Device for synthesizing chlorantraniliprole intermediate

Abstract

The utility model discloses a device for synthesizing a chlorantraniliprole intermediate, which mainly comprises a feeding device and a double-medium reactor, and the feeding device is connected with the double-medium reactor through a material pipeline; the feeding device comprises a reaction material A feeding pump and a reaction material B feeding pump; the double-medium reactor comprises a reactor, a heat exchange device I and a heat exchange device II, and the reactor is bordered with the heat exchange device I and the heat exchange device II. The utility model overcomes the problem that various reaction temperatures are not easy to control, not only can effectively control the reaction temperature, but also can prevent the reaction from being violent and overhigh in temperature and improve the safety performance of the reaction, is also suitable for the type of reaction heat release and heat transfer after the reaction needs to be initiated at a certain temperature, and has important significance for industrialization.

Description

Technical Field

[0001] The utility model belongs to the technical field of chemical equipment, and specifically relates to a device for synthesizing a chlorantraniliprole intermediate. Background Art

[0002] 3-Bromo-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carboxylic acid ethyl ester is an important intermediate for the synthesis of new nicotinic acid receptor insecticides such as chlorantraniliprole, which can widely and efficiently control chewing mouthparts pests on fruit trees, vegetables, field crops, specialty crops and lawns. The synthesis of 3-Bromo-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carboxylic acid ethyl ester is a more violent oxidation reaction, which is difficult to control. When the temperature control is unstable, there are more side reactions, more impurities are generated, and the yield is reduced. This device is a dual-medium continuous reaction device, which is a reaction device for reactions with more violent changes, difficult to control, and the need for initiation. Through the cold and heat exchange of the dual medium, the temperature change of the reaction can be effectively controlled, so that the reaction effect is stable, the generation of reaction impurities is reduced, and the safety of the reaction is improved. Summary of the invention

[0003] In view of the above problems, the utility model provides a device for synthesizing a chlorantraniliprole intermediate, aiming to solve the problem that the existing reaction is fast and the temperature is difficult to control.

[0004] The utility model adopts the following technical scheme: a device for synthesizing chlorantraniliprole intermediates, mainly comprising a feeding device and a dual-medium reactor, wherein the feeding device and the dual-medium reactor are connected through a material pipeline;

[0005] The feeding device comprises a feed pump for reaction material A and a feed pump for reaction material B; a ball feed valve A is arranged on the front material pipeline of the feed pump for reaction material A, and a screw flow control valve A is arranged on the rear material pipeline; a ball feed valve B is arranged on the front material pipeline of the feed pump for reaction material B, and a screw flow control valve B is arranged on the rear material pipeline;

[0006] The dual-medium reactor comprises a reactor, a heat exchange device I and a heat exchange device II, wherein the reactor is connected to the heat exchange device I and the heat exchange device II; the reactor comprises a material inlet, a material mixer, a reactor inner cavity, and a material outlet, wherein the material inlet comprises an inlet for reaction material A and an inlet for reaction material B; the heat exchange device I is provided with an inlet for heat exchange medium I and an outlet for heat exchange medium I; the heat exchange device II is provided with an inlet for heat exchange medium II and an outlet for heat exchange medium II;

[0007] Furthermore, the inner cavity of the reactor is made of stainless steel or enamel;

[0008] Furthermore, a heat exchange medium I control valve is provided on the heat exchange medium I inlet material pipeline;

[0009] Furthermore, a heat exchange medium II control valve is provided on the heat exchange medium II inlet material pipeline;

[0010] Furthermore, a material quality detection valve is also provided at the front end of the material discharge port;

[0011] Furthermore, a pressure gauge A is provided on the material pipeline between the rotary flow control valve A and the feed pump for material A; a pressure gauge B is provided on the material pipeline between the rotary flow control valve B and the feed pump for material B;

[0012] Furthermore, a pressure gauge valve A is provided on the front material pipeline of the pressure gauge A; a pressure gauge valve B is provided on the front material pipeline of the pressure gauge B;

[0013] Furthermore, the internal media of the heat exchange device I and the heat exchange device II are the same medium or different media;

[0014] Furthermore, the outer side wall of the dual-medium reactor is provided with a heat-insulating jacket;

[0015] Furthermore, the internal medium of the heat exchange device I and the heat exchange device II can be selected from one or two of water, silicone oil, ethanol or ethylene glycol.

