Continuous reaction device

Abstract

The utility model discloses a continuous reaction device which comprises a Grignard liquid preparation device, the output end of the Grignard liquid preparation device is connected with a boronizing liquid preparation device, and a solvent and materials are continuously added into the Grignard liquid preparation device and the boronizing liquid preparation device to prepare a target product; the output end of the boronizing liquid preparation device is connected with the desolventizing kettle; the output end of the desolventizing kettle is connected with a centrifugal machine, and the target product is obtained after separation; the Grignard reagent and the bixafen intermediate are continuously reacted and prepared through the Grignard liquid preparation device and the boronizing liquid preparation device, the continuous stability is high, the production cost is reduced, the reaction time is shortened, and the safety is high.

Description

Technical Field

[0001] This utility model relates to the field of chemical synthesis technology, and in particular to a continuous reaction device. Background Technology

[0002] Bifenpyraclostrobin is a pyrazole amide fungicide discovered, developed and produced by Bayer AG of Germany. It is mainly used to control leaf spot and leaf rust diseases in cereals. It has the characteristics of broad spectrum and high efficiency and is one of the important products of succinic acid deoxygenase inhibitor fungicides. 3,4-Dichlorophenylboronic acid is one of the important intermediates in the synthesis of bifenpyraclostrobin.

[0003] In related technologies, batch reactors are often used to synthesize 3,4-dichlorophenylboronic acid products. However, the reaction is difficult to control, materials are prone to backmixing, and product yield and purity are low. Furthermore, the highly reactive Grignard reagent 3,4-dichlorophenyl magnesium bromide used in the synthesis of the target product is extremely prone to violent decomposition and explosion upon contact with water and oxygen. This places high demands on the reaction equipment, and large-scale storage poses a significant risk. Therefore, the reactors in related technologies cannot achieve efficient, continuous, and safe multi-equipment continuous reactions. Utility Model Content

[0004] The purpose of this invention is to address the shortcomings of existing technologies by proposing a continuous reaction device.

[0005] To achieve the above objectives, the present invention adopts the following technical solution: a continuous reaction device, comprising:

[0006] Apparatus preparation device;

[0007] The output end of the Grignard liquid preparation device is connected to the borate liquid preparation device, and the Grignard liquid preparation device and the borate liquid preparation device continuously add solvent and materials to prepare the target product.

[0008] The output end of the borohydride preparation device is connected to the desolvation vessel;

[0009] The output end of the desolventizing vessel is connected to a centrifuge to separate and obtain the target product.

[0010] As a further description of the above technical solution: the formula preparation device includes a first storage tank, the input end of the first storage tank is provided with a first solvent pump and a first material pump, and the output end of the first storage tank is provided with a first delivery pump.

[0011] As a further description of the above technical solution: the first delivery pump is connected to the Grignard reactor.

[0012] The output end of the Geiger reactor is equipped with a Geiger liquid filter;

[0013] The output end of the liquid filter is connected to a one-way regulating valve;

[0014] The output end of the one-way regulating valve is connected to the input end of the borosilicate preparation device.

[0015] As a further description of the above technical solution: the Grignard reactor is provided with a first condenser, a magnesium shavings feeding port and a first sampling port.

[0016] As a further description of the above technical solution: the borylation liquid preparation device includes a borylation reactor, and the input end of the borylation reactor is also connected to a second storage tank.

[0017] As a further description of the above technical solution: the input end of the second liquid storage tank is provided with a second solvent pump and a second material pump, and the output end of the second liquid storage tank is connected to a second delivery pump.

[0018] As a further description of the above technical solution: the boronizing reactor is provided with a second condenser and a second sampling port.

[0019] As a further description of the above technical solution: the output end of the borylation reactor is connected to the desolvation reactor via a third delivery pump.

[0020] As a further description of the above technical solution: the output end of the desolvation vessel is connected to the centrifuge via a fourth transfer pump.

[0021] As a further description of the above technical solution: heating jackets are provided on the Grignard reactor and the borylation reactor.

[0022] The above technical solution has the following advantages or beneficial effects:

[0023] The Grignard reagent and bifenthiophanate-methyl intermediates can be prepared by using Grignard solution preparation equipment and borosilicate preparation equipment. The continuous reaction preparation is highly stable, reduces production costs and shortens reaction time, and is highly safe. Attached Figure Description

[0024] Figure 1 This is a schematic diagram of the reaction device proposed in this utility model.

