A continuous production device of 3,4,5-trifluorobromobenzene

Abstract

The utility model relates to a kind of 3,4,5-trifluorobromobenzene continuous production device, including feeding device, double medium reactor, gas-liquid separation buffer tank, tail gas condenser, each device is sequentially connected by material pipeline;The feeding device includes metering pump, check valve, feed control valve, is sequentially connected with double medium reactor feed inlet after passing through material pipeline connection.The utility model is controlled continuous discharge by setting rationing equipment, to realize the continuous feeding and discharge of 3,4,5-trifluorobromobenzene industrial production, reaction process is safe, efficient and convenient.

Description

Technical Field

[0001] This utility model belongs to the field of chemical production equipment, specifically relating to a continuous production equipment for 3,4,5-trifluorobromobenzene. Background Technology

[0002] 3,4,5-Trifluorobromobenzene is an important pesticide intermediate, mainly used in the synthesis of fluopyram, a fungicide that inhibits succinate dehydrogenase. In existing technologies, the conventional reaction typically uses 1,2,3-trifluorobenzene as a raw material, dichloroethane as a solvent, and an aqueous solution of sodium bromide containing a buffer solution. Sodium hypochlorite is then added dropwise to induce a bromination reaction. The basic reaction condition is a 1:1 molar ratio of 1,2,3-trifluorobenzene to the aqueous solution of sodium bromide containing a buffer solution, employing a traditional batch reaction method. However, conventional reactions suffer from problems such as high exothermic reaction, high risk, and instability of diazonium salts, which easily decompose, resulting in low product yield and content.

[0003] In addition, the prior art CN119215815A discloses continuous production equipment and methods for 3,4,5-trifluorobromobenzene, including: a continuous feeding device, a continuous sulfonation reaction tank, and a continuous post-processing device. It involves multiple units of continuous reaction. If a problem occurs in any link, it may cause the entire production line to stop, resulting in significant losses and making it difficult to handle.

[0004] Given the vast market demand, it is crucial to develop more convenient and efficient continuous production equipment to achieve continuous feeding and discharging for the industrial production of 3,4,5-trifluorobromobenzene. This invention employs precise control of the feed rate and ratio, resulting in less backmixing and lower impurities during the reaction process, significantly improving production efficiency and ensuring product quality stability. Summary of the Invention

[0005] The purpose of this invention is to provide a continuous production device for 3,4,5-trifluorobromobenzene, in order to solve the problem of more efficient and convenient continuous production.

[0006] To achieve the above-mentioned technical objectives, the present invention adopts the following technical solution: a continuous production device for 3,4,5-trifluorobromobenzene, comprising a feeding device, a dual-media reactor, a gas-liquid separation buffer tank, and a tail gas condenser, wherein each device is connected in sequence via a material pipeline; the feeding device comprises a metering pump, a check valve, and a feeding control valve, which are connected in sequence via a material pipeline and then connected to the inlet of the dual-media reactor.

[0007] The dual-media reactor is provided with a discharge port at the rear end and a microchannel baffle inside. The dual-media reactor is also provided with a reaction calorimeter at the front end. The reaction calorimeter is connected in parallel with a one-way intelligent stop valve.

[0008] The discharge port is connected to the feed pipe control valve and then to the gas-liquid separation buffer tank. The gas-liquid separation buffer tank is equipped with a discharge pipe control valve at the bottom, an upper exhaust pipe at the top, and a liquid level gauge on the side wall. A pressure reducing valve is installed on the pipeline connecting the upper exhaust pipe and the tail gas condenser. The tail gas condenser includes an inlet pipe, a tail gas treatment pipe, and a condensation jacket.

[0009] A product quality inspection valve and a discharge control device are installed on the front end pipeline of the discharge pipe control valve, and a flame ionization detector is installed on the upper part of the product quality inspection valve.

[0010] Furthermore, a pressure gauge is also installed on the material pipeline between the metering pump and the check valve;

[0011] Furthermore, a quality inspection valve is also installed on the material pipeline between the check valve and the feed control valve;

[0012] Furthermore, a feed valve and a feed control device are also provided on the material pipeline at the front end of the metering pump;

[0013] Furthermore, the metering pumps include a mixed reaction liquid metering pump and a sodium nitrite aqueous solution metering pump;

[0014] Furthermore, the dual-media reactor is also provided with a first media inlet, a first media outlet, a second media inlet, and a second media outlet;

[0015] Furthermore, the microchannel partition includes a forward microchannel partition and a reverse microchannel partition, wherein the forward microchannel partition and the reverse microchannel partition are sequentially and repeatedly connected.

