Thifluzamide production system

Abstract

The utility model relates to the technical field of thifluzamide, in particular to a thifluzamide production system which comprises a reaction kettle body provided with a medium jacket on the outer side, a first stirring paddle is mounted in the reaction kettle body, and a polytetrafluoroethylene coating is arranged on the outer side of the first stirring paddle; a raw material inlet, a first outlet and a second outlet are formed in the top of the reaction kettle body, the raw material inlet is communicated with the mixing kettle discharge hole, and a second stirring paddle is arranged in the mixing kettle; the first outlet is communicated with a vacuum pipeline, the vacuum pipeline is communicated with a first condenser, and the first condenser is communicated with a toluene receiving tank; the second outlet is communicated with a reflux pipeline, the reflux pipeline is communicated with a second condenser, and the second condenser is communicated with the interior of the reaction kettle body; a bottom discharge port of the reaction kettle body is communicated with a washing filter through a discharge pipe; a solid discharge port of the washing filter is connected with a dryer. According to the utility model, the corrosion risk in the reaction process can be reduced, the heating and cooling functions are realized by arranging the medium interlayer, and the side reaction is avoided.

Description

Technical Field

[0001] This utility model relates to the field of thifluzamide technology, specifically to a thifluzamide production system. Background Technology

[0002] Thifluzamide, also known as thiamethoxam, has the chemical name 2',6'-dibromo-2-methyl-4'-trifluoromethoxy-4-trifluoromethyl-1,3-thiadiazole-5-hydroxyaniline and the molecular formula C. 13 H6Br2F6N2O2S, belonging to the thiazole amide class of bactericides, possesses strong systemic conductivity and long-lasting effect. The synthesis of thifluzamide can be achieved using 2-methyl-4-(trifluoromethyl)-1,3-thiazole-5-carboxylic acid as a starting material, mixed with thionyl chloride and heated under reflux. After the reflux reaction is complete, toluene is removed under reduced pressure. Then, 2,6-dibromo-4-trifluoromethoxyaniline is added to the reaction solution, and the mixture is heated under reflux until the reaction is complete. The specific reaction route is as follows:

[0003] .

[0004] In the production of thifluzamide, the reaction vessel has a significant impact on product quality and production efficiency. Firstly, the reactants for thifluzamide include thionyl chloride, which poses a corrosion risk to exposed metal components inside the reaction vessel. This could cause metal impurities to fall into or transfer into the reaction system, affecting product quality. Secondly, temperature control is crucial during the synthesis of thifluzamide. Excessively high reaction temperatures can easily trigger side reactions, forming more impurities and impacting product quality and yield. Utility Model Content

[0005] To address the technical problem that the reaction vessel has a significant impact on product quality during the production of thifluamide, this utility model provides a thifluamide production system that can reduce the risk of corrosion during the reaction process and achieve heating and cooling functions by setting up a medium jacket to avoid the occurrence of side reactions.

[0006] The technical solution of this utility model is as follows:

[0007] A thifluzamide production system includes a reactor body, a media jacket is provided on the outside of the reactor body, the media inlet and media outlet of the media jacket are connected through a media circulation pipeline, and the media circulation pipeline is provided with a circulation pump and a heat exchanger.

[0008] The reactor body is equipped with a first stirring blade, and the outside of the first stirring blade is coated with polytetrafluoroethylene.

[0009] The top of the reactor body is equipped with a raw material inlet, a thionyl chloride inlet, an acetonitrile inlet, a 2,6-dibromo-4-trifluoromethoxyaniline inlet, and a water inlet. The raw material inlet is connected to the discharge port of the mixing vessel. The interior of the mixing vessel is equipped with a second stirring paddle. The top of the mixing vessel is equipped with a toluene inlet and a 2-methyl-4-(trifluoromethyl)-1,3-thiazolyl-5-carboxylic acid inlet.

[0010] The reactor body is also equipped with a first outlet and a second outlet at the top. The first outlet is connected to one end of a vacuum pipe, which is equipped with a valve and a vacuum pump. The other end of the vacuum pipe is connected to the tube-side inlet of the first condenser, and the tube-side outlet of the first condenser is connected to a toluene receiving tank. The second outlet is connected to one end of a reflux pipe, which is equipped with a valve. The other end of the reflux pipe is connected to the tube-side inlet of the second condenser, and the tube-side outlet of the second condenser is connected to the interior of the reactor body.