[0025] Legend:

[0026] 1. Apparatus for preparing sorbate solution; 11. First storage tank; 12. First solvent pump; 13. First material pump; 14. First transfer pump; 15. Apparatus reaction vessel; 16. Apparatus solution filter; 17. One-way regulating valve; 18. First condenser; 19. Magnesium shavings feed port; 110. First sampling port; 2. Apparatus for preparing borate solution; 21. Boration reaction vessel; 22. Second storage tank; 23. Second solvent pump; 24. Second material pump; 25. Second transfer pump; 26. Second condenser; 27. Second sampling port; 28. Third transfer pump; 3. Desolventizing vessel; 31. Fourth transfer pump; 4. Centrifuge; 5. Heating mantle. Detailed Implementation

[0027] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0028] Reference Figure 1 One embodiment of this utility model is a continuous reaction apparatus, comprising: a Grignard liquid preparation device 1; the output end of the Grignard liquid preparation device 1 is connected to a borate liquid preparation device 2, and solvents and materials are continuously added to the Grignard liquid preparation device 1 and the borate liquid preparation device 2 to prepare the target product; the output end of the borate liquid preparation device 2 is connected to a desolvation vessel 3; the output end of the desolvation vessel 3 is connected to a centrifuge 4, and the target product is obtained after separation.

[0029] In this embodiment, the continuous reaction preparation of Grignard reagent and bifenthiophanate intermediate is achieved by using Grignard solution preparation device 1 and borate solution preparation device 2. The continuous reaction has high stability, reduces production costs and shortens reaction time, and has high safety. The target product generated is 3,4-dichlorophenylboronic acid.

[0030] The gram liquid preparation device 1 includes a first storage tank 11, with a first solvent pump 12 and a first material pump 13 installed at the input end of the first storage tank 11, and a first delivery pump 14 installed at the output end of the first storage tank 11.

[0031] The first delivery pump 14 is connected to the Geiger reactor 15; the output end of the Geiger reactor 15 is equipped with a Geiger liquid filter 16; the output end of the Geiger liquid filter 16 is connected to a one-way regulating valve 17; the output end of the one-way regulating valve 17 is connected to the input end of the borosilicate preparation device 2.

[0032] In this embodiment, the first delivery pump 14 is connected to the Grignard reactor 15, enabling it to deliver materials to the Grignard reactor 15 for reaction. After the reaction products are output from the Grignard reactor 15, they first pass through the Grignard liquid filter 16. The function of this filter is to remove solid impurities from the reaction liquid to ensure the purity of the liquid entering subsequent devices. Then, the filtered liquid flows into the one-way regulating valve 17. The one-way regulating valve 17 ensures that the liquid flows in only one direction, preventing backflow and ensuring the stability of the system.

[0033] The Grignard reactor 15 is equipped with a first condenser 18, a magnesium shavings feed port 19, and a first sampling port 110.

[0034] In this embodiment, the first condenser 18 condenses the vapors or volatiles generated during the reaction. In a Grignard reaction, solvents or other volatile substances may be generated. The first condenser 18 condenses and returns these substances to the Grignard reactor 15, thus avoiding material loss and maintaining the material balance of the reaction system. The magnesium shavings feed port 19 allows for convenient and accurate addition of magnesium shavings into the Grignard reactor 15 to ensure the smooth progress of the reaction. The first sampling port 110 samples and tests the Grignard reagents, monitoring the reaction progress and determining whether the reaction is proceeding as expected.

[0035] The borylation solution preparation apparatus 2 includes a borylation reactor 21, the input end of which is connected to a second storage tank 22. The input end of the second storage tank 22 is equipped with a second solvent pump 23 and a second material pump 24, and the output end of the second storage tank 22 is connected to a second transfer pump 25. The borylation reactor 21 is equipped with a second condenser 26 and a second sampling port 27.

[0036] In this embodiment, the borination reactor 21 is the site where the borination reaction takes place. In the borination reactor 21, the Grignard reagent, after being processed from the Grignard reactor 15, reacts with other reagents, such as borate esters, to generate a borinated liquid. These reagents can be added to the borination reactor 21 in advance as needed for the reaction.

[0037] The boronizing reactor 21 and the second storage tank 22 work together. The second storage tank 22 provides materials to the boronizing reactor 21, which then reacts the input materials to produce a boronized liquid. The second condenser 26 condenses and recovers the generated volatiles, and the second sampling port 27 monitors the reaction in real time. They work together to ensure that the boronizing reaction can proceed efficiently and stably, ultimately producing a boronized liquid that meets the quality requirements.

[0038] The output end of the boronizing reactor 21 is connected to the desolvation reactor 3 via the third transfer pump 28.

[0039] In this embodiment, the desolventizing vessel 3 is used for quenching, separating, and desolventizing the borohydride solution.

[0040] The output end of the desolventizing vessel 3 is connected to the centrifuge 4 via the fourth transfer pump 31.

