Reaction device

Abstract

The utility model discloses a reaction device. The reaction device comprises a preparation kettle and a dissolving kettle, the output ends of the preparation kettle and the dissolving kettle are connected with the reaction kettle; the mother liquor is output into a filter after being reacted in the reaction kettle, and the output end of the filter is connected with a mother liquor tank; and the mother liquor tank conveys the reaction liquid to a post-treatment stage through a transfer pump. According to the device, the configuration kettle, the dissolving kettle, the high-pressure reaction kettle, the filter, the mother liquor tank and the material transfer pump are matched for use, the use amount of chlorination reagent solid light can be greatly reduced by 50% due to the use of the high-pressure reaction kettle, the phosgene content in tail gas is reduced by more than 90%, the production cost is effectively reduced, and the production efficiency is improved. Meanwhile, the phosgene content in the waste gas is lower, and the treatment is more convenient.

Description

Technical Field

[0001] The utility model relates to the technical field of chemical equipment, in particular to a reaction device. Background Art

[0002] 4,6-Dichloropyrimidine is mainly used in the production of azoxystrobin and is an important intermediate of azoxystrobin.

[0003] The preparation of 4,6-dichloropyrimidine using solid-state photochlorination of 4,6-dihydroxypyrimidine produces no phosphorus-containing wastewater and does not require acid-binding agents, making it a green and clean process. However, this method is slow and has low triphosgene atom utilization. A large amount of phosgene generated by solid-state photolysis is not utilized and escapes into the exhaust gas along with the generated gas. Furthermore, a large amount of phosgene is mixed with the hydrochloric acid in the exhaust gas, seriously complicating exhaust gas treatment. Utility Model Content

[0004] The purpose of the utility model is to solve the shortcomings of the prior art and to propose a reaction device.

[0005] In order to achieve the above-mentioned purpose, the present invention adopts the following technical solution: a reaction device comprising:

[0006] Configuration kettle and dissolving kettle;

[0007] The output ends of the configuration kettle and the dissolution kettle are connected to the reaction kettle;

[0008] After the reaction in the reactor, the liquid is output to the filter, and the output end of the filter is connected to the mother liquid tank;

[0009] The mother liquid tank transports the reaction liquid to the post-processing stage through a transfer pump.

[0010] As a further description of the above technical solution: a first condenser is provided at the upper input end of the configuration kettle, and a second condenser is provided at the upper input end of the dissolution kettle.

[0011] As a further description of the above technical solution: one end of the first condenser and the second condenser is connected to the outside through a pipeline for discharging exhaust gas.

[0012] As a further description of the above technical solution: the output end of the dissolving kettle is connected to the reaction kettle via a drip pump.

[0013] As a further description of the above technical solution: the upper ends of the configuration kettle, the dissolution kettle and the reaction kettle are connected to the vacuum pipeline and the nitrogen pipeline through valves.

[0014] As a further description of the above technical solution: a venting pipeline is also provided at the upper end of the reactor through a valve.

[0015] As a further description of the above technical solution: an emergency emptying pipeline is provided between the configuration kettle and the reaction kettle.

[0016] As a further description of the above technical solution: the dripping pump is a high-pressure dripping pump, and the reactor is a high-pressure reactor.

[0017] As a further description of the above technical solution: the reactor is provided with a pressure gauge and a thermometer.

[0018] As a further description of the above technical solution: the output end of the material transfer pump is connected through a pipeline to transport the reaction liquid in the mother liquid tank to the post-processing device.

[0019] The above technical solution has the following advantages or beneficial effects:

[0020] 1. By configuring the coordinated use of the kettle, dissolving kettle, high-pressure reactor, filter, mother liquid tank, and transfer pump, the use of the high-pressure reactor can significantly reduce the use of chlorination reagents for light fixation, which can reduce the use of light fixation by 50%, and reduce the phosgene content in the tail gas by more than 90%, effectively reducing production costs. At the same time, the phosgene content in the waste gas is lower, and treatment is more convenient. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 This is a schematic structural diagram of the reaction device proposed in the present invention.