[0016] Furthermore, the gas-liquid separation buffer tank is also equipped with an insulation jacket on its exterior;

[0017] Furthermore, the insulation jacket is provided with an insulation jacket inlet and an insulation jacket outlet.

[0018] Furthermore, the condenser jacket includes a cold water inlet and a cold water outlet.

[0019] Beneficial effects:

[0020] 1) The gas-liquid separation buffer tank automation device enables continuous automation of the 3,4,5-trifluorobromobenzene synthesis process;

[0021] 2) By precisely controlling the feed rate and feed ratio, the reaction process has less backmixing and lower impurity levels, enabling continuous production, significantly improving production efficiency, reducing the generation of reaction impurities, and ensuring the stability of product quality. Attached Figure Description

[0022] Figure 1 This is a schematic diagram of the structure of the continuous production device for 3,4,5-trifluorobromobenzene according to this utility model;

[0023] In the picture:

[0024] 1-Mixed reaction liquid metering pump, 11-Infeed valve a, 12-Infeed control device a, 13-Pressure gauge a, 14-Check valve a, 15-Quality inspection valve a, 16-Infeed control valve a; 2-Sodium nitrite aqueous solution metering pump, 21-Infeed valve b, 22-Infeed control device b, 23-Pressure gauge b, 24-Check valve b, 25-Quality inspection valve b, 26-Infeed control valve b, 27-One-way intelligent check valve; 3-Dual media reactor, 31-First inlet, 32-Second inlet, 33-Outlet, 341-First media inlet, 342-First media outlet, 343-Second media inlet, 344 - Second medium outlet, 35- Microchannel baffle, 351- Microchannel forward baffle, 352- Microchannel reverse baffle, 36- Reaction calorimeter; 4- Gas-liquid separation buffer tank, 41- Feed pipe control valve, 42- Discharge pipe control valve, 43- Level gauge, 44- Upper exhaust pipe, 45- Pressure reducing valve, 46- Insulation jacket, 461- Insulation jacket inlet, 462- Insulation jacket outlet; 5- Tail gas condenser, 51- Inlet pipe, 52- Tail gas treatment pipe, 53- Condensation jacket, 531- Cold water inlet, 532- Cold water outlet; 6- Flame ionization detector, 61- Product quality inspection valve, 62- Discharge control device. Detailed Implementation

[0025] To make the technical solutions and advantages of this utility model clearer, the technical solutions in the embodiments of this utility model are clearly and completely described below in conjunction with specific accompanying drawings. The described embodiments are only a part of the embodiments of this utility model. All other embodiments obtained by those skilled in the art based on the embodiments of this utility model without creative effort are within the protection scope of this utility model.

[0026] The present invention will be further described below with reference to the accompanying drawings:

[0027] like Figure 1 The continuous production apparatus for 3,4,5-trifluorobromobenzene shown includes a feeding device, a dual-media reactor 3, a gas-liquid separation buffer tank 4, and a tail gas condenser 5, with each device connected in sequence via a material pipeline.

[0028] The feeding device includes a metering pump, a check valve, and a feed control valve, which are connected to the feed inlet of the dual-media reactor 3 via material pipelines in sequence.

[0029] The metering pumps include a mixed reaction liquid metering pump 1 and a sodium nitrite aqueous solution metering pump 2; the check valves include check valve a14 and check valve b24; and the feed control valves include feed control device a12 and feed control device b22.

[0030] The mixed reaction solution in the metering pump 1 is a mixed solution prepared by mixing 50% sulfuric acid solution of 2,3,4-trifluoro-6-bromoaniline, 50% hypophosphoric acid solution, and 30% copper sulfate aqueous solution in a ratio of 1:1:1.

[0031] A pressure gauge is also installed on the material pipeline between the metering pump and the check valve; a pressure gauge a13 is also installed on the material pipeline between the metering pump 1 for the mixed reaction liquid and the check valve a14; and a pressure gauge b23 is also installed on the material pipeline between the metering pump 2 for the sodium nitrite aqueous solution and the check valve b24.

