transport the second reaction raw material stored therein to the continuous sulfonation reaction tank 401 .

[0146] An o-dichlorobenzene feeding pump 101 and a first liquid flow meter 201 are also provided on the pipeline between the first raw material tank 301 and the continuous sulfonation reaction tank 401. The flow of o-dichlorobenzene entering the continuous sulfonation reaction tank 401 can be monitored in real time by the first liquid flow meter 201, so that the opening size of the o-dichlorobenzene feeding pump 101 can be controlled to achieve control of the flow entering the continuous sulfonation reaction tank 401; a chlorosulfonic acid feeding pump 102 and a second liquid flow meter 202 are also provided on the pipeline between the second raw material tank 302 and the continuous sulfonation reaction tank 401. The flow of chlorosulfonic acid entering the continuous sulfonation reaction tank 401 can be monitored in real time by the second liquid flow meter 202, so that the opening size of the chlorosulfonic acid feeding pump 102 can be controlled.

[0147] By providing the first raw material tank 301 and the second raw material tank 302, continuous feeding can be achieved and the steps of repeatedly adding materials and waiting for the raw materials to react completely in traditional batch reactions can be avoided, thereby greatly shortening the production cycle and improving production efficiency. Through continuous raw material supply, the reaction feed rate and proportion can be more accurately controlled to ensure the consistency and accuracy of the reaction conditions, which is crucial to improving product purity and yield. In a continuous reaction, the material addition and reaction process can be carried out more smoothly, avoiding the violent heat release or pressure mutation caused by adding a large amount of reactants at one time, thereby reducing the safety risk in the reaction process. Since the material flow in the continuous reaction process is continuous , there is no need to equip a large-volume reactor like batch reactions to process a large amount of materials at one time, so the volume of the reaction device can be reduced and the equipment investment cost can be reduced. Continuous production can minimize manual operation and has a high degree of automation, which reduces the personal safety risk of operators and also reduces product quality problems caused by improper manual operation. The design of continuous reaction devices is usually easier to automate and maintain, and can achieve continuous monitoring and adjustment of reaction parameters to maintain optimal reaction conditions. In continuous reactions, the residence time of raw materials in the reactor can be precisely controlled, avoiding waste of raw materials due to incomplete or excessive reaction and improving the utilization rate of raw materials.

[0148] Furthermore, the continuous post-processing device comprises:

[0149] A continuous nitration unit, the inlet of which is connected to the outlet of the continuous sulfonation reaction tank 401, so as to continuously nitrate the continuous sulfonation product and obtain a continuous nitration product;

[0150] A continuous esterification unit, wherein the inlet of the continuous esterification unit is connected to the outlet of the continuous nitration unit to continuously esterify the continuous nitration product and obtain a continuous esterification product;

[0151] A continuous chlorine-based fluorination unit, wherein the inlet of the continuous chlorine-based fluorination unit is connected to the outlet of the continuous esterification unit to continuously chlorine-based fluorination the continuous esterification product and obtain a continuous chlorine-based fluorination product;

[0152] A continuous bromination unit, wherein the inlet of the continuous bromination unit is connected to the outlet of the continuous chloro-fluorination unit to continuously bromine the continuous chloro-fluorination product and obtain a continuous bromination product;

[0153] A continuous diazotization unit, wherein the inlet of the continuous diazotization unit is connected to the outlet of the continuous bromination unit to continuously diazotize the continuous bromination products and obtain continuous diazotization products;

[0154] The inlet of the continuous fluorination unit is connected to the outlet of the continuous diazotization unit to continuously fluorinate the continuous diazotization product and obtain 3,4,5-trifluorobromobenzene.

[0155] The continuous post-processing device includes the above multiple continuous units. This continuous production mode greatly shortens the reaction and post-processing time, avoids the static waiting and repeated transfer of materials in traditional batch reactions, and effectively improves the fluency and efficiency of the production process. In addition, continuous operation can more accurately control reaction conditions, such as temperature, pressure and material ratio, thereby improving the selectivity of the reaction and the utilization rate of raw materials, and ultimately improving the yield of the product. Through continuous batching and continuous reaction, especially in highly dangerous reaction steps such as chlorofluorination and fluorination, direct contact between on-site personnel and highly dangerous chemicals is avoided, significantly reducing operational risks. The continuous reactor can better control exothermic reactions, reduce heat accumulation, prevent the dangers that may be caused by sudden temperature increases, and ensure the safety of the production process. In the continuous post-processing process, the overall amount of solvent is reduced through optimized solvent use and recovery strategies, thereby reducing the amount of wastewater, waste gas and waste solids generated in the production process, and effectively controlling environmental impacts. At the same time, continuous production reduces the number of reused equipment and reduces equipment investment costs. It also improves yields and reduces the consumption of raw materials and energy, thereby reducing overall production costs. In continuous production, each step can be completed by automated equipment such as pumps, flow meters and PLC control systems, reducing human intervention. This not only improves the convenience and accuracy of operation, but also reduces the errors caused by human operation, ensuring the stability and consistency of product quality.

[0156] Further, the continuous nitrification unit comprises:

[0157] A continuous water washing component 402, the inlet of which is connected to the continuous sulfonation reaction tank 401, so as to continuously wash the continuous sulfonation product with water to obtain a continuous water washing product;

[0158] A first continuous liquid separation component 601, wherein the inlet of the first continuous liquid separation component 601 is connected to the outlet of the continuous water washing component 402, so as to continuously separate the continuous water washing product system and obtain a first organic phase;

[0159] A continuous nitration component 403, which is used to provide a continuous nitration reaction site, and the inlet end of the continuous nitration component 403 is connected to the outlet end of the first continuous liquid separation component 601;

[0160] The first acid storage tank 304, the outlet of the first acid storage tank 304 is connected to the inlet end of the continuous nitration component 403, so as to transport the first acid solution into the continuous nitration component 403 and mix it with the first organic phase in the continuous nitration component 403 to obtain a continuous nitration product; the outlet of the continuous nitration component 403 is connected to the continuous esterification unit.

[0161] The continuous water washing part 402 is one or more of a fully mixed reactor and a dynamic tubular reactor, the first continuous liquid separation part 601 is any one or more of a centrifugal extractor, a continuous extraction column, and a static liquid separator, and the continuous nitrification part 403 is one or more of a dynamic tubular reactor and a fully mixed reactor;

[0162] It also includes a water storage tank 303, the outlet end of the water storage tank 303 is connected to the first water feed pump 103, and the outlet end of the first water feed pump 103 is connected to a third liquid flow meter 203, and the flow rate of water entering the continuous sulfonation reaction tank 401 can be monitored in real time by the third liquid flow meter 203, so that the opening size of the first water feed pump 103 can be controlled in real time according to the detection result of the third liquid flow meter 203, and a second sulfuric acid feed pump 104 and a fourth liquid flow meter 204 are provided on the pipeline between the continuous nitration component 403 and the first acid storage tank 304, and the flow rate of the first acid solution entering the first acid storage tank 304 can be monitored in real time by the fourth liquid flow meter 204, so that the opening size of the second sulfuric acid feed pump 104 can be controlled in real time according to the detection result of the fourth liquid flow meter 204, and a nitrating agent solid feeder 501 is also provided, and the nitrating agent solid feeder 501 outputs The end is connected to the inlet end of the continuous nitrating component 403, which is used to continuously transport the solid nitrating reagent into the continuous nitrating component 403, wherein the nitrating reagent potassium nitrate in the continuous nitrating process of the present application is fed into the continuous nitrating component 403 in a solid manner to react with the continuous sulfonation product and the first acid solution. The process is a solid-liquid heterogeneous reaction. The solid feeding port of the solid nitrating reagent and the overflow port of the continuous nitrating product in the continuous nitrating component 403 are both located at the top of the continuous nitrating component 403. The potassium nitrate solid settles slowly in the first acid solution with relatively high viscosity, i.e., the concentrated sulfuric acid system. Therefore, the added potassium nitrate is easily thrown directly into the overflow port by the stirring centrifugal force and flows out, resulting in a lot of potassium nitrate being lost without reacting. Therefore, the overflow port of the continuous nitrating component 403 is improved, and a baffle is added near the overflow port to prevent the newly added potassium nitrate solid from directly overflowing. The position of the baffle 4031 is as shown in FIG. Figure 2 As shown, no stirring blades are installed within a certain distance below the overflow port, such as Figure 2 As shown, the stirring paddle extending in the vertical direction in the middle is provided with stirring blades, and a static space is formed between the uppermost stirring blade and the top of the continuous nitrification component 403 to further prevent the newly added potassium nitrate solid from directly overflowing.

[0163] Since the continuous nitration reaction adopts continuous flow operation, the residence time of the material in the reactor is uniform, which helps to enhance the efficiency of mass transfer and heat transfer. Compared with the traditional intermittent reaction, the contact between the material and the nitrating agent is more complete, and the distribution of heat energy is more uniform, thereby improving the selectivity and conversion rate of the reaction. In the continuous nitration reaction, the reaction conditions can be optimized by precisely controlling the reaction temperature, pressure and feed rate to ensure that the reaction is carried out under the most suitable environment. This precise control helps to reduce the generation of by-products and improve the purity and yield of the main product. In the continuous nitration process, due to the precise control of the reaction conditions and efficient mass transfer and heat transfer, the use of excessive chemicals can be reduced, costs can be saved, and the generation of toxic and harmful by-products can be reduced, which is beneficial to environmental protection. The continuous nitration unit is integrated with other continuous units, and the entire process is automatically controlled to reduce manual operation, which not only improves production efficiency, but also reduces the risk of operating errors, and further enhances the safety of production. The integration of the continuous nitration unit with other continuous processing units realizes a full continuous production chain from raw materials to products, which is conducive to improving the flexibility of the production line and the ability to respond to market changes.

[0164] Further, the continuous esterification unit comprises:

[0165] A third raw material tank 305, wherein the third raw material tank 305 is used for storing a quenching agent;

[0166] A first continuous quenching component 404, wherein the inlet of the first continuous quenching component 404 is connected to the outlet of the third raw material tank 305 and the outlet of the continuous nitration unit, respectively, so as to continuously quench the continuous nitration product with a quenching agent to obtain a continuous quenching product;

[0167] A first continuous filtering component 701, wherein the inlet of the first continuous filtering component 701 is connected to the outlet of the first continuous quenching component 404, so as to continuously filter the continuous quenching product to obtain a continuous filtering product;

[0168] A first continuous dosing component 405, wherein the inlet of the first continuous dosing component 405 is connected to the outlet of the first continuous filtering component 701 to provide a continuous dosing reaction site for the continuous filtering product;

[0169] A first solvent storage tank 306, the outlet of which is in communication with the first continuous dosing component 405, so as to continuously dosing with the continuously filtered product in the first continuous dosing component 405, and obtain a first continuous dosing product, and transport the first continuous dosing product to the first liquid storage tank 307 in communication with the outlet end of the first continuous dosing component 405 for temporary storage;

[0170] The continuous esterification component 406, the outlet of the first liquid storage tank 307 is connected to the inlet of the continuous esterification component 406, so as to transport the first continuous batching product into the continuous esterification component 406;

[0171] The outlet of the first solid feeder 503 is connected to the inlet of the continuous esterification component 406 to transport the first solid additive into the continuous esterification component 406 so that the first solid additive is mixed with the first continuous batching product to carry out continuous esterification to obtain a continuous esterification product. The outlet of the continuous esterification component 406 is connected to the continuous chlorine-based fluorination unit.

