2-ethylthio-3-chloro-trifluorotoluene production device

Abstract

The utility model discloses a 2-ethylthio-3-chloro-trifluorotoluene production device which comprises a DMF (Dimethyl Formamide) head tank, an ethanethiol head tank, a 2-fluoro-3-chloro-trifluorotoluene feeding pipe and an etherification reaction kettle, the etherification reaction kettle comprises a reaction kettle main body, a cooling jacket is arranged on a shell of the reaction kettle main body, and the cooling jacket is connected with the etherification reaction kettle. And a built-in cooling coil pipe is arranged in the shell of the reaction kettle main body. The etherification reaction kettle has the advantages that the built-in cooling coil pipe is additionally arranged on the basis of cooling of the jacket of the shell, frozen saline water can be fed into the etherification reaction kettle through the built-in cooling coil pipe, then heat released by reaction is directly taken away in time, solvent volatilization is reduced, meanwhile, side reaction can be effectively inhibited, and the service life of the etherification reaction kettle is prolonged. Impurities are reduced, and the yield of the intermediate is improved. In addition, the solvent volatilized along with the tail gas is condensed through the first condenser to be recycled, and the recycling rate of the solvent is increased.

Description

Technical fields:

[0001] This utility model relates to the field of penoxsulam production technology, and more specifically to a 2-ethylthio-3-chloro-trifluorotoluene production apparatus. Background technology:

[0002] Penoxsulam is a sulfonamide herbicide, mainly used for the efficient control of various weeds in rice paddies and seedling beds. It also has good control efficacy against barnyard grass that has developed resistance to herbicides such as sulfonylureas and acetyl-CoA carboxylase inhibitors. Furthermore, the residual penoxsulam is easily degraded by photosynthesis and microorganisms.

[0003] 2-Ethylthio-3-chloro-trifluorotoluene is an important intermediate in the production of penoxsulam. This intermediate is produced from 2-fluoro-3-chlorotrifluorotoluene and ethanethiol as raw materials, with DMF as solvent, through a nucleophilic substitution reaction in an etherification reactor under the influence of strong bases such as sodium hydroxide and potassium hydroxide. This reaction is highly exothermic, and excessively high temperatures result in excessive impurities, affecting the yield of the intermediate. Therefore, a low-temperature environment is more conducive to this reaction. However, traditional etherification reactors only have a jacket on the shell through which chilled brine is circulated to regulate the temperature, achieving only external temperature control and failing to regulate the internal temperature of the reactor. This leads to excessively high temperatures at the center of the reactor, resulting in a large amount of solvent being discharged into the tail gas manifold, wasting raw materials. Furthermore, excessively high center temperatures increase impurities, severely affecting the yield of the intermediate and impacting production costs. Moreover, controlling the heat of reaction requires slowing down the production rate, severely restricting yield and increasing production costs. Utility model content:

[0004] The purpose of this invention is to provide a production apparatus for 2-ethylthio-3-chloro-trifluorotoluene.

[0005] This utility model is implemented by the following technical solution: a 2-ethylthio-3-chloro-trifluorotoluene production device, comprising a DMF high-level tank, an ethanethiol high-level tank, a 2-fluoro-3-chloro-trifluorotoluene feed pipe, and an etherification reactor. The outlet of the DMF high-level tank, the outlet of the ethanethiol high-level tank, and the 2-fluoro-3-chloro-trifluorotoluene feed pipe are all connected to the inlet of the etherification reactor. The etherification reactor includes a reactor body, a cooling jacket is provided in the shell of the reactor body, and an internal cooling coil is provided inside the shell of the reactor body. The gas phase outlet of the etherification reactor is connected to the inlet of a first condenser. The liquid phase outlet of a condenser is connected to the inlet of a first recovery tank, and the outlet of the first recovery tank is connected to the inlet of the etherification reactor. The bottom outlet of the etherification reactor is connected to the inlet of a filter press, and the solid phase outlet of the filter press is connected to a sodium fluoride discharge pipe. The liquid phase outlet of the filter press is connected to the inlet of a distillation kettle. The bottom outlet of the distillation kettle is connected to a crude 2-ethylthio-3-chloro-trifluorotoluene discharge pipe. The gas phase outlet of the distillation kettle is connected to the inlet of a second condenser, and the liquid phase outlet of the second condenser is connected to the inlet of a second recovery tank. The outlet of the second recovery tank is connected to the inlet of the DMF high-level tank.

[0006] Furthermore, both the first condenser and the second condenser include a circulating water heat exchanger and a chilled brine heat exchanger connected in series.