[0022] Legend:

[0023] 1. Preparation kettle; 2. Dissolution kettle; 3. First condenser; 4. Second condenser; 5. Reactor; 6. Dropping pump; 7. Filter; 8. Mother liquor tank; 9. Transfer pump. DETAILED DESCRIPTION

[0024] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0025] Reference Figure 1 The utility model provides an embodiment: a reaction device, comprising: a configuration kettle 1 and a dissolving kettle 2; the output ends of the configuration kettle 1 and the dissolving kettle 2 are connected to the reactor 5; the output after the reaction in the reactor 5 is output to the filter 7, and the output end of the filter 7 is connected to the mother liquid tank 8; the mother liquid tank 8 transports the reaction liquid to the post-processing stage through the transfer pump 9.

[0026] In this embodiment, the kettle 1 is configured for the configuration of raw materials and catalysts, the dissolving kettle 2 is used for dissolving solid light in dichloroethane, and the kettle 1 and the dissolving kettle 2 are configured as stirring kettles, which can fully stir the materials inside; the reactor 5 is used as a container for the chlorination reaction of 4,6-dihydroxypyrimidine and solid light, and is used for the chlorination reaction of the raw material 4,6-dihydroxypyrimidine and solid light under the action of the catalyst. The phosgene decomposed by solid light can be fully utilized in the reactor, thereby saving solid light. The filter 7 is arranged below the output end of the reactor 5 to filter out the insoluble matter and impurities after the reaction. The mother liquid tank 8 is arranged behind the filter 7 to receive the filtered reaction liquid. The material transfer pump 9 is arranged behind the mother liquid tank 8 to transfer the material to the post-processing desolventizing and distillation operation. The desolventizing and distillation section is used to prepare high-quality 4,6-dichloropyrimidine.

[0027] By configuring the coordinated use of the kettle 1, the dissolving kettle 2, the reactor 5, the filter 7, the mother liquid tank 8, and the transfer pump 9, the use of the reactor 5 can significantly reduce the use of the chlorination reagent for light fixation, which can reduce the use of light fixation by 50%, and reduce the phosgene content in the tail gas by more than 90%, effectively reducing the production cost. At the same time, the phosgene content in the waste gas is lower, and the treatment is more convenient.

[0028] The material of the configuration kettle 1 is glass-lined, the material of the dissolving kettle 2 is glass-lined, and the material of the reaction kettle 5 is C276, which can meet the requirements of high temperature and high pressure use.

[0029] A first condenser 3 is provided at the upper input end of the configuration kettle 1 , and a second condenser 4 is provided at the upper input end of the dissolution kettle 2 .

[0030] In this embodiment, the volatilized solvent in the preparation kettle 1 and the dissolution kettle 2 is condensed and refluxed by the first condenser 3 and the second condenser 4 .

[0031] One end of the first condenser 3 and the second condenser 4 is connected to the outside through a pipeline for discharging exhaust gas.

[0032] The output end of the dissolving kettle 2 is connected to the reaction kettle 5 via a dripping pump 6 , and is in communication with the reaction kettle 5 , and is used to drip the light-fixing solution into the reaction kettle 5 under high pressure.

[0033] The upper ends of the configuration kettle 1, the dissolving kettle 2 and the reaction kettle 5 are connected to the vacuum pipeline and the nitrogen pipeline through valves.

[0034] In this embodiment, the environment inside the configuration kettle 1, the dissolution kettle 2 and the reaction kettle 5 is in a negative pressure state through the vacuum pipeline, which is convenient for transporting the raw materials. A nitrogen pipeline is provided for subsequent nitrogen replacement in the reaction.

[0035] A vent line is also provided at the upper end of the reactor 5 through a valve, so that the residual gas can be discharged after the reaction is completed.

[0036] An emergency drain line is provided between the configuration kettle 1 and the reaction kettle 5 .

[0037] In this embodiment, the reactor 5 is provided with an emergency drain line, which is used to drain the materials to a safe place in case of abnormal temperature, pressure and other indicators during the reaction process, thereby reducing safety risks.

[0038] The dripping pump 6 is a high-pressure dripping pump, and the reactor 5 is a high-pressure reactor. The reactor 5 is provided with a pressure gauge.