[0172] A first liquid feed pump 105 and a fifth liquid flow meter 205 are provided on the pipeline between the third raw material tank 305 and the first continuous quenching component 404. The fifth liquid flow meter 205 can monitor the flow of the quenching agent entering the first continuous quenching component 404 in real time, so as to control the opening size of the first liquid feed pump 105 according to the detection result of the fifth liquid flow meter 205. A fourth solid feeder 502 is also provided on the pipeline between the first continuous filtering component 701 and the first continuous dosing component 405 to continuously deliver the continuous filtration product to the first continuous dosing component 405. 5, a second liquid feed pump 106 and a sixth liquid flow meter 206 are provided on the pipeline between the first liquid storage tank 307 and the continuous esterification component 406, and the flow rate of the first solvent entering the first continuous dosing component 405 can be monitored in real time by the sixth liquid flow meter 206, so as to control the opening of the second liquid feed pump 106 according to the flow rate of the first solvent, and a third liquid feed pump 107 and a seventh liquid flow meter 207 are provided on the pipeline between the first liquid storage tank 307 and the continuous esterification component 406, and the flow rate of the first continuous dosing product entering the continuous esterification component 406 can be monitored in real time by the seventh liquid flow meter 207, and the opening of the third liquid feed pump 107 can be controlled. Exemplarily, the first continuous quenching component 404 is one or more of a dynamic tubular reactor and a fully mixed reactor, the first continuous filtering component 701 is one or more of a candle filter and a horizontal centrifuge, the first continuous dosing component 405 is one or more of a dynamic tubular reactor and a fully mixed flow reactor, and the continuous esterification component 406 is one or more of a dynamic tubular reactor and a fully mixed reactor.

[0173] Continuous processes can better control reaction conditions and reduce the risk of runaway exothermic reactions due to rapid accumulation of materials. Especially in highly dangerous reactions such as sulfonation and fluorination, continuous operation avoids manual on-site participation, reduces the chance of operators coming into contact with highly dangerous chemicals, and significantly improves production safety. Continuous operation reduces energy losses in intermittent operations, such as energy consumption in heating and cooling processes, thereby reducing energy consumption in the entire production process. In addition, it also reduces the reliance on manual operation, reduces the requirements for operator skills, and also reduces the exposure time of personnel in high-risk environments, improving production safety.

[0174] Further, the continuous chlorine-based fluorination unit comprises:

[0175] A second continuous filtering component 702, the inlet of which is connected to the continuous esterification unit to continuously filter the continuous esterification product to obtain a second continuous filtering product;

[0176] A first continuous concentrating component 801, wherein the inlet of the first continuous concentrating component 801 is connected to the outlet of the second continuous filtering component 702, so as to continuously concentrate the second continuous filtering product to obtain a first continuous concentrated product;

[0177] A second continuous dosing component 407, the inlet of which is connected to the outlet of the first continuous concentration component 801, so as to provide a continuous dosing reaction site for the first continuous concentration product;

[0178] A dimethylformamide storage tank 308, the outlet of which is in communication with the second continuous batching component 407, so that the dimethylformamide stored in the dimethylformamide storage tank 308 is transported to the second continuous batching component 407 and mixed with the first continuous concentrated product in the second continuous batching component 407 to perform continuous batching to obtain a second continuous batching product, and the second continuous batching product is transported to the second liquid storage tank 309 in communication with the outlet of the second continuous batching component 407 for storage;

[0179] A continuous chlorine-based fluorination component 408, the inlet of which is connected to the outlet of the second liquid storage tank 309 to provide a continuous fluorination reaction site;

[0180] The second solid feeder 505, the outlet of the second solid feeder 505 is connected to the continuous chlorine-based fluorination component 408 to transport the fluorinating agent and continuously mix it with the second continuous batching product to obtain a continuous chlorine-based fluorination product, and the outlet of the continuous chlorine-based fluorination component 408 is connected to the continuous bromination unit.

[0181] A fifth solid feeder 504 is provided on the pipeline between the first continuous concentration component 801 and the second continuous dosing component 407 for conveying the first continuous concentrated product to the second continuous dosing component 407. A fourth liquid feed pump 108 and an eighth liquid flow meter 208 are provided on the pipeline between the dimethylformamide storage tank 308 and the second continuous dosing component 407. The eighth liquid flow meter 208 can monitor the flow rate entering the second continuous dosing component 407 in real time to control the valve opening of the fourth liquid feed pump 108. A fifth liquid feed pump 108 is provided on the pipeline between the second liquid storage tank 309 and the continuous chlorine-based fluorination component 408. The feed pump 109 and the ninth liquid flow meter 209, the ninth liquid flow meter 209 is used to monitor the flow rate of the second continuous batching product entering the continuous chlorine-based fluorination component 408, so as to control the valve opening of the fifth liquid feed pump 109, wherein the second continuous filtering component 702 is one or more of a candle filter and a horizontal screw centrifuge, the first continuous concentrating component 801 is one or more of a falling film evaporator, a thin film evaporator, and a flash tank, the second continuous batching component 407 is one or more of a dynamic tubular reactor and a fully mixed flow reactor, and the continuous chlorine-based fluorination component 408 is one or more of a dynamic tubular reactor and a fully mixed reactor.

[0182] Through continuous filtration, concentration and batching, the reaction conditions can be precisely controlled, the residence time of materials can be reduced, and the unstable yield and by-product generation caused by improper operation or fluctuations in reaction conditions in traditional batch reactions can be avoided. Continuous batching can adjust the ratio in real time to ensure that the reactants reach the optimal state before entering the fluorination reaction, thereby improving the selectivity and yield of the fluorination reaction. At the same time, the continuous process can effectively control the heat of reaction and reduce safety hazards. The continuous concentration process can more efficiently recycle and reuse solvents and reduce the total consumption of solvents. In addition, continuous batching and reaction can reduce the excessive use of chemicals, thereby reducing chemical costs and reducing waste generation. The filtration and concentration units in the continuous process can continuously remove solids and solvents produced in the reaction, simplify the post-processing process, reduce purification costs, and reduce the discharge of wastewater and exhaust gas, which has a positive impact on environmental protection.

[0183] Further, the consecutive brominated units include:

[0184] A second continuous concentrating component 802, the inlet of which is connected to the outlet of the continuous chlorine-based fluorination unit to continuously concentrate the continuous chlorine-based fluorination product to obtain a second continuous concentrated product;

[0185] A continuous hydrolysis reaction component 409, the inlet of which is in communication with the outlet of the second continuous concentration component 802, so as to provide a continuous hydrolysis reaction site;

[0186] A water storage unit 310, wherein the outlet of the water storage unit 310 is connected to the inlet of the continuous hydrolysis reaction unit 409 to transport water and mix the water with the second continuous concentrated product in the continuous hydrolysis reaction unit 409 to perform continuous hydrolysis to obtain a continuous hydrolyzed product;

[0187] A first continuous distillation component 901, the inlet of the first continuous distillation component 901 is connected to the outlet of the continuous hydrolysis reaction component 409, so as to continuously distill the continuous hydrolysis product to obtain a continuous distillation product;

[0188] A continuous bromination reaction component 410, the inlet of which is connected to the outlet of the first continuous distillation component 901, providing a continuous bromination reaction site;

[0189] a third solid feeder 506, wherein the outlet of the third solid feeder 506 is connected to the inlet of the continuous bromination reaction unit 410 to deliver the brominating agent;

[0190] The second acid storage tank 311, the outlet of the second acid storage tank 311 is connected to the inlet of the continuous bromination reaction component 410 to transport the second acid solution and mix it with the brominating agent and the continuous distillation product to perform continuous bromination to obtain a continuous bromination product. The outlet of the continuous bromination reaction component 410 is connected to the continuous diazotization unit.

[0191] A sixth liquid feed pump 110 and a tenth liquid flow meter 210 are also provided between the water storage component 310 and the continuous hydrolysis reaction component 409. The tenth liquid flow meter 210 is used to detect the size of the liquid flow entering the continuous hydrolysis reaction component 409 in real time to control the valve opening of the sixth liquid feed pump 110. A first sulfuric acid feed pump 111 and an eleventh liquid flow meter 211 are also provided on the pipeline between the second acid storage tank 311 and the continuous bromination reaction component 410. The eleventh liquid flow meter 211 can monitor the flow of the second acid liquid entering the continuous bromination reaction component 410 in real time to control the valve opening of the first sulfuric acid feed pump 111. Exemplarily, the second continuous concentration component 802 is one or more of a falling film evaporator, a thin film evaporator, and a flash tank, the continuous hydrolysis reaction component 409 is one or more of a dynamic tubular reactor and a fully mixed reactor, the first continuous distillation component 901 is one or more of a plate distillation tower and a packed distillation tower, and the continuous bromination reaction component 410 is one or more of a dynamic tubular reactor and a fully mixed reactor.

[0192] By the second continuous concentration part 802, the continuous chlorine-based fluorination product is continuously concentrated, and the production cycle can be significantly shortened and production efficiency can be improved. At the same time, the continuous operation mode can respond to the changes of process parameters more quickly than the traditional intermittent operation, and the flexibility of the reaction process is improved. The use of the continuous hydrolysis reaction part 409 and the continuous bromination reaction part 410 makes the whole reaction process not need to be manually operated frequently, and the opportunity of manual contact with hazardous chemicals is reduced, especially the potential danger of high-risk operation in the intermittent reactor is avoided, thereby improving the safety of the whole production process, the connection between the water storage part 310 and the continuous hydrolysis reaction part 409 realizes the accurate measurement and continuous addition of water, which helps to optimize the use of water resources and reduce waste. At the same time, the connection between the second acid storage tank 311 and the continuous bromination reaction part 410 ensures the continuous supply of the second acid solution, improves the use efficiency of the second acid solution, and reduces the reaction cost. The first continuous distillation part 901 performs continuous distillation on the continuous hydrolyzed product, and the separation conditions can be more accurately controlled to improve product purity and yield. Compared with intermittent distillation, continuous distillation can separate the target product more effectively and reduce the interference of impurities, thereby improving the quality and yield of the final product. The setting of the tenth liquid flow meter 210 and the eleventh liquid flow meter 211 can monitor and control the flow of the liquid in real time to ensure the stability of the reaction conditions, which is conducive to realizing the automatic control of the entire production process, reducing the influence of human factors, and improving the stability and consistency of the process. The continuous reaction and separation technologies such as continuous concentration, continuous hydrolysis, continuous bromination and continuous distillation can significantly reduce energy consumption, reduce the size and quantity of equipment, reduce equipment investment and maintenance costs, and improve equipment utilization.

[0193] Further, the continuous diazotization unit comprises:

[0194] A continuous extraction component 1101, wherein the inlet of the continuous extraction component 1101 is connected to the outlet of the continuous bromination unit to continuously extract the continuous bromination product to obtain a second organic phase;

[0195] A third solvent storage tank 312, the outlet of the third solvent storage tank 312 is connected to the third continuous dosing component 411 to transport the third solvent therein, the outlet of the continuous extraction component 1101 is connected to the inlet of the third continuous dosing component 411 to transport the second organic phase, and continuously dosing with the third solvent to obtain a third continuous dosing product, and the third continuous dosing product is transported to the third liquid storage tank 313 connected to the outlet end of the third continuous dosing component 411 for storage;

[0196] A continuous reduction component 1001, wherein the inlet of the continuous reduction component 1001 is connected to the outlet of the third liquid storage tank 313, so as to continuously reduce the third continuous batching product to obtain a continuous reduction product;

[0197] The inlet of the third continuous concentrating unit 803 is connected to the outlet of the continuous reducing unit 1001 to continuously concentrate the continuous reduction product to obtain a third continuous concentrated product;

[0198] The fourth continuous dosing component 412, whose inlet end is connected to the outlet of the third continuous concentrating component 803, so as to accommodate the third continuous concentrated product;

[0199] The third acid storage tank 314, whose outlet end is connected to the inlet of the fourth continuous batching component 412, is used to transport the third acid solution into the fourth continuous batching component 412 and mix it with the third continuous concentrated product to continuously batch and obtain the third continuous batching product;

[0200] The continuous diazo component 413, whose inlet end is connected to the outlet of the fourth continuous dosing component 412, is used to accommodate the third continuous dosing product;

[0201] The outlet of the nitrosylsulfuric acid storage component 315 is connected to the inlet of the continuous diazo component 413 to continuously transport nitrosylsulfuric acid into the continuous diazo component 413 and mix it with the third continuous ingredient product in the continuous diazo component 413 to perform continuous diazotization to obtain a continuous diazotization product. The outlet of the continuous diazo component 413 is connected to the continuous fluorination unit.