[0032] A quality inspection valve is also installed on the material pipeline between the check valve and the feed control valve. A quality inspection valve a15 is also installed on the material pipeline between the check valve a14 and the feed control device a12. A quality inspection valve b25 is also installed on the material pipeline between the check valve b24 and the feed control device b22.

[0033] The metering pump is equipped with a feed valve and a feed control device on the front-end material pipeline; the mixed reaction liquid metering pump 1 is equipped with a feed valve a11 and a feed control device a12 on the front-end material pipeline; the sodium nitrite aqueous solution metering pump 2 is equipped with a feed valve b21 and a feed control device b22 on the front-end material pipeline.

[0034] The dual-media reactor is further provided with a first media inlet 31, a first media outlet 32, a second media inlet 33, and a second media outlet 34; the rear end of the dual-media reactor 3 is provided with an outlet 33 and an internal microchannel baffle 35, the microchannel baffle 35 including a forward microchannel baffle 351 and a reverse microchannel baffle 352; the forward microchannel baffle 351 and the reverse microchannel baffle 352 are sequentially and repeatedly connected; the front end of the dual-media reactor 3 is also provided with a reaction calorimeter 36, the reaction calorimeter 36 is connected in parallel with a one-way intelligent stop valve 27; the one-way intelligent stop valve 27 can effectively block material backflow and realize automatic feeding control.

[0035] The discharge port 33 is connected to the feed pipe control valve 41 and then to the gas-liquid separation buffer tank 4. The gas-liquid separation buffer tank 4 is equipped with a discharge pipe control valve 42 at the bottom, an upper exhaust pipe 44 at the top, and a level gauge 43 on the side wall. The level gauge 43 can measure the liquid level and interface of the liquid medium in the gas-liquid separation buffer tank 4.

[0036] The gas-liquid separation buffer tank 4 is also provided with an insulation jacket 46, which is provided with an insulation jacket inlet 461 and an insulation jacket outlet 462.

[0037] A pressure reducing valve 45 is provided on the connecting pipeline between the upper exhaust pipe 44 and the exhaust gas condenser 5. The exhaust gas condenser 5 includes an air inlet pipe 51, an exhaust gas treatment pipe 52, and a condensing jacket 53. The condensing jacket 53 includes a cold water inlet 531 and a cold water outlet 532.

[0038] A product quality inspection valve 61 and a discharge control device 62 are installed on the front end pipeline of the discharge pipe control valve 41. A flame ionization detector 6 is installed on the upper part of the product quality inspection valve 61.

[0039] Example 1

[0040] A mixed solution consisting of 50% sulfuric acid solution of 2,3,4-trifluoro-6-bromoaniline, 50% hypophosphoric acid solution, and 30% copper sulfate aqueous solution in a 1:1:1 ratio is continuously pumped into the dual-media reactor 3 via a mixed reaction liquid metering pump 1 and a 30% sodium nitrite aqueous solution metering pump 2 at a flow rate of 4:1 for reaction.

[0041] Before the reactants are introduced, the reaction calorimeter 36 is started, and the temperature control system of the regulating device is used to keep the inside of the reactor stable at 50°C.

[0042] The discharge port 33 is connected to the feed pipe control valve 41 and then to the gas-liquid separation buffer tank 4. After the reactant material is reacted in the dual-medium reactor 3, it enters the gas-liquid separation buffer tank 4 along with the entrained gas. When the continuous reaction pressure reaches the set value of 1MPa, the pressure reducing valve 45 automatically opens, and the gas is discharged from the exhaust pipe 44. It is then condensed by the tail gas condenser 5 to condense and recover the liquid material, while the gas material enters the tail gas treatment.

[0043] The production unit yielded 228 kg of 3,4,5-trifluorobromobenzene, with a normalization rate of 94% as determined by gas chromatography and a reaction yield of 88%.

[0044] Example 2

[0045] A mixed solution consisting of 50% sulfuric acid solution of 2,3,4-trifluoro-6-bromoaniline, 50% hypophosphoric acid solution, and 30% copper sulfate aqueous solution in a 1:1:1 ratio is continuously pumped into the dual-media reactor 3 via a mixed reaction liquid metering pump 1 and a 30% sodium nitrite aqueous solution metering pump 2 at a flow rate of 3:1 for the reaction to take place.