[0041] In this embodiment, centrifuge 4 is used to perform reflux pulping and centrifugation operations to obtain the target product.

[0042] Heating jackets 5 are provided on the Grignard reactor 15 and the boronizing reactor 21 for temperature control.

[0043] Working principle:

[0044] (1) Open all flow regulating valves, and then add methyltetrahydrofuran and 3,4-dichlorobromobenzene to the first storage tank 11 through the first solvent pump 12 and the first material pump 13 respectively; add methyltetrahydrofuran and 3,4-dichlorobromobenzene to the second storage tank 22 through the second solvent pump 23 and the second material pump 24; add magnesium shavings to the Grignard reactor 15 through the magnesium shavings feed port 19 and fix them with a filter element.

[0045] (2) Close all valves and pumps, and replace the air in the glycidyl liquid preparation device and the borate liquid preparation device with vacuum nitrogen.

[0046] (3) Turn on the first transfer pump 14 and add the mixture in the first storage tank 11 to the Gottlieb reactor 15. Stir at low temperature. When there is a significant temperature rise, the reaction is successfully initiated. Then turn on the first solvent pump 12 and the first material pump 13 and continue to add the mixture to the Gottlieb reactor 15 at a certain speed through the first transfer pump 14.

[0047] (4) When the reaction liquid overflows from the Geiger reaction vessel 15, it flows through the Geiger liquid filter 16 and the one-way regulating valve 17 into the boronizing reaction vessel 21. Then, the second solvent pump 23, the second material pump 24 and the second transfer pump 25 are turned on and slowly added to the boronizing reaction vessel 21 at a certain speed to carry out the boronizing reaction.

[0048] (5) When the reaction liquid overflows from the boronizing reactor 21, the third transfer pump 28 is turned on to add the reaction liquid to the desolventizing reactor 3 for quenching, separation and desolventizing. Then the fourth transfer pump 31 is turned on to transfer the liquid to the centrifuge 4 for reflux pulping and centrifugal drying to obtain 3,4-dichlorophenylboronic acid.

[0049] Finally, it should be noted that the above description is only a preferred embodiment of the present utility model and is not intended to limit the present utility model. Although the present utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present utility model should be included within the protection scope of the present utility model.

Claims

1. A continuous reaction apparatus, characterized by, The application relates to a preparation device for a boron-containing solution. The output end of the preparation device (1) is connected with a boron-containing solution preparation device (2), and the preparation device (1) and the boron-containing solution preparation device (2) continuously add solvent and materials to prepare a target product. The output end of the boron-containing solution preparation device (2) is connected with a desolventizing kettle (3). The output end of the desolventizing kettle (3) is connected with a centrifuge (4) to obtain the target product after separation. The preparation device (1) comprises a first liquid storage tank (11), the input end of the first liquid storage tank (11) is provided with a first solvent pump (12) and a first material pump (13), and the output end of the first liquid storage tank (11) is provided with a first conveying pump (14).

2. The reaction apparatus of claim 1, wherein: The first conveying pump (14) is connected with a format reaction kettle (15).

3. The reaction apparatus of claim 2, wherein: The output end of the format reaction kettle (15) is provided with a format liquid filter (16). The output end of the format liquid filter (16) is connected with a one-way regulating valve (17). The output end of the one-way regulating valve (17) is connected with the input end of the boron-containing solution preparation device (2). The format reaction kettle (15) is provided with a first condenser (18), a magnesium chip feeding port (19) and a first sampling port (110).

4. The reaction apparatus of claim 3, wherein: The boron-containing solution preparation device (2) comprises a boron-containing reaction kettle (21), and the input end of the boron-containing reaction kettle (21) is further connected with a second liquid storage tank (22).

5. The reaction apparatus of claim 3, wherein: The input end of the second liquid storage tank (22) is provided with a second solvent pump (23) and a second material pump (24), and the output end of the second liquid storage tank (22) is connected with a second conveying pump (25).

6. The reaction apparatus of claim 5, wherein: The boron-containing reaction kettle (21) is provided with a second condenser (26) and a second sampling port (27).

7. The reaction apparatus of claim 5, wherein: The output end of the boron-containing reaction kettle (21) is connected with the desolventizing kettle (3) through a third conveying pump (28).

8. The reaction apparatus of claim 5, wherein: The output end of the desolventizing kettle (3) is connected with the centrifuge (4) through a fourth conveying pump (31).

9. The reactor of claim 1, wherein: The format reaction kettle (15) and the boron-containing reaction kettle (21) are provided with a heating jacket (5).

10. The reaction apparatus of claim 5, wherein: ​

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