[0202] An ethanol feed pump 112 and a twelfth liquid flow meter 212 are also provided on the pipeline between the third solvent storage tank 312 and the third continuous dosing component 411. The twelfth liquid flow meter 212 is used to monitor the flow of ethanol entering the third continuous dosing component 411 in real time to control the valve opening of the ethanol feed pump 112. A seventh liquid feed pump 113 and a twelfth liquid flow meter 213 are also provided on the pipeline between the third liquid storage tank 313 and the continuous reduction component 1001. The twelfth liquid flow meter 213 monitors the flow of the continuous reduction product entering the continuous reduction component 1001 in real time to control the valve opening of the seventh liquid feed pump 113. A third sulfuric acid feed pump 114 and a thirteenth liquid flow meter 214 are also provided on the pipeline between the third acid storage tank 314 and the fourth continuous dosing component 412. The thirteenth liquid flow meter 214 is used to monitor the flow of the third acid liquid entering the fourth continuous dosing component 412 in real time to control the valve opening of the third sulfuric acid feed pump 114. A nitrosyl sulfuric acid feed pump 115 and a fourteenth liquid flow meter 215 are also provided on the pipeline between the nitrosyl sulfuric acid storage component 315 and the continuous diazo component 413. The fourteenth liquid flow meter 215 is used to monitor the flow of nitrosyl sulfuric acid entering the continuous diazo component 413 in real time to control the valve opening of the nitrosyl sulfuric acid feed pump 115.

[0203] Exemplarily, the continuous extraction component 1101 is one or more of a continuous extraction column and a centrifugal extractor, the third continuous concentration component 803 is one or more of a dynamic tubular reactor and a fully mixed flow reactor, the continuous reduction component 1001 is one or more of an axially adiabatic fixed bed reactor, a radially adiabatic fixed bed reactor, and a shell-and-tube fixed bed reactor, the third continuous concentration component 803 is one or more of a falling film evaporator, a thin film evaporator, and a flash tank, the fourth continuous dosing component 412 is one or more of a dynamic tubular reactor and a fully mixed flow reactor, and the continuous diazo component 413 is one or more of a dynamic tubular reactor and a fully mixed flow reactor.

[0204] The continuous diazotization unit transforms the diazotization reaction from the traditional batch operation mode to continuous operation, reducing the risk of large accumulation of reactants and products in the equipment. In particular, for reactions with strong exothermicity, the reaction heat can be removed in time to avoid safety problems caused by heat accumulation. In addition, continuous operation reduces the number of manual handling of highly hazardous chemicals and reduces the risk of personnel contact with hazardous substances. Compared with traditional batch operations, the use of continuous extraction components and continuous concentration components can significantly reduce the amount of solvent used and improve the recycling rate of solvents. Reduce energy consumption. For example, in the continuous concentration step, by optimizing operating conditions such as temperature and vacuum, more efficient energy utilization can be achieved and overall production costs can be reduced. The product after continuous diazotization enters the continuous fluorination unit. Due to the continuous operation of the previous step, it can ensure that the product entering the fluorination unit has higher purity and fewer impurities, which is crucial to the efficiency of subsequent reactions and product quality.

[0205] Further, the continuous fluorination unit comprises:

[0206] A second continuous quenching component 414, the inlet of which is connected to the outlet of the continuous diazotization unit;

[0207] The urea containing part 316 has an outlet connected to the inlet of the second continuous quenching part 414, so as to continuously deliver urea to the second continuous quenching part 414 and mix it with the continuous diazotization product in the second continuous quenching part 414 to perform continuous quenching to obtain a second quenched product system;

[0208] a fluorination reaction component 415, the inlet of which is connected to the outlet of the second continuous quenching component 414 to accommodate a second quenching product system;

[0209] A hydrofluoric acid storage component 317, whose outlet is connected to the inlet of the fluorination reaction component 415, so as to continuously transport the hydrofluoric acid and mix it with the second quenched product system in the fluorination reaction component 415 to obtain a first fluorination product;

[0210] The inlet of the second continuous distillation component 902 is connected to the outlet of the fluorination reaction component 415 to continuously flow the first fluorination product to obtain 3,4,5-trifluorobromobenzene, and the 3,4,5-trifluorobromobenzene is transported to the product tank 318 for storage.

[0211] A urea solution feed pump 116 and a fifteenth liquid flow meter 216 are provided on the pipeline between the urea containing component 316 and the second continuous quenching component 414. The fifteenth liquid flow meter 216 is used to monitor the flow rate of urea entering the second continuous quenching component 414 in real time to control the opening size of the valve of the urea solution feed pump 116. A hydrofluoric acid feed pump 117 and a sixteenth liquid flow meter 217 are provided on the pipeline between the hydrofluoric acid storage component 317 and the fluorination reaction component 415. The sixteenth liquid flow meter 217 is used to monitor the flow rate of hydrofluoric acid entering the fluorination reaction component 415 in real time to control the opening size of the valve of the hydrofluoric acid feed pump 117. The second continuous quenching component 414 is one or more of a dynamic tubular reactor and a fully mixed flow reactor, the fluorination reaction component 415 is one or more of a dynamic tubular reactor and a fully mixed flow reactor, and the second continuous distillation component 902 is one or more of a plate distillation tower and a packed distillation tower.

[0212] By precisely controlling the feed amounts of urea and hydrofluoric acid, the violent exotherm during the reaction is reduced, the safety risks caused by heat accumulation are lowered, the batch addition of highly dangerous chemicals such as hydrofluoric acid in traditional intermittent reactions is avoided, the direct contact between personnel and highly toxic materials is reduced, and production safety is improved.

[0213] According to another aspect of the present invention, a continuous production method of 3,4,5-trifluorobromobenzene is provided, which is applied to the above-mentioned production equipment for preparing 3,4,5-trifluorobromobenzene, and the production method comprises: controlling o-dichlorobenzene to be continuously fed to a continuous sulfonation reaction tank 401 in a first feed amount and chlorosulfonic acid to be continuously fed to a second feed amount, respectively, and performing a continuous sulfonation reaction under a first preset condition to obtain a continuous sulfonation product; controlling the continuous sulfonation product to be continuously fed to a continuous post-treatment device for continuous post-treatment to obtain 3,4,5-trifluorobromobenzene; wherein the first preset condition is that the first reaction temperature is 50°C to 80°C, the sulfonation reaction time is 120min to 130min, the first feed amount is 10g / min to 30g / min, and the second feed amount is that the amount of chlorosulfonic acid added to every 1g of o-dichlorobenzene is 1g to 3g.

[0214] In a preferred embodiment, the continuous production method further comprises: controlling the continuous sulfonation product to be continuously transported to a continuous nitration unit for continuous esterification to obtain a continuous esterification product; controlling the continuous esterification product to be continuously transported to a continuous chlorination fluorination unit for continuous chlorination fluorination to obtain a continuous chlorination fluorination product; controlling the continuous chlorination fluorination product to be continuously transported to a continuous bromination unit for continuous bromination to obtain a continuous bromination product; controlling the continuous bromination product to be continuously transported to a continuous diazotization unit for continuous diazotization to obtain a continuous diazotization product; controlling the continuous diazotization product to be continuously transported to a continuous fluorination unit for continuous fluorination to obtain 3,4,5-trifluorobromobenzene.

[0215] Through continuous sulfonation reaction, the reaction time can be significantly shortened from the traditional batch reaction time (which may be up to several hours) to 120min~300min, which not only speeds up the production cycle, but also reduces the accumulation of heat during the reaction and reduces the safety risks caused by improper temperature control. Compared with traditional batch reactions, continuous processes can reduce a large number of manual operations and reduce labor costs. At the same time, continuous operation can more accurately control the feed amount and reaction conditions of materials, improve the utilization rate of raw materials, reduce the generation of by-products and waste, thereby reducing production costs and environmental impact. Continuous reactions can achieve stability and controllability of the reaction process by accurately controlling the feed rate and reaction conditions of materials, avoid yield fluctuations caused by batch inconsistency, and improve product quality and consistency. Continuous post-processing steps can reduce the number of material transfers and reduce the risk of material loss and contamination during the transfer process. At the same time, continuous water washing, continuous quenching and other steps can be processed immediately after the reaction, reducing the storage time of intermediates, avoiding the degradation of intermediates, and improving the yield of the overall reaction. The continuous process reduces direct contact between personnel and highly dangerous chemicals (such as hydrofluoric acid), reduces the potential harm of chemicals to operators, improves the working environment, and increases the safety of the production process.

[0216] In addition, preferably, the continuous production method also includes: controlling the continuous sulfonation product to be transported to the continuous water washing component 402 with a third feed amount, and continuously washing the continuous sulfonation product with a set water amount under the second preset condition to obtain a continuous water-washed product; controlling the continuous water-washed product to enter the first continuous liquid separation component 601 with a fourth feed amount to perform continuous liquid separation under the third preset condition, and obtain a first organic phase; controlling the first organic phase to be transported to the continuous nitration component 403 with a fifth feed amount, and at the same time, controlling the first acid solution to be transported to the continuous nitration component 403 with a set acid solution amount, and continuously nitrifying under the action of the nitrating agent under the fourth preset condition to obtain a continuous nitration product; wherein the third feed amount is 15g / min~45g / min, and the water amount is set to a volume of water contained in every 1g of the third feed amount of 0.5ml~1.5ml; and / or, the second preset condition is that the water washing temperature is 5℃~10℃, the washing time is 10min~30min; and / or, the fourth feed amount is 20g / min~60g / min; and / or, the third preset condition is that the first continuous liquid separation temperature is 20℃~40℃; and / or, the first continuous liquid separation time is 5min~10min; and / or, the fifth feed amount is 10g / min~15g / min, and the acid solution amount is set to 30g~45g of the first acid solution contained in every 1g of the third feed amount; and / or, the type of nitrating agent is one or more of potassium nitrate, sodium nitrate, and concentrated nitric acid; and / or, the amount of nitrating agent is 0.8g~1.5g of the nitrating agent contained in every 1g of the third feed amount; and / or, the fourth preset condition is that the nitrating temperature is 0℃~20℃, and the nitrating time is 60min~180min; and / or, the first acid solution is concentrated sulfuric acid with a mass concentration of 81%~98%.

[0217] Continuous production reduces the number of batch feeding and material transfers, especially for high-risk reactions such as sulfonation and fluorination, avoiding direct contact between personnel and hazardous chemicals, significantly reducing safety risks. The continuous production mode shortens the reaction time, reduces the volume of reaction equipment, and reduces energy consumption. At the same time, the increase in the degree of automation reduces the dependence on manual operation, which greatly shortens the production cycle. The material feed rate and reaction conditions in the continuous production process are more stable, avoiding problems such as unstable product yields caused by manual operation in intermittent production, and improving product purity and yield. Continuous production reduces the use of solvents and reduces purification costs. At the same time, it reduces the generation of three wastes, reduces environmental protection treatment costs, and effectively controls the overall production cost. The design of continuous equipment is relatively simple, and the manufacturing cost is low. At the same time, it reduces the demand for large reactors and reduces equipment investment and maintenance costs.

[0218] Preferably, the continuous production method further comprises: controlling the continuous nitration product to be delivered to the first continuous quenching component 404 at a sixth feed amount, and continuously quenching the continuous nitration product under fifth preset conditions with a solvent of a set solvent amount to obtain a continuous quenching product; controlling the continuous quenching product to be delivered to the first continuous filtering component 701 at a seventh feed amount, and continuously filtering under sixth preset conditions to obtain a continuous filtration product; controlling the continuous filtration product to be delivered to the first continuous dosing component 405 at an eighth feed amount, and controlling the first solvent in the first solvent storage tank 306 to be delivered to the first continuous filtration component 701 at a eighth feed amount, and continuously filtering under sixth preset conditions to obtain a continuous filtration product. The first continuous batching product is controlled to be delivered to the continuous esterification component 406 at a feed rate of 30 g / min to 80 g / min, and at the same time, the first solid feeder 503 is controlled to deliver the first solid additive to the continuous esterification component 406 at a second set amount, and the continuous esterification is carried out at a temperature of 40° C. to 70° C. for an esterification time of 30 min to 180 min to obtain a continuous esterification product; wherein the sixth feed rate is 50 g / min~120g / min, the amount of solvent is set to be 1ml~3ml for every 1g of the sixth feed amount; and / or, the solvent is one or more of tap water, purified water, and deionized water; and / or, the fifth preset condition is that the temperature of the first continuous quenching is 5℃~20℃, and the first continuous quenching time is 10min~30min; and / or, the seventh feed amount is 200g / min~420g / min; and / or, the sixth preset condition is that the first continuous filtration temperature is in the range of 10℃~20℃, and the first continuous filtration time is 10 min~30min; and / or, the eighth feed amount is 10g / min~15g / min, the sixth preset condition is that the first continuous batching temperature is 20℃~50℃, the first continuous batching time is 10min~30min, the first set amount is 2ml~5ml of the first solvent added per 1g of the eighth feed amount; and / or, the second set amount is 1.2g~3.5g of the first solid additive added per 1g of the first continuous batching product; and / or, the first solid additive is any one or more of potassium carbonate, cesium carbonate and sodium carbonate.