[0007] Furthermore, a preheater is connected between the liquid phase outlet of the filter press and the feed inlet of the distillation vessel, and the outlets of the circulating water heat exchangers of the first condenser and the second condenser are connected to the inlet of the preheater.

[0008] Furthermore, a buffer tank is provided between the liquid phase outlet of the second condenser and the inlet of the second recovery tank, and a connecting pipe connects the second recovery tank and the buffer tank.

[0009] Advantages of this invention: The etherification reactor in this application incorporates a built-in cooling coil in addition to the existing jacketed cooling system. This built-in cooling coil allows chilled brine to be introduced into the reactor, directly removing the heat released during the reaction. This reduces solvent evaporation, effectively suppresses side reactions, minimizes impurities, and increases the yield of intermediates. Furthermore, the solvent evaporated with the exhaust gas is recovered through condensation in the first condenser, improving solvent recovery efficiency. Water from the circulating water heat exchanger is sent to the preheater to preheat the material before it enters the distillation vessel, thereby increasing the feed temperature and reducing steam consumption. Attached image description:

[0010] Figure 1This is an overall structural diagram of Example 1.

[0011] Figure 2 This is an overall structural diagram of Example 2.

[0012] 1. DMF high-level tank; 2. Ethyl mercaptan high-level tank; 3. 2-Fluoro-3-chlorotrifluorotoluene feed pipe; 4. Etherification reactor; 41. Cooling jacket; 42. Cooling coil; 5. First condenser; 6. First recovery tank; 7. Filter press; 8. Sodium fluoride discharge pipe; 9. Distillation kettle; 10. 2-Ethylthio-3-chlorotrifluorotoluene crude product discharge pipe; 11. Second condenser; 12. Second recovery tank; 13. Circulating water heat exchanger; 14. Chilled brine heat exchanger; 17. Preheater; 18. Buffer tank; 19. Connecting pipe. Detailed implementation method:

[0013] In the description of this utility model, it should be noted that the terms "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this utility model. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.

[0014] Example 1: As Figure 1As shown, a 2-ethylthio-3-chloro-trifluorotoluene production apparatus includes a DMF high-level tank 1, an ethanethiol high-level tank 2, a 2-fluoro-3-chloro-trifluorotoluene feed pipe 3, and an etherification reactor 4. The outlets of the DMF high-level tank 1, the ethanethiol high-level tank 2, and the 2-fluoro-3-chloro-trifluorotoluene feed pipe 3 are all connected to the inlet of the etherification reactor 4. The etherification reactor 4 includes a reactor body, a cooling jacket 41 installed in the shell of the reactor body, and an internal cooling coil 42 installed inside the shell of the reactor body. The gas phase outlet of the etherification reactor 4 is connected to the inlet of a first condenser 5, and the liquid phase outlet of the first condenser 5 is connected to the gas phase outlet of the first condenser 5. The outlet of the first recovery tank 6 is connected to the inlet of the first recovery tank 6, and the outlet of the first recovery tank 6 is connected to the inlet of the etherification reactor 4. The bottom outlet of the etherification reactor 4 is connected to the inlet of the filter press 7. The solid phase outlet of the filter press 7 is connected to the sodium fluoride discharge pipe 8, and the liquid phase outlet of the filter press 7 is connected to the inlet of the distillation kettle 9. The bottom outlet of the distillation kettle 9 is connected to the crude 2-ethylthio-3-chloro-trifluorotoluene discharge pipe 10. The gas phase outlet of the distillation kettle 9 is connected to the inlet of the second condenser 11, and the liquid phase outlet of the second condenser 11 is connected to the inlet of the second recovery tank 12. The outlet of the second recovery tank 12 is connected to the inlet of the DMF high-level tank 1. Both the first condenser 5 and the second condenser 11 include a circulating water heat exchanger 13 and a chilled brine heat exchanger 14 connected in series. A buffer tank 18 is provided between the liquid phase outlet of the second condenser 11 and the inlet of the second recovery tank 12, and a connecting pipe 19 connects the second recovery tank 12 and the buffer tank 18.

[0015] Production process:

[0016] The DMF solvent, ethanethiol, and 2-fluoro-3-chlorotrifluorotoluene raw materials, supplied from the DMF high-level tank 1, the ethanethiol high-level tank 2, and the 2-fluoro-3-chlorotrifluorotoluene feed pipe 3, are fed into the etherification reactor 4 in a certain proportion. Sodium hydroxide is added to the etherification reactor 4 through the manhole, and the raw materials react under the action of sodium hydroxide. During this process, the internal temperature of the etherification reactor 4 is reduced to -20°C by feeding chilled brine into the cooling jacket 41 and the cooling coil 42, and the heat of reaction is removed from the etherification reactor 4 by the chilled brine.