[0046] Before the reactants are introduced, the reaction calorimeter 36 is started, and the temperature control system of the regulating device is used to keep the inside of the reactor stable at 50°C.

[0047] The discharge port 33 is connected to the feed pipe control valve 41 and then to the gas-liquid separation buffer tank 4. After the reactant material is reacted in the dual-medium reactor 3, it enters the gas-liquid separation buffer tank 4 along with the entrained gas. When the continuous reaction pressure reaches the set value of 1MPa, the pressure reducing valve 45 automatically opens, and the gas is discharged from the exhaust pipe 44. It is then condensed by the tail gas condenser 5 to condense and recover the liquid material, while the gas material enters the tail gas treatment.

[0048] The production unit yielded 224 kg of 3,4,5-trifluorobromobenzene, with a normalization rate of 93% as determined by gas chromatography and a reaction yield of 86%.

[0049] The above embodiments are merely preferred technical solutions of this utility model and should not be regarded as limitations on this utility model. The protection scope of this utility model should be the technical solution described in the claims, including equivalent substitutions of the technical features described in the claims. That is, equivalent substitutions and improvements within this scope are also within the protection scope of this utility model.

Claims

1. A continuous production apparatus for 3,4,5-trifluorobromobenzene, characterized in that, It includes a feeding device, a dual-media reactor, a gas-liquid separation buffer tank, and a tail gas condenser, with each device connected in sequence via a material pipeline. The feeding device includes a metering pump, a check valve, and a feed control valve, which are connected to the feed inlet of the dual-media reactor via a material pipeline. The dual-media reactor has a discharge port at the rear end and a microchannel baffle inside. The dual-media reactor also has a reaction calorimeter at the front end, which is connected in parallel with a one-way intelligent check valve. The discharge port is connected to the feed pipe control valve and then to the gas-liquid separation buffer tank. The gas-liquid separation buffer tank is equipped with a discharge pipe control valve at the bottom, an upper exhaust pipe at the top, and a level gauge on the side wall. A pressure reducing valve is installed on the pipeline connecting the upper exhaust pipe and the tail gas condenser. The tail gas condenser includes an inlet pipe, a tail gas treatment pipe, and a condensation jacket. A product quality inspection valve and a discharge control device are installed on the pipeline at the front end of the discharge pipe control valve. A flame ionization detector is installed on the upper part of the product quality inspection valve.

2. The continuous production apparatus for 3,4,5-trifluorobromobenzene according to claim 1, characterized in that, A pressure gauge is also installed on the material pipeline between the metering pump and the check valve.

3. The continuous production apparatus for 3,4,5-trifluorobromobenzene according to claim 1, characterized in that, A quality inspection valve is also installed on the material pipeline between the check valve and the feed control valve.

4. The continuous production apparatus for 3,4,5-trifluorobromobenzene according to claim 1, characterized in that, The metering pump is also equipped with a feed valve and a feed control device on the front-end material pipeline.

5. The continuous production apparatus for 3,4,5-trifluorobromobenzene according to claim 1, characterized in that, The metering pumps include a mixed reaction liquid metering pump and a sodium nitrite aqueous solution metering pump.

6. The continuous production apparatus for 3,4,5-trifluorobromobenzene according to claim 1, characterized in that, The dual-media reactor is further provided with a first media inlet, a first media outlet, a second media inlet, and a second media outlet.

7. The continuous production apparatus for 3,4,5-trifluorobromobenzene according to claim 1, characterized in that, The microchannel partition includes a forward microchannel partition and a reverse microchannel partition, which are sequentially and repeatedly connected.

8. The continuous production apparatus for 3,4,5-trifluorobromobenzene according to claim 1, characterized in that, The gas-liquid separation buffer tank is also equipped with an insulation jacket.

9. The continuous production apparatus for 3,4,5-trifluorobromobenzene according to claim 8, characterized in that, The insulation jacket is provided with an insulation jacket inlet and an insulation jacket outlet.

10. The continuous production apparatus for 3,4,5-trifluorobromobenzene according to claim 1, characterized in that, The condenser jacket includes a cold water inlet and a cold water outlet.

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