[0219] The continuous production process avoids the cumbersome material transfer and waiting time in traditional batch reactions, allowing the reaction and post-processing steps to be seamlessly connected, greatly shortening the production cycle, improving material utilization and reaction selectivity, and thus increasing the overall yield of the product. By precisely controlling the feed rate, reaction temperature and time, especially in high-risk reactions such as sulfonation and fluorination, the use of continuous reactors instead of batch reactors reduces the accumulation of heat during the reaction and reduces the risk of accidents caused by heat runaway. At the same time, through the PLC automatic control system, manual operations are reduced, direct contact between personnel and highly dangerous chemicals is avoided, and the safety of personnel in the production process is improved. The continuous process reduces the use of solvents, reduces the generation of three wastes in the post-processing process, and reduces the purification cost. In addition, the use of continuous reactors reduces the cost of equipment investment because they are relatively small in size and are superior to traditional equipment in terms of mass transfer and heat transfer efficiency, reducing the need for high-performance equipment.

[0220] In a preferred embodiment, the continuous production method further comprises: controlling the continuous esterification product to be transported to the second continuous filtering component 702 at a feed rate of 50 g / min to 150 g / min, and continuously filtering at a filtering temperature of 10°C to 30°C and a filtering time of 10 min to 30 min to obtain a second continuous filtering product; controlling the second continuous filtering product to be transported to the first continuous concentrating component 801 at a feed rate of 30 g / min to 80 g / min, and continuously filtering at a first concentrating temperature of 40°C to 6 ...50 g / min to 150 g / min, and continuously filtering at a filtering temperature of 10°C to 30°C and a filtering time of 10 min to 30 min to obtain a second continuous filtering product; controlling the second continuous filtering product to be transported to the first continuous concentrating component 801 at a feed rate of 50 g / min to 150 g / min, and continuously filtering at a filtering temperature of 10°C to 30°C and a filtering time of 10 min to The first concentration pressure is -0.06MPa to -0.1MPa, and the first concentration time is 30min to 60min, so as to obtain a first continuous concentrated product; the first continuous concentrated product is controlled to be delivered to the second continuous dosing component 407 at a feeding rate of 10g / min to 15g / min, and the second solvent in the dimethylformamide storage tank 308 is controlled to be continuously dosed at a temperature of 20°C to 40°C and a dosing time of 10min to 30min with a third set amount, so as to obtain a second continuous concentrated product; Continuously batched product; controlling the second continuous batched product to be delivered to the continuous chlorine-based fluorination component 408 at a feed rate of 25g / min~80g / min, and controlling the second solid feeder 505 to continuously deliver the fluorinating agent to the continuous chlorine-based fluorination component 408 at a fourth set dosage, and continuously mixing under the condition of a fifth set dosage of the catalyst to obtain a continuous chlorine-based fluorination product; wherein the type of the second solvent is one or more of N,N-dimethylformamide, N,N-dimethylacetamide; and / or the type of the fluorinating agent is potassium fluoride, One or more of sodium fluoride and boron trifluoride; and / or the type of catalyst is one or more of tetraphenylphosphonium bromide and 4-bromobenzyltriphenylphosphonium bromide; and / or the third set dosage is 2mL~5mL of dimethylformamide added per 1g of the first continuous concentrated product; and / or the fourth set dosage is 0.15g~0.3g of the fluorinating agent added per 1g of the second continuous batching product; and / or the fifth set dosage is 0.1g~0.5g of the catalyst added per 1g of the second continuous batching product.

[0221] The continuous production method of the present invention can accurately control the reaction conditions (such as temperature, pressure, residence time) by adopting a continuous reactor, such as a dynamic tubular reactor, a fully mixed flow reactor, a plug flow reactor, etc., so as to improve the mass transfer and heat transfer effect, and improve the selectivity and yield of the reaction. Especially in the highly dangerous steps of sulfonation and fluorination, direct manual contact with hazardous chemicals is avoided, and the safety risk in the production process is significantly reduced. Compared with the traditional batch kettle reaction, the continuous process greatly reduces the volume of the reaction equipment. Especially for highly exothermic reactions, the continuous reactor can effectively dissipate heat and reduce heat accumulation, thereby avoiding the need for large-scale heat exchange equipment and reducing the equipment investment cost. At the same time, the continuous production line has a compact layout and reduces the floor space. The implementation of post-processing processes such as continuous filtration, concentration, and distillation reduces the use of solvents, reduces energy consumption, reduces the generation of three wastes, and reduces environmental protection treatment costs. The combination of continuous batching and reaction improves the utilization rate of materials and further reduces production costs. The continuous process reduces the time for material transfer and intermediate product processing, shortens the entire production cycle, and improves production efficiency. For example, the implementation of continuous nitration, chlorofluorination and other steps significantly reduces the reaction time. The precise control of continuous batching and the stable conditions during the continuous reaction process help to improve product quality and yield. In particular, the continuous chlorofluorination and continuous diazofluorination steps can more effectively control the reaction, avoid the formation of by-products, and improve the yield of the target product.

[0222] In a preferred embodiment, the continuous production method further comprises: controlling the continuous chlorine-based fluorination product to be delivered to the second continuous concentration component 802 at a feed rate of 40 g / min to 100 g / min, and continuously concentrating at a concentration temperature of 90°C to 140°C, a concentration pressure of -0.06 MPa to 0-0.1 MPa, and a concentration time of 30 min to 60 min to obtain a second continuous concentrated product; controlling the second continuous concentrated product to be delivered to the continuous water at a feed rate of 20 g / min to 50 g / min; The continuous hydrolysis reaction part 409 is controlled, and the water storage part 310 is controlled to deliver the water with the sixth set amount to the continuous hydrolysis reaction part 409, and the continuous hydrolysis is carried out under the conditions of the hydrolysis temperature of 10° C. to 50° C. and the hydrolysis time of 60 min to 180 min to obtain a continuous hydrolysis product; the continuous hydrolysis product is controlled to be delivered to the first continuous distillation part 901 at a feed rate of 40 g / min to 100 g / min, and the distillation temperature is 100° C. to 180° C. and the distillation pressure is -0.08 MPa to -0.1 MPa. The continuous distillation is carried out under the pressure to obtain a continuous distillation product; the continuous distillation product is controlled to be delivered to the continuous bromination reaction part 410 at a feed rate of 3g / min~10g / min, and the bromination agent is continuously delivered to the continuous bromination reaction part 410 at a seventh set amount in the third solid feeder 506, and the second acid solution in the second acid storage tank 311 is controlled to be delivered to the continuous bromination reaction part 410 at an eighth set amount, and the continuous bromination is carried out under the conditions of a bromination temperature of 40°C~60°C and a bromination time of 30min~90min. Bromination to obtain a continuous brominated product; wherein the type of the brominating agent is one or more of dibromohydantoin, bromine, and N-bromosuccinimide; and / or, the sixth set amount is 3 mL to 5 mL of water added per 1 g of the second continuous concentrated product; and / or, the seventh set amount is 1 g to 2 g of the brominating agent added per 1 g of the second continuous concentrated product; and / or, the eighth set amount is 2 g to 5 g of the second acid solution added per 1 g of the second continuous concentrated product; and / or, the second acid solution is 81% to 98% sulfuric acid.

[0223] The continuous production method greatly shortens the reaction time, reduces the loading and unloading and transfer of materials, improves the utilization efficiency of the reactor, makes the entire production process more efficient, and significantly shortens the production cycle. By using continuous reactors, especially for high-risk reactions such as sulfonation and fluorination, the reaction conditions can be precisely controlled, avoiding the instantaneous accumulation of a large amount of heat, reducing the risk of runaway reaction and explosion, and improving the safety of the production process. Continuous batching, reaction and post-treatment processes ensure the consistency of reaction conditions, reduce the occurrence of side reactions, and improve product purity and yield. For example, by optimizing the continuous chlorofluorination and continuous hydrolysis processes, the product yields can reach 71.3% and 81.9%, respectively.

[0224] In a preferred embodiment, the continuous production method further includes: controlling the continuous bromination product to be continuously transported to the continuous extraction component 1101 at a feed rate of 15 g / min to 30 g / min, and continuously extracting at a temperature of 30° C. to 50° C. and a time of 15 min to 45 min to obtain a second organic phase; controlling the second organic phase to be continuously transported to the third continuous batching component 411 at a feed rate of 5 g / min to 15 g / min and the third solvent in the third solvent storage tank 312 at a ninth set amount, and continuously batching at a temperature of 20° C. to 40° C. and a time of 10 min to 30 min to obtain a third continuous batching product; The third continuous batching product is controlled to be transported to the continuous reduction component 1001 at a feed rate of 40 g / min to 90 g / min, and is continuously reduced under the conditions of the reducing agent being the tenth set amount, the reduction temperature being 40° C. to 80° C., the pressure being 0.3 MPa to 1.0 MPa, and the time being 30 to 60 min to obtain a continuous reduction product; the continuous reduction product is controlled to be transported to the third continuous concentration component 803 at a feed rate of 40 g / min to 90 g / min, and is continuously concentrated under the conditions of the concentration temperature being 40° C. to 60° C. and the concentration pressure being -0.06 MPa to 0-0.1 MPa to obtain a third continuous concentrated product; the third continuous The concentrated product is fed at a feed rate of 10 g / min to 15 g / min, and the third acid solution in the third acid storage tank 314 is fed to the fourth continuous batching component 412 at an eleventh set dosage, and is continuously batched under the conditions of a reaction temperature of 0°C to 20°C and a residence time of 10 min to 20 min to obtain a third continuous batching product; the third continuous batching product is controlled to be fed to the continuous diazo component 413 at a feed rate of 30 g / min to 75 g / min, and the nitrosylsulfuric acid storage component 315 is controlled to be fed to the continuous diazo component 413 at a twelfth set dosage, so that the third continuous batching product is mixed with the nitrosylsulfuric acid, and the reaction temperature is -20°C. ~0℃, reaction residence time of 30min~90min, continuous diazotization reaction is carried out under the conditions of ethanol, methanol, isopropanol, or several thereof; and / or, the type of reducing agent is one or several of Raney nickel, palladium carbon, and aluminum-nickel alloy catalyst; and / or, the third acid solution is concentrated sulfuric acid with a concentration of 30%~70%, and the concentration of nitrosylsulfuric acid is 30%~50%; and / or, the ninth set dosage is 3mL~5mL of the third solvent added per 1g of the second organic phase; and / or, the tenth set dosage is 0.05g~0.2g; and / or, the eleventh set amount is 5g~10g of the third acid solution added per 1g of the third continuous concentrated product; and / or, the twelfth set amount is 3g~5g of nitrosylsulfuric acid added per 1g of the third continuous batching product.