[0017] The gas phase discharged from the etherification reactor 4 is condensed by the first condenser 5. The condensate discharged from the first condenser 5 is collected in the first recovery tank 6. When the liquid in the first recovery tank 6 reaches a certain level, the collected liquid is sent back to the etherification reactor 4 for reuse.

[0018] The liquid phase discharged from the etherification reactor 4 is first separated into solid and liquid phases by the filter press 7. The separated solid phase is discharged through the sodium fluoride discharge pipe 8, while the separated liquid phase is sent to the distillation reactor 9 for distillation. The crude 2-ethylthio-3-chlorotrifluorotoluene at the bottom of the distillation reactor 9 is discharged to the subsequent purification system through the crude 2-ethylthio-3-chlorotrifluorotoluene discharge pipe 10. The gas discharged from the distillation reactor 9 is sent to the second condenser 11 for condensation. The condensate is buffered by the buffer pipe 18 and then stored in the second recovery tank 12. The liquid collected in the second recovery tank 12 can be periodically returned to the DMF high-level tank 1 to realize solvent recovery.

[0019] Example 2: Its overall structure is the same as that of Example 1, except that, as Figure 2 As shown, a preheater 17 is connected between the liquid phase outlet of the filter press 7 and the feed inlet of the distillation kettle 9. The outlets of the circulating water heat exchangers 13 of the first condenser 5 and the second condenser 11 are connected to the inlet of the preheater 17. In the production process of Example 1, the outlet temperature of the circulating water heat exchanger 13 is 40-50°C. In order to realize the recovery and utilization of heat and reduce the steam consumption of the distillation kettle 9, the outlet water of the circulating water heat exchanger 13 is sent to the preheater 17 to preheat the material before it enters the distillation kettle 9, thereby increasing the feed temperature of the distillation kettle 9 and reducing steam consumption.

[0020] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of this utility model, and are not intended to limit it. Although the utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of this utility model.

Claims

1. A 2-ethylsulfanyl-3-chloro-trifluoromethylbenzene production device comprising a DMF head tank, an ethyl mercaptan head tank, a 2-fluoro-3-chlorotrifluoromethylbenzene feed pipe, and an etherification reactor, the discharge port of the DMF head tank, the discharge port of the ethyl mercaptan head tank, and the 2-fluoro-3-chlorotrifluoromethylbenzene feed pipe are all in communication with the feed port of the etherification reactor, characterized in that, The etherification reactor comprises a reactor main body, a cooling jacket is arranged on the shell of the reactor main body, and an internal cooling coil is arranged in the shell of the reactor main body; the gas phase outlet of the etherification reactor is communicated with the inlet of a first condenser, the liquid phase outlet of the first condenser is communicated with the inlet of a first recovery tank, and the discharge outlet of the first recovery tank is communicated with the feeding inlet of the etherification reactor; the bottom discharge outlet of the etherification reactor is communicated with the inlet of a filter press, the solid phase outlet of the filter press is communicated with a sodium fluoride discharge pipe, the liquid phase outlet of the filter press is communicated with the inlet of a distillation kettle; the bottom discharge outlet of the distillation kettle is communicated with a 2-ethylsulfanyl-3-chloro-trifluoromethylbenzene crude product discharge pipe, the gas phase outlet of the distillation kettle is communicated with the inlet of a second condenser, the liquid phase outlet of the second condenser is communicated with the inlet of a second recovery tank, and the discharge outlet of the second recovery tank is communicated with the feeding inlet of a DMF high tank.

2. A device for producing 2-ethylsulfanyl-3-chloro-tolunitrifluoride according to claim 1, characterized in that, The first condenser and the second condenser both comprise a circulating water heat exchanger and a refrigerated brine heat exchanger connected in series.

3. A device for producing 2-ethylsulfanyl-3-chloro-tolunitrifluoride according to claim 2, characterized in that, A preheater is connected between the liquid phase outlet of the filter press and the feeding inlet of the distillation kettle, and the outlet of the circulating water heat exchanger of the first condenser and the outlet of the circulating water heat exchanger of the second condenser are communicated with the inlet of the preheater.

4. The apparatus according to claim 1, wherein A buffer tank is arranged between the liquid phase outlet of the second condenser and the inlet of the second recovery tank, and a communication pipe is communicated between the second recovery tank and the buffer tank.

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