[0011] The bottom of the reactor body is also equipped with a discharge port, which is connected to a washing filter through a discharge pipe. The solid discharge port of the washing filter is connected to a dryer through a conveying device.

[0012] Furthermore, the medium circulation pipeline is connected to the tube side of the heat exchanger, the shell side inlet of the heat exchanger is connected to the heating agent inlet pipeline and the cooling agent inlet pipeline respectively, and the shell side outlet of the heat exchanger is connected to the heating agent outlet pipeline and the cooling agent outlet pipeline respectively. Valves are installed on the heating agent inlet pipeline, the cooling agent inlet pipeline, the heating agent outlet pipeline and the cooling agent outlet pipeline respectively.

[0013] Furthermore, the inner wall of the reactor body is provided with an enamel layer. Enamel has good corrosion resistance and chemical stability. This utility model uses enamel material as the inner wall material of the reactor body, which can better resist erosion, extend the service life of the reactor, and ensure product quality.

[0014] Furthermore, the reactor body is equipped with an online thermometer. Technicians can determine whether the reaction system has reached the reaction temperature based on the detection results of the online thermometer. They can also use controllers to receive and analyze the temperature signals transmitted by the online thermometer and further control the opening and closing of valves and other components.

[0015] Furthermore, multiple baffles are staggered inside the medium jacket, which can continuously change the flow direction of the medium during the flow process, further enhancing the heat transfer effect.

[0016] Furthermore, a sampling port is provided on the discharge pipe to facilitate technicians in taking samples to test whether the material reaction is complete.

[0017] Furthermore, the toluene receiving tank is connected to the toluene inlet of the mixing vessel via a pipeline. By setting up this structure, the toluene removed under reduced pressure within the reactor body can be reused in the reaction as a solvent.

[0018] The beneficial effects of this utility model are as follows:

[0019] According to the thifluzamide synthesis route, the temperature inside the reactor needs to be adjusted and controlled within different ranges, including the heating reflux temperature (approximately 60-90°C), room temperature, and crystallization temperature (approximately 10-15°C). This invention incorporates a heat exchanger in the medium circulation pipeline, connecting both the heating agent and the cooling agent. Depending on the reaction progress, the valves can be manually or controlled by a controller to switch the carriers within the heat exchanger, thus allowing the medium to be cooled or heated within it. The heat-exchanged medium is then passed through a medium jacket to heat or cool the reaction system, thereby controlling the reaction temperature and reducing side reactions. Secondly, this invention features a polytetrafluoroethylene (PTFE) coating on the outside of the stirring paddle. The extremely low surface energy of PTFE provides corrosion resistance and reduces material adhesion to the stirring paddle. Simultaneously, a first outlet and a second outlet are located at the top of the reactor body for depressurization desolvation and heating reflux operations, respectively. This allows for multiple reactions to proceed within the same reactor body, reducing material loss due to transfer and lowering the risk of contamination. Attached Figure Description

[0020] To more clearly illustrate the technical solution of this utility model, the drawings used in the description will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0021] Figure 1 This is a schematic diagram of the thifluzamide production system in Example 1.

[0022] In the diagram, 1-Reaction vessel body, 2-Washing filter, 3-Dryer, 4-Sampling port, 5-Media jacket, 6-Baffle plate, 7-Media circulation pipeline, 8-Circulation pump, 9-Heat exchanger, 10-Heating agent feed pipeline, 11-Coolant feed pipeline, 12-Heating agent discharge pipeline, 13-Coolant discharge pipeline, 14-First stirring paddle, 15-Mixing vessel, 16-Second stirring paddle, 17-Vacuum pipeline, 18-Vacuum pump, 19-First condenser, 20-Toluene receiving tank, 21-Reflux pipeline, 22-Second condenser. Detailed Implementation

[0023] To make the objectives, features, and advantages of this utility model more apparent and understandable, the technical solutions of this utility model will be clearly and completely described below with reference to the accompanying drawings of the specific embodiments. Obviously, the embodiments described below are only some embodiments of this utility model, and not all embodiments. Based on the embodiments of this patent, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this patent.