[0225] By adopting a continuous process, especially for high-risk reactions such as sulfonation and fluorination, manual intervention and material transfer can be reduced, and safety risks can be reduced. At the same time, the use of continuous reactors makes the reaction conditions more stable, improves the selectivity and yield of the reaction, shortens the production cycle, and reduces energy consumption and material waste. Controlling the feed rate and setting the dosage, using advanced flow meters and automatic feeding systems, can ensure the accurate material ratio of each reaction step, reduce the generation of by-products, and improve the yield. Accurately setting the reaction temperature and pressure, such as bromination reaction at 40~60℃, is conducive to improving the reaction rate and conversion rate, while reducing the risk of safety accidents caused by excessive temperature. Continuous concentration is carried out at a specific temperature and vacuum pressure, which helps to effectively separate the product and reduce energy consumption. Continuous extraction and concentration processes, such as the treatment of the second organic phase in the continuous extraction component, can effectively reduce impurities and improve the purity of the target product. The continuous reduction reaction in the continuous reduction component is carried out under mild conditions, avoiding the catalyst deactivation and product decomposition that may be caused by high temperature and high pressure. Continuous reduction uses a fixed bed reactor, which reduces the loss of catalysts and safety risks during the recovery process. The precise control of solvent in continuous batching improves the utilization rate of solvent and reduces production costs.

[0226] In a preferred embodiment, the continuous production method further includes: controlling the continuous diazotization product to be delivered to the second continuous quenching component 414 at a feed rate of 150 / min~250 / min, and controlling the urea holding component 316 to be continuously delivered to the second continuous quenching component 414 at a twelfth set dosage, and continuously quenching under the conditions of a quenching temperature of 10~20°C and a quenching residence time of 10min~30min to obtain a second quenching product system; controlling the second quenching product system to be delivered to the fluorination reaction component 415 at a feed rate of 300g / min~600g / min, and controlling the hydrofluoric acid storage component 317 to continuously deliver hydrofluoric acid to the fluorination reaction component 415 at a thirteenth set dosage, and continuously fluorinating under the conditions of a first catalyst, a reaction temperature of 40°C~80°C, and a reaction residence time of 30min~90min to obtain a first fluorination product. ; Control the first fluorination product to be delivered to the second continuous distillation component 902 at a dosage of 200 g / min~500 g / min, and continuously distill under the conditions of a second distillation temperature of 40°C~60°C and a second distillation pressure of -0.08 MPa~-0.1 MPa to obtain 3,4,5-trifluorobromobenzene; wherein the quenching temperature is 10°C~20°C, and the concentration of hydrofluoric acid is 30%~50%; and / or, the type of the first catalyst is One or more of cuprous oxide, cupric sulfate, and cupric oxide; and / or, the amount of the first catalyst is 0.005g~0.02g per 1g of the second quenched product system; and / or, the twelfth set amount is 0.8g~1.6g of urea contained in every 1g of the continuous diazotization product; and / or, the thirteenth set amount is 0.03g~0.1g of hydrofluoric acid added per 1g of the second quenched product.

[0227] By replacing traditional batch reactions with continuous reactions, especially the highly dangerous sulfonation and fluorination reactions, manual on-site operations are avoided, the risk of contact with hazardous chemicals such as hydrofluoric acid is reduced, and the safety of the production process is improved. The continuous process shortens the reaction time, reduces material transfer, and improves production efficiency. Especially in highly exothermic reactions such as nitration, bromination, and fluorination, continuous reactions reduce heat accumulation, avoid the occurrence of danger, and improve the continuity and controllability of the reaction. Continuous reactions reduce the size of equipment and reduce equipment investment costs. The continuous post-treatment process reduces the use of solvents, reduces purification costs and the amount of three wastes discharged. The entire production process has a high degree of automation, reduces manual operations, and reduces labor costs. Continuous batching technology ensures the precise ratio of reactants, improves the selectivity of the reaction and the yield of the product. The continuous process also helps to improve the utilization rate of raw materials and reduce the generation of by-products.

[0228] The beneficial effects of the present application are further illustrated by examples below:

[0229] Example 1

[0230] like Figure 1As shown, the first raw material tank 301 (o-dichlorobenzene storage tank) is connected to the inlet of the continuous sulfonation reaction tank 401 through a pipeline, and o-dichlorobenzene is continuously supplied through the o-dichlorobenzene feeding pump 101 and the first liquid flowmeter 201. The second raw material tank 302 (chlorosulfonic acid storage tank) is connected to the inlet of the continuous sulfonation reaction tank 401 through a pipeline, and chlorosulfonic acid is continuously supplied through the chlorosulfonic acid feeding pump 102 and the second liquid flowmeter 202 to perform a continuous sulfonation reaction. The outlet of the continuous sulfonation reaction tank 401 is connected to the inlet of the continuous water washing component 402 (a fully mixed reactor or a dynamic tubular reactor) through a pipeline, and water is continuously supplied through the first water feed pump 103 and the third liquid flowmeter 203 to perform continuous water washing to obtain a continuous water washing product. The outlet of the continuous water washing component 402 is connected to the first continuous liquid separation component 601 (a centrifugal extractor, a continuous extraction column or a static liquid separation machine). The first continuous liquid separation unit 601 is connected to a first continuous quenching unit 404 (a first continuous quenching unit or a second continuous quenching unit) to continuously separate the water-washed product to obtain a first organic phase. The organic phase outlet of the first continuous liquid separation unit 601 is connected to the inlet of the continuous nitration unit 403 (a dynamic tubular reactor or a fully mixed reactor); the first acid storage tank 304 supplies the first acid solution to the continuous nitration unit 403 through the second sulfuric acid feed pump 104 and the fourth liquid flowmeter 204 to perform continuous nitration in the continuous nitration unit 403. The outlet of the continuous nitration unit 403 is connected to the first continuous quenching unit 404. The continuous nitration product is continuously quenched to obtain a continuous quenching product. The outlet of the first continuous quenching unit 404 is connected to the first continuous filtering unit 701 (a candle filter or a horizontal screw centrifuge) to continuously filter the continuous quenching product to obtain a continuous filtration product. The outlet of the first continuous filtering unit 701 is connected to the first continuous batching unit 405;The first solvent storage tank 306 supplies solvent to the first continuous batching component 405 through the second liquid feed pump 106 and the sixth liquid flow meter 206 to perform continuous batching to obtain a first continuous batching product. The outlet of the first continuous batching component 405 is connected to the first liquid storage tank 307 to transport the first continuous batching product into the first liquid storage tank 307. The first liquid storage tank 307 is connected to the continuous esterification component 406 to continuously transport the first continuous batching product therein. The first solid feeder 503 supplies solid to the continuous esterification component 406. The outlet of the continuous esterification component 406 is connected to the continuous chlorine-based fluorination component 408 through the second continuous filtering component 702 (candle filter or horizontal screw centrifuge), and the dimethylformamide storage tank 308 supplies the solvent to the second continuous batching component 407 through the fourth liquid feed pump 108 and the eighth liquid flow meter 208 to perform continuous batching to obtain a second continuous batching product. The outlet of the second continuous batching component 407 is connected to the second liquid storage tank 309, and the second continuous batching product is transported to the second liquid storage tank 309. Temporary storage, the second liquid storage tank 309 is connected to the continuous chlorine-based fluorination component 408 through a pipeline, the second continuous filtering component 702 and the first continuous concentrating component 801 (falling film evaporator, etc.) are connected in series to perform continuous filtration and concentration, the outlet of the first continuous concentrating component 801 is connected to the second continuous batching component 407 to perform continuous batching and preparation for fluorination, the second solid feeder 505 supplies the fluorinating agent to the continuous chlorine-based fluorination component 408, the outlet of the continuous chlorine-based fluorination component 408 is connected to the continuous bromination unit, and the outlet of the first continuous concentrating component 801 is connected to the continuous water The continuous hydrolysis reaction part 409 is connected to a first continuous rectification part 901 (a plate-type or packed rectification tower) for continuous rectification. The outlet of the first continuous rectification part 901 is connected to a continuous bromination reaction part 410. The third solid feeder 506 supplies a brominating agent to the continuous bromination reaction part 410.The second acid storage tank 311 supplies the second acid liquid to the continuous bromination reaction unit 410 through the first sulfuric acid feed pump 111 and the eleventh liquid flow meter 211, and the outlet of the continuous bromination reaction unit 410 is connected to the continuous extraction unit 1101 (continuous extraction column or centrifugal extractor) for continuous extraction. The third solvent storage tank 312 supplies the solvent to the third continuous dosing unit 411 through the ethanol feed pump 112 and the twelfth liquid flow meter 212, and the outlet of the third continuous dosing unit 411 is connected to the third liquid storage tank 313 for continuous reduction, and the outlet of the third liquid storage tank 313 is connected to the continuous reduction unit 1001 for continuous reduction reaction, and the outlet of the continuous reduction unit 1001 is connected to the third continuous concentrating unit 803 for continuous concentration, and the outlet of the third continuous concentrating unit 803 is connected to the fourth continuous dosing unit 412; the third acid storage tank 314 supplies the second acid liquid to the continuous bromination reaction unit 410 through the third sulfuric acid feed pump 114 and the thirteenth liquid flow meter 212, and the outlet of the third continuous dosing unit 411 is connected to the third liquid storage tank 313 for continuous reduction, and the outlet of the third liquid storage tank 313 is connected to the continuous reduction unit 1001 for continuous reduction reaction, and the outlet of the continuous reduction unit 1001 is connected to the third continuous concentrating unit 803 for continuous concentration, and the outlet of the third continuous concentrating unit 803 is connected to the fourth continuous dosing unit 412; The liquid flow meter 214 supplies the third acid solution to the fourth continuous dosing component 412, and the outlet of the fourth continuous dosing component 412 is connected to the continuous diazo component 413; the nitrosyl sulfuric acid storage component 315 supplies nitrosyl sulfuric acid to the continuous diazo component 413 through the nitrosyl sulfuric acid feed pump 115 and the fourteenth liquid flow meter 215, and the outlet of the continuous diazo component 413 is connected to the second continuous quenching component 414, and the urea solution is supplied through the urea solution feed pump 116 and the fifteenth liquid flow meter 216, and the outlet of the second continuous quenching component 414 is connected to the fluorination reaction component 415; the hydrofluoric acid storage component 317 supplies hydrofluoric acid through the hydrofluoric acid feed pump 117 and the sixteenth liquid flow meter 217, and the outlet of the fluorination reaction component 415 is connected to the second continuous distillation component 902 (plate type or packing type distillation tower), and continuous distillation is performed to finally obtain the product 3,4,5-trifluorobromobenzene and send it to the product tank 318. ;

[0231] Example 2

[0232]