[0016] The beneficial effects of the utility model are:

[0017] 1) The utility model can solve the type of reaction that is more drastic, difficult to control or requires gradient cooling by setting up a dual-medium reactor device for bidirectional circulation heat exchange. The temperature change of the reaction can be effectively controlled by the temperature difference exchange of the dual medium;

[0018] 2) The device of the utility model is suitable for reactions that require a certain temperature to initiate the reaction, and the reaction releases heat after initiation and requires heat removal;

[0019] 3) The utility model improves the reaction safety performance by controlling the violent reaction, and is easier to realize industrialization. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 A schematic diagram of the structure of a device for synthesizing a chlorantraniliprole intermediate in the utility model;

[0021] In the figure,

[0022] 1-reaction material A feed pump, 11-ball feed valve A, 12-pressure gauge A, 13-pressure gauge valve A, 14-drain valve A, 15-screw flow control valve A;

[0023] 2-reaction material B feed pump, 21-spherical feed valve B, 22-pressure gauge B, 23-pressure gauge valve B, 24-drain valve B, 25-screw flow control valve B;

[0024] 3-reactor, 31-reaction material A inlet, 32-reaction material B inlet, 33-material mixer, 34-reactor inner cavity, 35-material quality detection valve, 36-material discharge port;

[0025] 4-heat exchange device I, 41-heat exchange medium I inlet, 42-heat exchange medium I control valve, 43-heat exchange medium I outlet; 5-heat exchange device II, 51-heat exchange medium II inlet, 52-heat exchange medium II control valve, 53-heat exchange medium II outlet;

[0026] 6- Insulation jacket. DETAILED DESCRIPTION

[0027] In order to have a clearer understanding of the technical features, purposes and effects of the utility model, the specific implementation methods of the utility model are now described with reference to the accompanying drawings.

[0028] Embodiment 1:

[0029] like Figure 1 The device shown is a device for synthesizing a chlorantraniliprole intermediate, which mainly includes a feeding device and a dual-medium reactor. The feeding device is connected to the dual-medium reactor through a material pipeline; A is a DMF solution of raw materials used for reaction synthesis, and B is a DMF slurry of potassium persulfate.

[0030] The feeding device comprises a reaction material A feeding pump 1 and a reaction material B feeding pump 2; a ball feeding valve A11 is arranged on the front end material pipeline of the reaction material A feeding pump 1, and a screw flow control valve A15 is arranged on the rear end material pipeline; a ball feeding valve B12 is arranged on the front end material pipeline of the reaction material B feeding pump 2, and a screw flow control valve B25 is arranged on the rear end material pipeline; the DMF solution passes through the reaction material A feeding pump 1, the heat exchange device I4 is started, and the temperature control system of the regulating device heats the reaction material to 70°C. After the temperature is reached, the system temperature is maintained; at this time, the DMF slurry of potassium persulfate passes through the reaction material B feeding pump 2, and the heat device I4 and the heat exchange device II5 are adjusted at the same time to continue to heat the mixed material to 80°C, so as to ensure that the temperature of the mixed material can continue to rise to reach the reaction initiation temperature.

[0031] A pressure gauge A12 is provided on the material pipeline between the rotary flow control valve A15 and the feed pump 1 for material A; a pressure gauge B22 is provided on the material pipeline between the rotary flow control valve B25 and the feed pump 2 for material B; a pressure gauge thread valve A13 is provided on the material pipeline in front of the pressure gauge A12; a pressure gauge thread valve B23 is provided on the material pipeline in front of the pressure gauge B22; the dual-medium reactor includes a reactor 3, a heat exchange device I4 and a heat exchange device II5, and the reactor is connected to the heat exchange device I4 and the heat exchange device II5; the inner cavity of the reactor 3 is made of stainless steel or enamel.