[0024] Example 1

[0025] A thifluzamide production system includes a reactor body 1, a washing filter 2, and a dryer 3. The reactor body 1 has a discharge port at the bottom, which is connected to the washing filter 2 through a discharge pipe. The solid discharge port of the washing filter 2 is connected to the dryer 3 through a conveying device. A sampling port 4 is provided on the discharge pipe.

[0026] The reactor body 1 is provided with a medium jacket 5 on the outside. Multiple baffles 6 are installed alternately inside the medium jacket 5. The medium inlet and medium outlet of the medium jacket 5 are connected through a medium circulation pipeline 7. The medium circulation pipeline 7 is provided with a circulation pump 8 and a heat exchanger 9. Specifically, the medium circulation pipeline 7 is connected to the tube side of the heat exchanger 9. The shell side inlet of the heat exchanger 9 is connected to the heating agent inlet pipeline 10 and the coolant inlet pipeline 11, respectively. The shell side outlet of the heat exchanger 9 is connected to the heating agent outlet pipeline 12 and the coolant outlet pipeline 13, respectively. Valves are respectively installed on the heating agent inlet pipeline 10, the coolant inlet pipeline 11, the heating agent outlet pipeline 12, and the coolant outlet pipeline 13.

[0027] The inner wall of the reactor body 1 is provided with an enamel layer. A first stirring paddle 14 is installed inside the reactor body 1. The outer side of the first stirring paddle 14 is provided with a polytetrafluoroethylene coating. An online thermometer is also installed inside the reactor body 1 to monitor the material temperature inside the reactor body 1.

[0028] The top of the reaction vessel body 1 is equipped with a raw material inlet, a thionyl chloride inlet, an acetonitrile inlet, a 2,6-dibromo-4-trifluoromethoxyaniline inlet, and a water inlet. The raw material inlet is connected to the discharge port of the mixing vessel 15. The mixing vessel 15 is equipped with a second stirring paddle 16 inside. The top of the mixing vessel 15 is equipped with a toluene inlet and a 2-methyl-4-(trifluoromethyl)-1,3-thiazole-5-carboxylic acid inlet.

[0029] The reactor body 1 is also provided with a first outlet and a second outlet at the top. The first outlet is connected to one end of a vacuum pipe 17, which is equipped with a valve and a vacuum pump 18. The other end of the vacuum pipe 17 is connected to the tube-side inlet of the first condenser 19. The tube-side outlet of the first condenser 19 is connected to a toluene receiving tank 20, which is connected to the toluene inlet of the mixing vessel 15 through a pipe. The second outlet is connected to one end of a reflux pipe 21, which is equipped with a valve and a reflux pump 19. The other end of the reflux pipe 21 is connected to the tube-side inlet of the second condenser 22, and the tube-side outlet of the second condenser 22 is connected to the interior of the reactor body 1.