[0233] The o-dichlorobenzene feeding pump 101 is controlled to continuously deliver o-dichlorobenzene to the continuous sulfonation reaction tank 401 at a feeding rate of 10.0 g / min, and the chlorosulfonic acid feeding pump 102 is controlled to continuously deliver chlorosulfonic acid to the continuous sulfonation reaction tank 401 at a feeding rate of 16.0 g / min. The reaction tank is kept at a temperature of 60° C. for 120 minutes to perform a continuous sulfonation reaction to obtain a system containing 3,4-dichlorobenzenesulfonyl chloride. The system is controlled to continuously deliver the system to the continuous water washing component 402 at a feeding rate of 26.0 g / min, and water is controlled to continuously deliver the system to the continuous water washing component 402 at a rate of 15.0 g / min. The system is washed with water at 5° C. for 10 minutes to obtain a system containing 3,4-dichlorobenzenesulfonyl chloride. The system is transported to the first continuous liquid separation component 601 at a feed rate of 41.0 g / min for continuous liquid separation. The yield of the first organic phase obtained after liquid separation is 91.3% (the first organic phase here is 3,4-dichlorobenzenesulfonic acid). The obtained first organic phase is transported to the continuous nitration component 403 at a feed rate of 14.0 g / min, and the first acid solution (98% concentrated sulfuric acid) is controlled to be transported to the continuous nitration component 403 at a feed rate of 30.0 g / min, and potassium nitrate is controlled to be transported to the continuous nitration component 403 at a feed rate of 16.8 g / min, and stays at a temperature of 10°C for 60 minutes. The system containing 3,4-dichloro-5-nitrobenzenesulfonic acid is obtained at a rate of 6 The feed rate of 0.8 g / min was transported to the first continuous quenching component 404, and the pure water with a feed rate of 121.6 g / min was continuously quenched in the first continuous quenching component 404, and the mixture was kept at 5°C for 10 min. The obtained system containing 3,4-dichloro-5-nitrobenzenesulfonic acid entered the first continuous filtering component 701 at a feed rate of 182.4 g / min for continuous filtration, and the yield of the obtained product system was 89.6%. The obtained product system was continuously transported to the first continuous dosing component 405 at a feed rate of 15.7%, and the mixture was continuously mixed with methanol at a feed rate of 27.0 g / min. The mixture was stopped at a dosing temperature of 30°C. The system containing 3,4-dichloro-5-nitrobenzenesulfonic acid was transported to the first liquid storage tank 307 at a feed rate of 42.8 g / min for temporary storage. The system containing 3,4-dichloro-5-nitrobenzenesulfonic acid was continuously transported to the continuous esterification component 406 at a feed rate of 42.8 g / min, mixed with potassium carbonate at a feed rate of 44.9 g / min, and kept at 60°C for 60 min. The system containing methyl 3,4-dichloro-5-nitrobenzenesulfonate was transported to the second continuous filtering component 702 at a feed rate of 87.7 g / min for continuous filtration. The filtration system containing methyl 3,4-dichloro-5-nitrobenzenesulfonate was filtered at a rate of 41.The feed rate of 2 g / min was transported to the first continuous concentration component 801, and the concentration temperature was kept at 50°C for 30 min to obtain 3,4-dichloro-5-nitrobenzenesulfonic acid methyl ester, and the yield was 92.3%. The obtained 3,4-dichloro-5-nitrobenzenesulfonic acid methyl ester was continuously transported to the second continuous dosing component 407, and dimethylformamide (DMF) was controlled to be transported to the second continuous dosing component 407 at a feed rate of 26.8 g / min, and was continuously mixed with the 3,4-dichloro-5-nitrobenzenesulfonic acid methyl ester in the second continuous dosing component 407 at a temperature of 20°C and a residence time of 20 min. The obtained 3,4-dichloro-5-nitrobenzenesulfonic acid methyl ester was The system containing methyl 3,4-dichloro-5-nitrobenzenesulfonate is transported to the second liquid storage tank 309 at a rate of 40.2 g / min for temporary storage, and the system containing methyl 3,4-dichloro-5-nitrobenzenesulfonate is controlled to be transported to the continuous chlorine-based fluorination component 408 at a feeding rate of 40.2 g / min. At the same time, potassium fluoride is controlled to be transported to the continuous chlorine-based fluorination component 408 at a feeding rate of 6.2 g / min and tetraphenylphosphonium bromide is controlled to be transported to the continuous chlorine-based fluorination component 408 at a feeding rate of 8.1 g / min. The system is kept at 120° C. for 3 hours, and the system containing methyl 3,4-dichloro-5-nitrobenzenesulfonate is transported to the second continuous concentration component 802 at a feeding rate of 54.5 g / min for continuous concentration, and a mixed solution containing methyl 3,4-dichloro-5-nitrobenzenesulfonate is obtained. The product was transported to the continuous hydrolysis reaction part 409 at a rate of 27.7 g / min, and stayed at 20°C for 60 min with pure water at a feed rate of 83.1 g / min. The yield of the obtained system containing 2,3-difluoronitrobenzene was 71.3%; the system containing 2,3-difluoronitrobenzene was transported to the first continuous distillation part 901, and the feed rate of dibromohydantoin was controlled to be 4.9 g / min, and the second acid solution (81%~98% sulfuric acid) was continuously transported to the continuous bromination reaction part 410 at a rate of 9.9 g / min, and stayed at 60°C for 60 min. The system containing 3,4-difluoro-5-nitrobromobenzene was continuously transported at a rate of 19.7 g / min. The mixture was sent to the continuous extraction part 1101 and continuously mixed and extracted with tap water at a feed rate of 60 g / min, and the yield of the second organic phase was 81.9% (the second organic phase was 3,4-difluoro-5-aminobromobenzene). The second organic phase was sent to the third continuous dosing part 411 at a rate of 6.39 g / min, and mixed with ethanol at a feed rate of 19.2 g / min at a temperature of 20°C for 30 mi. The obtained 3,4-difluoro-5-nitrobromobenzene was sent to the continuous reduction part 1001 at a rate of 25.6 g / min, and a continuous reduction reaction occurred in the atmosphere of hydrogen with Raney nickel as the reducing agent. The obtained 3,4-difluoro-5-nitrobromobenzene system was 26.7g / min is transported to the third continuous concentration component 803 for continuous concentration, and the obtained 3,4-difluoro-5-aminobromobenzene is 95%. The obtained 3,4-difluoro-5-aminobromobenzene is transported to the fourth continuous dosing component 412 at a rate of 4.1g / min, and mixed with the third acid solution (50% sulfuric acid) at a feed rate of 31.2g / min. The obtained system containing 3,4-difluoro-5-aminobromobenzene is transported to the continuous diazo component 413 at a feed rate of 35.3g / min, and mixed with 50% nitrosylsulfuric acid at a feed rate of 140.2%g / min in the continuous diazo component 413, and stays at a temperature of -10°C for 30min The obtained diazotization product system was transported to the second continuous quenching component 414 at a rate of 171.4 g / min, and mixed with a 30% urea aqueous solution at a feed rate of 154.26 g / min at 10°C for quenching for 20 minutes; the obtained diazonium salt-containing product system was transported to the fluorination reaction component 415 at a rate of 325.7 g / min, and stayed with cuprous oxide and hydrofluoric acid solution at a feed rate of 31.6 g / min at a reaction temperature of 60°C for 60 minutes, and the obtained system containing 3,4,5-trifluorobromobenzene was transported to the second continuous distillation component 902 for continuous distillation to obtain the final product 3,4,5-trifluorobromobenzene with a yield of 86.8%. .

[0234] Example 3

[0235] The similarities between the present embodiment and embodiment 2 are not repeated here. The difference is that the reaction temperature of the continuous sulfonation in the continuous sulfonation reaction tank 401 is changed from 60° C. in embodiment 1 to 50° C., and the other conditions remain unchanged. The yield of 3,4-dichlorobenzenesulfonic acid is 89.4%.

[0236] Example 4

[0237] The similarities between the present embodiment and embodiment 2 are not repeated here. The difference is that during the esterification, the esterification time is changed from the original 60 min to 45 min, and the yield of 3,4-dichloro-5-nitrobenzenesulfonic acid methyl ester is 78.5%.

[0238] Example 5

[0239] The similarities between the present embodiment and the embodiment 2 are not repeated here. The difference is that the bromide in the bromination reaction is changed from dibromohydantoin in the embodiment 1 to N-bromosuccinimide, and the yield of the obtained second organic phase is 84.4% (the second organic phase is 3,4-difluoro-5-aminobromobenzene).

[0240] Example 6

[0241] The similarities between the present embodiment and embodiment 1 are not repeated here. The difference is that the catalyst of the fluorination reaction is changed from cuprous oxide in embodiment 1 to cuprous sulfate, and the yield of the final product 3,4,5-trifluorobromobenzene is 84.7%.

[0242] From the above description, it can be seen that the above embodiments of the present invention achieve the following technical effects: by changing the traditional batch reaction into a continuous reaction, frequent manual operation and material transfer are avoided, and the frequency of personnel contact during the operation of highly dangerous chemicals is reduced, thereby significantly improving the safety of the production process. During the reaction process, since the reactions of each part are continuous, the heat loss during the reaction process is reduced, the energy required for cooling and heating is reduced, and the standing time of the material during the reaction process is reduced, which effectively reduces the overall energy consumption. The continuous reaction reduces the use of solvents, reduces the generation of wastewater, waste gas and solid waste, is beneficial to environmental protection and reduces production costs. In addition, the use of a continuous reaction device avoids the transmission of The "cleaning-loading-reaction-unloading-cleaning" cycle process of the traditional batch reaction increases the continuous operation time of the equipment, thereby improving the equipment utilization rate. Continuous production reduces manual intervention and reduces the dependence on operating skills. It also reduces the number of employees and reduces labor costs. In the continuous production process, the continuous flow of raw materials and products reduces the storage time of materials, reduces the risk of material deterioration, and optimizes material management. The continuous reaction device can also adjust the reaction speed and scale according to production needs, which improves the flexibility of the production system and can quickly respond to market changes. Continuous production reduces the volume of reaction equipment to a certain extent and reduces equipment investment costs. At the same time, the reduced amount of solvent in the post-treatment process also helps to reduce production costs.

[0243] 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.

[0244] 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.

[0245] 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.

[0246] 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.

[0247] 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.

[0248] 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 continuous production device for 3,4,5-trifluorobromobenzene, characterized in that: include: A continuous feeding device, the continuous feeding device is used to continuously supply a first reaction raw material and a second reaction raw material, the first reaction raw material is o-dichlorobenzene, and the second reaction raw material is chlorosulfonic acid; A continuous sulfonation reaction tank (401), the inlet of which is connected to the outlet of the continuous feeding device, for providing a reaction place for the first reaction raw material and the second reaction raw material to perform a continuous sulfonation reaction to obtain a continuous sulfonation product; A continuous post-treatment device, wherein the inlet of the continuous post-treatment device is connected to the outlet of the continuous sulfonation reaction tank (401) to continuously post-treat the continuous sulfonation product and obtain 3,4,5-trifluorobromobenzene.

2. The continuous production equipment of 3,4,5-trifluorobromobenzene according to claim 1, characterized in that: The continuous feeding device comprises: A first raw material tank (301), wherein the outlet of the first raw material tank (301) is connected to the inlet of the continuous sulfonation reaction tank (401), so as to continuously transport the first reaction raw material stored in the first raw material tank (301) to the continuous sulfonation reaction tank (401); The second raw material tank (302), the outlet of the second raw material tank (302) is connected to the inlet of the continuous sulfonation reaction tank (401), so as to continuously transport the second reaction raw material stored in the second raw material tank (302) to the continuous sulfonation reaction tank (401).

3. The continuous production equipment of 3,4,5-trifluorobromobenzene according to claim 1, characterized in that: The continuous post-processing device comprises: A continuous nitration unit, wherein the inlet of the continuous nitration unit is connected to the outlet of the continuous sulfonation reaction tank (401) to continuously nitrate the continuous sulfonation product and obtain a continuous nitration product; A continuous esterification unit, wherein the inlet of the continuous esterification unit is connected to the outlet of the continuous nitration unit to continuously esterify the continuous nitration product and obtain a continuous esterification product; A continuous chlorine-based fluorination unit, wherein the inlet of the continuous chlorine-based fluorination unit is connected to the outlet of the continuous esterification unit to continuously chlorine-based fluorination the continuous esterification product to obtain a continuous chlorine-based fluorination product; A continuous bromination unit, wherein the inlet of the continuous bromination unit is connected to the outlet of the continuous chlorination fluorination unit to continuously bromine the continuous chlorination fluorination product and obtain a continuous bromination product; A continuous diazotization unit, wherein the inlet of the continuous diazotization unit is connected to the outlet of the continuous bromination unit to continuously diazotize the continuous bromination product and obtain a continuous diazotization product; A continuous fluorination unit, wherein the inlet of the continuous fluorination unit is connected to the outlet of the continuous diazotization unit, so as to continuously fluorinate the continuous diazotization product and obtain the 3,4,5-trifluorobromobenzene.

4. The continuous production equipment of 3,4,5-trifluorobromobenzene according to claim 3, characterized in that: The continuous nitrification unit comprises: A continuous water washing component (402), wherein the inlet of the continuous water washing component (402) is connected to the continuous sulfonation reaction tank (401), so as to continuously wash the continuous sulfonation product with water to obtain a continuous water washing product; a first continuous liquid separation component (601), wherein the inlet of the first continuous liquid separation component (601) is connected to the outlet of the continuous water washing component (402), so as to continuously separate the continuous water washing product system and obtain a first organic phase; A continuous nitration component (403), the continuous nitration component (403) is used to provide a continuous nitration reaction site, and the inlet end of the continuous nitration component (403) is connected to the outlet end of the first continuous liquid separation component (601); A first acid storage tank (304), wherein the outlet of the first acid storage tank (304) is connected to the inlet of the continuous nitration component (403) so as to transport the first acid liquid into the continuous nitration component (403) and mix the first acid liquid with the first organic phase in the continuous nitration component (403) to obtain the continuous nitration product; and the outlet of the continuous nitration component (403) is connected to the continuous esterification unit.