[0032] The reactor 3 includes a material inlet, a material mixer 33, a reactor cavity 34, and a material outlet 36; wherein the reactor cavity 34 is configured to be S-shaped streamlined, which is conducive to the flow of the reaction materials and the internal medium, so that the heating is uniform. The material inlet includes a reaction material A inlet 31 and a reaction material B inlet 32; the front end of the material outlet 36 is also provided with a material quality detection valve 35. Through detection, if the reaction is not complete, the length of the equipment reactor needs to be increased to ensure the reaction insulation time and the raw materials can be completely converted.

[0033] The heat exchange device I4 is provided with a heat exchange medium I inlet 41 and a heat exchange medium I outlet 43, and a heat exchange medium I control valve 42 is provided on the heat exchange medium I inlet 41 material pipeline; the heat exchange device II5 is provided with a heat exchange medium II inlet 51 and a heat exchange medium II outlet 53, and a heat exchange medium II control valve 52 is provided on the heat exchange medium II inlet 51 material pipeline; the internal media of the heat exchange device I4 and the heat exchange device II5 are the same medium or different media; the internal media of the heat exchange device I4 and the heat exchange device II5 can be selected from one or two of water, silicone oil, ethanol or ethylene glycol, and the outer side wall of the dual-medium reactor is provided with a thermal insulation jacket 6 to maintain the system temperature at 70-75°C.

[0034] The above embodiments are only preferred technical solutions of the present utility model and should not be regarded as limitations of the present utility model. The protection scope of the present utility model should be the technical solutions recorded in the claims, including equivalent replacement solutions of the technical features in the technical solutions recorded in the claims, that is, equivalent replacement improvements within this scope are also within the protection scope of the present utility model.

Claims

1. A device for synthesizing a chlorantraniliprole intermediate, characterized in that: It mainly includes a feeding device and a dual-medium reactor, and the feeding device and the dual-medium reactor are connected through a material pipeline; The feeding device comprises a feed pump for reaction material A and a feed pump for reaction material B; a ball feed valve A is arranged on the front material pipeline of the feed pump for reaction material A, and a screw flow control valve A is arranged on the rear material pipeline; a ball feed valve B is arranged on the front material pipeline of the feed pump for reaction material B, and a screw flow control valve B is arranged on the rear material pipeline; The dual-medium reactor comprises a reactor, a heat exchange device I and a heat exchange device II, wherein the reactor is connected to the heat exchange device I and the heat exchange device II; the reactor comprises a material inlet, a material mixer, a reactor inner cavity, and a material outlet, wherein the material inlet comprises an inlet for reaction material A and an inlet for reaction material B; the heat exchange device I is provided with an inlet for heat exchange medium I and an outlet for heat exchange medium I; the heat exchange device II is provided with an inlet for heat exchange medium II and an outlet for heat exchange medium II.

2. A device for synthesizing a chlorantraniliprole intermediate as claimed in claim 1, characterized in that: The inner cavity of the reactor is made of stainless steel or enamel.

3. A device for synthesizing a chlorantraniliprole intermediate as claimed in claim 1, characterized in that: A heat exchange medium I control valve is arranged on the heat exchange medium I inlet material pipeline.

4. A device for synthesizing a chlorantraniliprole intermediate as claimed in claim 1, characterized in that: A heat exchange medium II control valve is arranged on the heat exchange medium II inlet material pipeline.

5. The device for synthesizing a chlorantraniliprole intermediate according to claim 1, characterized in that: A material quality detection valve is also arranged at the front end of the material discharge port.

6. A device for synthesizing a chlorantraniliprole intermediate as claimed in claim 1, characterized in that: A pressure gauge A is provided on the material pipeline between the rotary flow control valve A and the feed pump for material A; a pressure gauge B is provided on the material pipeline between the rotary flow control valve B and the feed pump for material B.

7. A device for synthesizing a chlorantraniliprole intermediate as claimed in claim 6, characterized in that: A pressure gauge thread valve A is arranged on the material pipeline at the front end of the pressure gauge A; a pressure gauge thread valve B is arranged on the material pipeline at the front end of the pressure gauge B.

8. The device for synthesizing a chlorantraniliprole intermediate according to claim 1, characterized in that: The outer side wall of the dual-medium reactor is provided with a heat-insulating jacket.

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