[0039] In this embodiment, the reactor 5 is a high-pressure reactor and is configured as a stirred reactor. The pressure resistance of the high-pressure reactor is greater than 8 MPa. A thermometer is provided in the high-pressure reactor, which displays the temperature in the high-pressure reactor, making it convenient for the operator to adjust the temperature in the reactor; the high-pressure reactor is provided with a pressure gauge, which displays the pressure in the high-pressure reactor, making it convenient for the operator to adjust the pressure in the reactor.

[0040] The output end of the material transfer pump 9 is connected through a pipeline to transport the reaction liquid in the mother liquid tank 8 to the post-processing device.

[0041] Working principle:

[0042] Take dichloroethane as the reaction solvent as an example:

[0043] First, open the feeding port of the configuration kettle 1, add the weighed 4,6-dihydroxypyrimidine and the weighed composite catalyst, close the feeding port, pump in the solvent dichloroethane, turn on the stirring to suspend the material. Open the feeding port of the dissolution kettle 2, add the weighed triphosgene, close the feeding port, pump in the solvent dichloroethane, open the nitrogen pipeline for nitrogen replacement, stir and heat until the triphosgene is dissolved. Open the valve on the transfer pipeline below the configuration kettle 1 and transfer the material to the reactor 5. After the transfer is completed, flush the pipeline with a small amount of solvent. After the flushing is completed, close the valve. Nitrogen replaces the system gas in the reactor 5, stir and heat to the required reaction temperature, open the discharge valve of the dissolution kettle 2 and the feed valve of the reactor 5, and use the drip pump 6 to drop the triphosgene solution in the dissolution kettle 2 into the reactor 5. The dripping is completed after 3-4 hours, and the temperature is kept for 2 hours. When the pressure reaches 6Mpa, the reaction is completed. The material temperature was cooled to below 30°C. The vent line was opened to exhaust the gas in the kettle. The system gas was replaced with nitrogen. Sampling was performed for central control. The raw material 4,6-dihydroxypyrimidine content was less than 0.5%, indicating the reaction was complete. The bottom valve of the reactor 5 was opened and the material was discharged into the filter 7 to filter out impurities, insoluble matter, and unreacted raw material. The filtered reaction liquid was stored in the mother liquid tank 8. After filtration, the reaction liquid was transferred through the material transfer pump 9 to remove solvents and distilled to obtain pure 4,6-dichloropyrimidine.

[0044] Finally, it should be noted that the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art can still modify the technical solutions described in the aforementioned embodiments or make equivalent replacements for some of the technical features therein. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A reaction device, characterized in that: include: A kettle (1) and a dissolving kettle (2) are provided; The output ends of the configuration kettle (1) and the dissolution kettle (2) are connected to the reaction kettle (5); After the reaction in the reactor (5), the liquid is output to the filter (7), and the output end of the filter (7) is connected to the mother liquid tank (8); The mother liquid tank (8) transports the reaction liquid to the post-processing stage through the material transfer pump (9).

2. The reaction device according to claim 1, characterized in that: A first condenser (3) is provided at the upper input end of the configuration kettle (1), and a second condenser (4) is provided at the upper input end of the dissolution kettle (2).

3. The reaction device according to claim 2, characterized in that: One end of the first condenser (3) and the second condenser (4) are connected to the outside through a pipeline for discharging tail gas.

4. The reaction device according to claim 1, characterized in that: The output end of the dissolving kettle (2) is connected to the reaction kettle (5) via a drip pump (6).

5. The reaction device according to claim 1, characterized in that: The upper ends of the configuration kettle (1), the dissolving kettle (2) and the reaction kettle (5) are connected to a vacuum pipeline and a nitrogen pipeline through valves.

6. The reaction device according to claim 1, characterized in that: The upper end of the reactor (5) is also provided with a venting pipeline via a valve.

7. The reaction device according to claim 1, characterized in that: An emergency drain pipeline is provided between the configuration kettle (1) and the reaction kettle (5).

8. The reaction device according to claim 4, characterized in that: The dripping pump (6) is a high-pressure dripping pump, and the reactor (5) is a high-pressure reactor.

9. The reaction device according to claim 1, characterized in that: The reactor (5) is provided with a pressure gauge and a thermometer.

10. The reaction device according to claim 1, characterized in that: The output end of the material transfer pump (9) is connected via a pipeline to transport the reaction liquid in the mother liquid tank (8) to a post-processing device.

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