5. The continuous production equipment of 3,4,5-trifluorobromobenzene according to claim 3, characterized in that: The continuous esterification unit comprises: A third raw material tank (305), wherein the third raw material tank (305) is used to store a quenching agent; a first continuous quenching component (404), wherein the inlet of the first continuous quenching component (404) is respectively connected to the outlet of the third raw material tank (305) and the outlet of the continuous nitration unit, so as to continuously quench the continuous nitration product using the quenching agent to obtain a continuous quenching product; a first continuous filtering component (701), wherein the inlet of the first continuous filtering component (701) is connected to the outlet of the first continuous quenching component (404) so ​​as to continuously filter the continuous quenching product to obtain a continuous filtration product; a first continuous dosing component (405), wherein the inlet of the first continuous dosing component (405) is connected to the outlet of the first continuous filtering component (701) to provide a continuous dosing reaction site for the continuous filtering product; a first solvent storage tank (306), wherein the outlet of the first solvent storage tank (306) is in communication with the first continuous dosing component (405) so as to continuously dosing the continuously filtered product in the first continuous dosing component (405) and obtain a first continuously dosing product, and the first continuously dosing product is transported to a first liquid storage tank (307) in communication with the outlet of the first continuous dosing component (405) for temporary storage; A continuous esterification component (406), wherein the outlet of the first liquid storage tank (307) is connected to the inlet of the continuous esterification component (406) so as to transport the first continuous batching product into the continuous esterification component (406); A first solid feeder (503) has an outlet connected to the inlet of the continuous esterification component (406) to deliver a first solid additive into the continuous esterification component (406) so that the first solid additive is mixed with the first continuous batching product to carry out the continuous esterification to obtain the continuous esterification product. The outlet of the continuous esterification component (406) is connected to the continuous chlorine-based fluorination unit.

6. The continuous production equipment of 3,4,5-trifluorobromobenzene according to claim 3, characterized in that: The continuous chlorine-based fluorination unit comprises: a second continuous filtering component (702), wherein the inlet of the second continuous filtering component (702) is connected to the continuous esterification unit to continuously filter the continuous esterification product to obtain a second continuous filtering product; a first continuous concentrating component (801), wherein the inlet of the first continuous concentrating component (801) is connected to the outlet of the second continuous filtering component (702), so as to continuously concentrate the second continuous filtering product to obtain a first continuous concentrated product; a second continuous dosing component (407), wherein the inlet of the second continuous dosing component (407) is connected to the outlet of the first continuous concentration component (801) to provide a continuous dosing reaction site for the first continuous concentration product; a dimethylformamide storage tank (308), wherein the outlet of the dimethylformamide storage tank (308) is connected to the second continuous batching component (407), so that the dimethylformamide stored in the dimethylformamide storage tank (308) is transported to the second continuous batching component (407) and mixed with the first continuous concentrated product in the second continuous batching component (407) to perform continuous batching to obtain a second continuous batching product, and the second continuous batching product is transported to a second liquid storage tank (309) connected to the outlet of the second continuous batching component (407) for storage; A continuous chlorine-based fluorination component (408), wherein the inlet of the continuous chlorine-based fluorination component (408) is connected to the outlet of the second liquid storage tank (309) to provide a continuous fluorination reaction site; A second solid feeder (505), the outlet of which is connected to the continuous chlorine-based fluorination component (408) to transport the fluorinating agent and continuously mix it with the second continuous batching product to obtain the continuous chlorine-based fluorination product, and the outlet of the continuous chlorine-based fluorination component (408) is connected to the continuous bromination unit.

7. The continuous production equipment of 3,4,5-trifluorobromobenzene according to claim 3, characterized in that: The continuous brominated units include: a second continuous concentrating component (802), wherein the inlet of the second continuous concentrating component (802) is connected to the outlet of the continuous chlorine-based fluorination unit to continuously concentrate the continuous chlorine-based fluorination product to obtain a second continuous concentrated product; A continuous hydrolysis reaction component (409), wherein the inlet of the continuous hydrolysis reaction component (409) is connected to the outlet of the second continuous concentration component (802) to provide a continuous hydrolysis reaction site; A water storage component (310), wherein the outlet of the water storage component (310) is connected to the inlet of the continuous hydrolysis reaction component (409) to transport water and mix the water with the second continuous concentrated product in the continuous hydrolysis reaction component (409) to perform continuous hydrolysis to obtain a continuous hydrolyzed product; a first continuous distillation component (901), wherein the inlet of the first continuous distillation component (901) is connected to the outlet of the continuous hydrolysis reaction component (409) to continuously distill the continuous hydrolysis product to obtain a continuous distillation product; A continuous bromination reaction component (410), wherein the inlet of the continuous bromination reaction component (410) is connected to the outlet of the first continuous distillation component (901), providing a continuous bromination reaction site; a third solid feeder (506), wherein the outlet of the third solid feeder (506) is connected to the inlet of the continuous bromination reaction unit (410) to transport the brominating agent; A second acid storage tank (311), wherein the outlet of the second acid storage tank (311) is connected to the inlet of the continuous bromination reaction component (410) to transport the second acid solution and mix it with the brominating agent and the continuous distillation product to perform continuous bromination to obtain the continuous bromination product, and the outlet of the continuous bromination reaction component (410) is connected to the continuous diazotization unit.

8. The continuous production equipment of 3,4,5-trifluorobromobenzene according to claim 3, characterized in that: The continuous diazotization unit comprises: A continuous extraction component (1101), wherein the inlet of the continuous extraction component (1101) is connected to the outlet of the continuous bromination unit to continuously extract the continuous bromination product to obtain a second organic phase; a third solvent storage tank (312), wherein the outlet of the third solvent storage tank (312) is connected to a third continuous dosing component (411) so as to transport the third solvent therein; the outlet of the continuous extraction component (1101) is connected to the inlet of the third continuous dosing component (411) so as to transport the second organic phase and continuously dosing the second organic phase with the third solvent to obtain a third continuous dosing product; and the third continuous dosing product is transported to a third liquid storage tank (313) connected to the outlet of the third continuous dosing component (411) for storage; A continuous reduction component (1001), wherein the inlet of the continuous reduction component (1001) is connected to the outlet of the third liquid storage tank (313) to continuously reduce the third continuous batching product to obtain a continuous reduction product; A third continuous concentration component (803), whose inlet end is connected to the outlet of the continuous reduction component (1001), so as to continuously concentrate the continuous reduction product to obtain a third continuous concentrated product; a fourth continuous dosing component (412), the inlet end of which is connected to the outlet of the third continuous concentrating component (803) so as to accommodate the third continuous concentrating product; A third acid storage tank (314), whose outlet end is connected to the inlet of the fourth continuous batching component (412), is used to transport the third acid solution into the fourth continuous batching component (412) and mix it with the third continuous concentrated product to perform continuous batching to obtain a third continuous batching product; A continuous diazo component (413), the inlet end of which is connected to the outlet of the fourth continuous batching component (412), and is used to accommodate the third continuous batching product; The outlet of the nitrosylsulfuric acid storage component (315) is connected to the inlet of the continuous diazo component (413) so as to continuously transport nitrosylsulfuric acid into the continuous diazo component (413) and mix it with the third continuous batching product in the continuous diazo component (413) to perform continuous diazotization to obtain the continuous diazotization product. The outlet of the continuous diazo component (413) is connected to the continuous fluorination unit.

9. The continuous production equipment of 3,4,5-trifluorobromobenzene according to claim 3, characterized in that: The continuous fluorination unit comprises: A second continuous quenching component (414), the inlet of which is connected to the outlet of the continuous diazotization unit; a urea containing component (316), the outlet of which is connected to the inlet of the second continuous quenching component (414), so as to continuously deliver urea to the second continuous quenching component (414) and mix the urea with the continuous diazotization product in the second continuous quenching component (414) to perform continuous quenching to obtain a second quenched product system; a fluorination reaction component (415), the inlet of which is connected to the outlet of the second continuous quenching component (414) to accommodate the second quenching product system; A hydrofluoric acid storage component (317), the outlet of which is connected to the inlet of the fluorination reaction component (415) to continuously transport hydrofluoric acid and mix it with the second quenched product system in the fluorination reaction component (415) to obtain a first fluorination product; The inlet end of the second continuous distillation component (902) is connected to the outlet end of the fluorination reaction component (415) to continuously flow the first fluorination product to obtain the 3,4,5-trifluorobromobenzene, and the 3,4,5-trifluorobromobenzene is transported to the product tank (318) for storage.

10. A method for continuous production of 3,4,5-trifluorobromobenzene, characterized in that: The continuous production method is applied to the production equipment according to any one of claims 1 to 9 to prepare the 3,4,5-trifluorobromobenzene, and the production method comprises: Controlling o-dichlorobenzene to be continuously fed to a continuous sulfonation reaction tank (401) at a first feed amount and chlorosulfonic acid to be continuously fed to a second feed amount, respectively, and performing a continuous sulfonation reaction under a first preset condition to obtain a continuous sulfonation product; Controlling the continuous sulfonation product to be continuously transported to a continuous post-processing device for continuous post-processing to obtain 3,4,5-trifluorobromobenzene; Among them, the first preset condition is that the first reaction temperature is 50°C~80°C, the sulfonation reaction time is 120min~130min, the first feed amount is 10g / min~30g / min, and the second feed amount is 1g~3g of the chlorosulfonic acid added to every 1g of the o-dichlorobenzene.

11. The method for continuous production of 3,4,5-trifluorobromobenzene according to claim 10, characterized in that: The continuous production method further comprises: Controlling the continuous sulfonation product to be continuously transported to a continuous nitration unit for continuous esterification to obtain a continuous esterification product; Controlling the continuous esterification product to be continuously transported to a continuous chlorine-based fluorination unit for continuous chlorine-based fluorination to obtain a continuous chlorine-based fluorination product; Controlling the continuous chloro-fluorination product to be continuously delivered to a continuous bromination unit for continuous bromination to obtain a continuous bromination product; Controlling the continuous bromination product to be continuously transported to a continuous diazotization unit to perform continuous diazotization and obtain a continuous diazotization product; The continuous diazotization product is controlled to be continuously transported to a continuous fluorination unit to perform continuous fluorination, and the 3,4,5-trifluorobromobenzene is obtained.

12. The method for continuous production of 3,4,5-trifluorobromobenzene according to claim 10, characterized in that: The continuous production method further comprises: Controlling the continuous sulfonation product to be delivered to the continuous water washing component (402) at a third feed rate, so as to continuously wash the continuous sulfonation product with water at a set water volume under a second preset condition, and obtaining a continuous water washing product; Controlling the continuous water-washing product to enter the first continuous liquid separation component (601) at a fourth feed rate to perform continuous liquid separation under a third preset condition, and obtaining a first organic phase; Controlling the first organic phase to be delivered to the continuous nitration component (403) at a fifth feed rate, and at the same time, controlling the first acid solution to be delivered to the continuous nitration component (403) at a set acid solution rate, and performing continuous nitration under the action of the nitrating agent at a fourth preset condition to obtain the continuous nitration product; in, The third feed rate is 15 g / min to 45 g / min, and the set water volume is 0.5 ml to 1.5 ml of water per 1 g of the third feed rate; and / or, The second preset condition is that the water washing temperature is 5°C to 10°C and the water washing time is 10min to 30min; and / or, The fourth feed rate is 20 g / min to 60 g / min; and / or, The third preset condition is that the first continuous liquid separation temperature is 20°C to 40°C; and / or, The first continuous separation time is 5min to 10min; and / or, The fifth feed rate is 10 g / min to 15 g / min, and the set acid solution amount is 30 g to 45 g of the first acid solution contained in 1 g of the third feed rate; and / or, The nitrating agent is one or more of potassium nitrate, sodium nitrate and concentrated nitric acid; and / or, The amount of the nitrating agent used is 0.8 g to 1.5 g per 1 g of the third feed amount; and / or, The fourth preset condition is that the nitration temperature is 0°C to 20°C, and the nitration time is 60min to 180min; and / or, The first acid solution is concentrated sulfuric acid with a mass concentration of 81% to 98%.