[0030] Using the thifluzamide production system of this embodiment, toluene and 2-methyl-4-(trifluoromethyl)-1,3-thiazol-5-carboxylic acid are first introduced into the mixing vessel 15 through their respective inlets. After being mixed evenly by the second stirring paddle 16, they are introduced into the reactor body 1 through the raw material inlet located at the top of the reactor body 1. Then, thionyl chloride is added into the reactor body 1 through its corresponding inlet. The first stirring paddle 14 is turned on, and the circulation of the medium in the medium jacket is started. The corresponding heating or cooling agent is introduced into the shell side of the heat exchanger 9 to control the internal temperature of the reactor body 1. The material is maintained at a suitable temperature and then heated to the reflux temperature. The valve on the reflux pipe 21 is opened, and the evaporated material is condensed through the second condenser 22 and returned to the reactor body 1. After reacting for a period of time, the valve on the reflux pipe 21 is closed, and the medium is cooled using a coolant. The medium circulates in the medium jacket, reducing the temperature of the material in the reactor body 1 to room temperature. Then, the valve on the vacuum pipe 17 and the vacuum pump 18 are opened, and in conjunction with the medium jacket, the solvent (toluene) in the reaction liquid is removed by depressurization. The removed toluene passes through the first condenser 19. The resulting liquid phase is collected in toluene receiving tank 20, where this portion of toluene can be reused as a solvent. Then, the corresponding materials are introduced into the reactor body 1 through the acetonitrile inlet and the 2,6-dibromo-4-trifluoromethoxyaniline inlet. The medium in the media jacket heats the reaction liquid in the reactor body 1 to the reflux temperature. The valve on the reflux pipe 21 is opened, and the evaporated material is condensed by the second condenser 22 and returned to the reactor body 1. After a period of reaction, the valve on the reflux pipe 21 is closed, and a sample is taken from the sampling port 4 on the discharge pipe for analysis. After the reaction is complete, the coolant is passed through the shell side of the heat exchanger 9 to cool the medium. The cooled medium flows through the medium jacket to cool the reaction liquid. The first agitator 14 is turned on, and water is added to the reactor body 1 while stirring to allow the product to be fully separated. Then the material enters the washing filter 2 through the discharge pipe. The washing filter 2 is existing technology. Its function is to perform solid-liquid separation and rinsing of the reaction material. The solid after washing and filtration is discharged from the solid discharge port and sent to the dryer 3 through the conveying device for drying to obtain thifluzamide.

[0031] The above description of the disclosed embodiments enables those skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A thifluzamide production system comprising a reaction vessel body, characterized by, The medium jacket is provided outside the reaction kettle body, the medium inlet and the medium outlet of the medium jacket are communicated through a medium circulation pipeline, and the medium circulation pipeline is provided with a circulating pump and a heat exchanger. The first stirring paddle is installed inside the reaction kettle body, and a polytetrafluoroethylene coating is arranged outside the first stirring paddle. The reaction kettle body is provided with a raw material inlet, a thionyl chloride inlet, an acetonitrile inlet, a 2,6-dibromo-4-trifluoromethoxy aniline inlet and a water inlet at the top, wherein the raw material inlet is communicated with the discharge port of the mixing kettle, the mixing kettle is provided with a second stirring paddle inside, and the mixing kettle is provided with a toluene inlet and a 2-methyl-4-(trifluoromethyl)-1,3-thiazole-5-carboxylic acid inlet at the top. The reaction kettle body is further provided with a first outlet and a second outlet at the top, the first outlet is communicated with one end of a vacuum pipeline, a valve and a vacuum pump are arranged on the vacuum pipeline, the other end of the vacuum pipeline is communicated with the tube side inlet of the first condenser, and the tube side outlet of the first condenser is communicated with a toluene receiving tank; the second outlet is communicated with one end of a reflux pipeline, a valve is arranged on the reflux pipeline, and the other end of the reflux pipeline is communicated with the tube side inlet of the second condenser, and the tube side outlet of the second condenser is communicated with the inside of the reaction kettle body. The reaction kettle body is further provided with a discharge port at the bottom, the discharge port is communicated with a washing filter through a discharge pipe, and the solid discharge port of the washing filter is connected with a dryer through a conveying device.

2. The thifluzamide production system according to claim 1, wherein The medium circulation pipeline is communicated with the tube side of the heat exchanger, the shell side inlets of the heat exchanger are respectively communicated with a heating agent feeding pipeline and a cooling agent feeding pipeline, the shell side outlets of the heat exchanger are respectively communicated with a heating agent discharging pipeline and a cooling agent discharging pipeline, and valves are arranged on the heating agent feeding pipeline, the cooling agent feeding pipeline, the heating agent discharging pipeline and the cooling agent discharging pipeline.

3. The thifluzamide production system according to claim 1, wherein The inner wall of the reaction kettle body is provided with an enamel layer.

4. The thifluzamide production system according to claim 1, wherein An online thermometer is arranged inside the reaction kettle body.

5. The thifluzamide production system according to claim 1, wherein A plurality of baffles are arranged in the medium jacket.

6. The thifluzamide production system according to claim 1, wherein A sampling port is arranged on the discharge pipe.

7. The thifluzamide production system according to claim 1, wherein The toluene receiving tank is communicated with the toluene inlet of the mixing kettle through a pipeline.

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