13. The continuous production method of 3,4,5-trifluorobromobenzene according to claim 10, characterized in that: The continuous production method further comprises: Controlling the continuous nitration unit in the continuous post-treatment device to continuously nitrate the continuous sulfonation product to obtain a continuous nitration product, which is transported to the first continuous quenching component (404) at a sixth feed rate, and continuously quenching the continuous nitration product under a fifth preset condition with a solvent having a set solvent amount, to obtain the continuous quenching product; Controlling the continuous quenching product to be delivered to the first continuous filtering component (701) at a seventh feed rate, and performing continuous filtration under a sixth preset condition to obtain a continuous filtration product; Controlling the continuous filtration product to be delivered to the first continuous dosing component (405) at an eighth feed rate, and controlling the first solvent in the first solvent storage tank (306) to be delivered to the first continuous dosing component (405) at a first set amount, performing continuous dosing under a sixth preset condition, and obtaining a first continuous dosing product; Controlling the first continuous batching product to be delivered to the continuous esterification component (406) at a feed rate of 30 g / min to 80 g / min, and at the same time controlling the first solid feeder (503) to deliver the first solid additive to the continuous esterification component (406) at a second set amount, and performing continuous esterification at a temperature of 40° C. to 70° C. for an esterification time of 30 min to 180 min, so as to obtain the continuous esterification product; in, The sixth feed rate is 50 g / min to 120 g / min, and the set solvent amount is 1 ml to 3 ml of the solvent added per 1 g of the sixth feed rate; and / or, The solvent is one or more of tap water, purified water and deionized water; and / or, The fifth preset condition is that the temperature of the first continuous quenching is 5°C to 20°C, and the first continuous quenching time is 10min to 30min; and / or, The seventh feed rate is 200 g / min to 420 g / min; and / or, The sixth preset condition is that the first continuous filtration temperature is in the range of 10°C to 20°C, and the first continuous filtration time is 10min to 30min; and / or, The eighth feed rate is 10 g / min to 15 g / min, the sixth preset condition is that the first continuous batching temperature is 20° C. to 50° C., the first continuous batching time is 10 min to 30 min, and the first set dosage is 2 ml to 5 ml of the first solvent added per 1 g of the eighth feed rate; and / or, The second set dosage is 1.2 g to 3.5 g of the first solid additive added per 1 g of the first continuously batched product; and / or, The first solid additive is any one or more of potassium carbonate, cesium carbonate and sodium carbonate.

14. The method for continuous production of 3,4,5-trifluorobromobenzene according to claim 10, characterized in that: The method further comprises: Controlling the continuous esterification unit in the continuous post-treatment device to continuously esterify the continuous nitration product to obtain a continuous esterification product, and conveying the continuous esterification product to the second continuous filtering component (702) at a feed rate of 50 g / min to 150 g / min, and continuously filtering under the conditions of a filtration temperature of 10° C. to 30° C. and a filtration time of 10 min to 30 min, to obtain a second continuous filtration product; Controlling the second continuous filtration product to be transported to the first continuous concentration component (801) at a feed rate of 30 g / min to 80 g / min, and continuously concentrating under the conditions of a first concentration temperature of 40° C. to 60° C., a first concentration pressure of -0.06 MPa to -0.1 MPa, and a first concentration time of 30 min to 60 min, so as to obtain a first continuous concentrated product; Controlling the first continuous concentrated product to be delivered to the second continuous batching component (407) at a feed rate of 10 g / min to 15 g / min, and controlling the second solvent in the dimethylformamide storage tank (308) to be continuously batched at a third set amount at a temperature of 20° C. to 40° C. for a batching time of 10 min to 30 min, so as to obtain a second continuous batching product; Controlling the second continuous batching product to be delivered to the continuous chlorine-based fluorination component (408) at a feed rate of 25 g / min to 80 g / min, and controlling the second solid feeder (505) to continuously deliver the fluorinating agent to the continuous chlorine-based fluorination component (408) at a fourth set amount, and continuously mixing under the condition of a fifth set amount of catalyst to obtain the continuous chlorine-based fluorination product; in, The type of the second solvent is one or more of N,N-dimethylformamide and N,N-dimethylacetamide; and / or, The type of the fluorinating agent is one or more of potassium fluoride, sodium fluoride, and boron trifluoride; and / or, The type of the catalyst is one or more of tetraphenylphosphonium bromide and 4-bromobenzyltriphenylphosphonium bromide; and / or, The third set dosage is 2 mL to 5 mL of dimethylformamide added per 1 g of the first continuous concentrated product; and / or, The fourth set dosage is 0.15 g to 0.3 g of the fluorinating agent added per 1 g of the second continuous batching product; and / or, The fifth set dosage is that the dosage of the catalyst added per 1 g of the second continuously batched product is 0.1 g to 0.5 g.

15. The method for continuous production of 3,4,5-trifluorobromobenzene according to claim 10, characterized in that: The method further comprises: Controlling the continuous chlorination unit in the continuous post-treatment device to continuously chlorinate the continuous esterification product to obtain a continuous chlorination fluorination product, and conveying the continuous chlorination fluorination product to the second continuous concentration component (802) at a feed rate of 40 g / min to 100 g / min, and continuously concentrating at a concentration temperature of 90° C. to 140° C., a concentration pressure of -0.06 MPa to 0-0.1 MPa, and a concentration time of 30 min to 60 min to obtain a second continuous concentrated product; The second continuous concentrated product is controlled to be delivered to the continuous hydrolysis reaction part (409) at a feed rate of 20 g / min to 50 g / min, and the water storage part (310) is controlled to deliver a sixth set amount of water to the continuous hydrolysis reaction part (409), and continuous hydrolysis is performed under the conditions of a hydrolysis temperature of 10° C. to 50° C. and a hydrolysis time of 60 min to 180 min to obtain a continuous hydrolysis product; Controlling the continuous hydrolysis product to be transported to the first continuous distillation component (901) at a feed rate of 40 g / min to 100 g / min, and continuously distilling at a distillation temperature of 100° C. to 180° C. and a distillation pressure of -0.08 MPa to -0.1 MPa to obtain a continuous distillation product; Controlling the continuous distillation product to be fed into the continuous bromination reaction part (410) at a feed rate of 3 g / min to 10 g / min, controlling the third solid feeder (506) to continuously feed the brominating agent into the continuous bromination reaction part (410) at a seventh set amount, and controlling the second acid solution in the second acid storage tank (311) to be fed into the continuous bromination reaction part (410) at an eighth set amount, and performing continuous bromination under the conditions of a bromination temperature of 40° C. to 60° C. and a bromination time of 30 min to 90 min, to obtain the continuous bromination product; Wherein, the type of brominating agent is one or more of dibromohydantoin, bromine, and N-bromosuccinimide; and / or, The sixth set dosage is 3 mL to 5 mL of water added per 1 g of the second continuously concentrated product; and / or, The seventh set dosage is 1 g to 2 g of the brominating agent added per 1 g of the second continuously concentrated product; and / or, The eighth set dosage is 2-5 g of the second acid solution added per 1 g of the second continuously concentrated product; and / or, The second acid solution is 81% to 98% sulfuric acid.

16. The method for continuous production of 3,4,5-trifluorobromobenzene according to claim 10, characterized in that: The method further comprises: The continuous bromination product obtained by continuously brominating the continuous chlorofluorination product by controlling the continuous bromination unit in the post-treatment device is continuously transported to the continuous extraction component (1101) at a feed rate of 15 g / min to 30 g / min, and continuously extracted at a temperature of 30° C. to 50° C. and for a time of 15 min to 45 min to obtain a second organic phase; The second organic phase is controlled to be fed at a rate of 5 g / min to 15 g / min, and the third solvent in the third solvent storage tank (312) is continuously transported to the third continuous batching component (411) at a ninth set rate, and the batching is continued at a temperature of 20° C. to 40° C. and a time of 10 min to 30 min, to obtain a third continuous batching product; Controlling the third continuous batching product to be delivered to the continuous reduction component (1001) at a feed rate of 40 g / min to 90 g / min, and continuously reducing it under the conditions of the tenth set amount of reducing agent, the reduction temperature of 40° C. to 80° C., the pressure of 0.3 MPa to 1.0 MPa, and the time of 30 to 60 min to obtain a continuous reduction product; Controlling the continuous reduction product to be transported to the third continuous concentration component (803) at a feed rate of 40 g / min to 90 g / min, and continuously concentrating at a concentration temperature of 40° C. to 60° C. and a concentration pressure of -0.06 MPa to 0-0.1 MPa to obtain a third continuous concentrated product; The third continuous concentrated product is controlled to be fed at a rate of 10 g / min to 15 g / min, and the third acid solution in the third acid storage tank (314) is transported to the fourth continuous batching component (412) at an eleventh set amount, and the batching is continuously performed under the conditions of a reaction temperature of 0° C. to 20° C. and a residence time of 10 min to 20 min, to obtain a third continuous batching product; Controlling the third continuous batching product to be delivered to the continuous diazo component (413) at a feed rate of 30 g / min to 75 g / min, and controlling the nitrosylsulfuric acid storage component (315) to be delivered to the continuous diazo component (413) at a twelfth set amount, so that the third continuous batching product is mixed with the nitrosylsulfuric acid, and a continuous diazotization reaction is carried out under the conditions of a reaction temperature of -20°C to 0°C and a reaction residence time of 30 min to 90 min, so as to obtain the continuous diazotization product; Wherein, the third solvent is one or more of ethanol, methanol, and isopropanol; and / or, The type of reducing agent is one or more of Raney nickel, palladium carbon, and aluminum-nickel alloy catalyst; and / or, The third acid solution is concentrated sulfuric acid with a concentration of 30% to 70%, and the concentration of nitrosylsulfuric acid is 30% to 50%; and / or, The ninth set dosage is that the dosage of the third solvent added per 1 g of the second organic phase is 3 mL to 5 mL; and / or, The tenth set dosage is that the dosage of the reducing agent added to 1g of the third continuous batching product is 0.05g~0.2g; and / or, The eleventh setting amount is that the amount of the third acid solution added to 1g of the third continuous concentrated product is 5g-10g; and / or, The twelfth set dosage is that the dosage of the nitrosylsulfuric acid added in every 1g of the third continuous batching product is 3g~5g.

17. The method for continuous production of 3,4,5-trifluorobromobenzene according to claim 10, characterized in that: The method further comprises: Controlling the continuous diazotization unit in the post-treatment device to continuously diazotize the continuous bromination product to obtain a continuous diazotization product to be transported to the second continuous quenching component (414) at a feed rate of 150 / min to 250 / min, and controlling the urea containing component (316) to continuously transport the urea to the second continuous quenching component (414) at a twelfth set amount, and continuously quenching under the conditions of a quenching temperature of 10 to 20° C. and a quenching residence time of 10 min to 30 min, so as to obtain a second quenched product system; Controlling the second quenched product system to be delivered to the fluorination reaction component (415) at a feed rate of 300 g / min to 600 g / min, and controlling the hydrofluoric acid storage component (317) to continuously deliver hydrofluoric acid to the fluorination reaction component (415) at a thirteenth set amount, and performing a continuous fluorination reaction under the conditions of a first catalyst, a reaction temperature of 40° C. to 80° C., and a reaction residence time of 30 min to 90 min, so as to obtain a first fluorination product; Controlling the first fluorination product to be delivered to the second continuous distillation component (902) at a dosage of 200 g / min to 500 g / min, and continuously distilling the product at a second distillation temperature of 40° C. to 60° C. and a second distillation pressure of -0.08 MPa to -0.1 MPa to obtain the 3,4,5-trifluorobromobenzene; Wherein, the quenching temperature is 10°C to 20°C, and the concentration of the hydrofluoric acid is 30% to 50%; and / or, The first catalyst is one or more of cuprous oxide, cupric sulfate and cupric oxide; and / or, The amount of the first catalyst used is 0.005 g to 0.02 g per 1 g of the second quenched product system; and / or, The twelfth set dosage is that the dosage of the urea contained in 1g of the continuous diazotization product is 0.8g~1.6g; and / or, The thirteenth setting dosage is that the amount of the hydrofluoric acid added in every 1g of the second quenching product is 0.03g~0.1g.

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