An apparatus for the preparation of 2,4,4'-trichloro-2'-nitrodiphenyl ether

Abstract

This utility model discloses an apparatus for preparing 2,4,4'-trichloro-2'-nitrodiphenyl ether, relating to the technical field of 2,4,4'-trichloro-2'-nitrodiphenyl ether production apparatus. The inlet of the reaction vessel is connected via pipelines to a 2,4-dichlorophenol tank, a 2-nitro-4-chlorophenol tank, a sodium hydroxide tank, and an N,N-dimethylformamide tank. The outlet of the reaction vessel is connected via pipelines to an extraction tank. The inlet of the extraction tank is connected via pipelines to a deionized water tank and an ethyl acetate tank. The outlet of the extraction tank is connected via pipelines to an organic phase tank. The outlet of the organic phase tank is connected via pipelines to a drying tank. The inlet of the drying tank is connected via pipelines to an anhydrous sodium sulfate tank. The outlet of the drying tank is connected via pipelines to a vacuum distillation tank. The bottom outlet of the vacuum distillation tank is connected via pipelines to a product tank. The process is simple, and the product yield and purity are high.

Description

Technical Field

[0001] This utility model relates to the technical field of 2,4,4'-trichloro-2'-nitrodiphenyl ether production equipment, specifically to a preparation device for 2,4,4'-trichloro-2'-nitrodiphenyl ether. Background Technology

[0002] 2,4,4'-Trichloro-2'-nitrodiphenyl ether is an important organic synthesis intermediate widely used in pharmaceuticals, pesticides, and dyes. Currently, its traditional production process typically uses 2,4-dichlorophenol and 2,5-dichloronitrobenzene as raw materials, with a strong base as an acid-binding agent. Under strong alkaline conditions, the 2,5-dichloronitrobenzene raw material undergoes partial hydrolysis, causing the chlorine atom at the 2-position of its benzene ring to hydrolyze into a hydroxyl group, yielding 2,4,4'-trichloro-2'-nitrodiphenyl ether. However, this process requires prior hydrolysis of 2,5-dichloronitrobenzene, involves multiple reaction steps, produces numerous byproducts, and makes subsequent product separation difficult, resulting in low yield and purity. Summary of the Invention

[0003] The technical problem to be solved by this utility model is to provide a preparation device for 2,4,4'-trichloro-2'-nitrodiphenyl ether, which is simple in equipment and has high product yield and purity, in order to address the shortcomings of the existing technology.

[0004] To solve the above-mentioned technical problems, the technical solution of this utility model is as follows:

[0005] An apparatus for preparing 2,4,4'-trichloro-2'-nitrodiphenyl ether includes a reaction vessel. The inlet of the reaction vessel is connected via pipes to a 2,4-dichlorophenol tank, a 2-nitro-4-chlorophenol tank, a sodium hydroxide tank, and an N,N-dimethylformamide tank. The outlet of the reaction vessel is connected via pipes to an extraction tank. The inlet of the extraction tank is connected via pipes to a deionized water tank and an ethyl acetate tank. The outlet of the extraction tank is connected via pipes to an organic phase tank. The outlet of the organic phase tank is connected via pipes to a drying tank. The inlet of the drying tank is connected via pipes to an anhydrous sodium sulfate tank. The outlet of the drying tank is connected via pipes to a vacuum distillation tank. The bottom outlet of the vacuum distillation tank is connected via pipes to a product tank.

[0006] As an improved technical solution, the bottom inlet of the reactor is connected to a nitrogen tank via a pipeline.

[0007] As an improved technical solution, the top gas phase outlet of the vacuum distillation tank is connected to a first evaporator via a pipeline, the top gas phase outlet of the first evaporator is connected to an ethyl acetate recovery tank via a pipeline, and the outlet of the ethyl acetate recovery tank is connected to the ethyl acetate tank via a pipeline.

[0008] As an improved technical solution, the outlet of the extraction tank is connected to an inorganic phase tank via a pipeline, the outlet of the inorganic phase tank is connected to a second evaporator via a pipeline, and the top gas phase outlet of the second evaporator is connected to an N,N-dimethylformamide recovery tank via a pipeline.

[0009] As an improved technical solution, the outlet of the product tank is connected to a recrystallization tank via a pipeline, the inlet of the recrystallization tank is connected to a first solvent tank via a pipeline, the outlet of the recrystallization tank is connected to a centrifuge via a pipeline, the outlet of the centrifuge is connected to a dryer via a pipeline, and the outlet of the dryer is connected to a pure product tank via a pipeline.

[0010] As an improved technical solution, the centrifuge outlet is connected to a rinsing tank via a pipe, the rinsing tank inlet is connected to a second solvent tank via a pipe, and the rinsing tank outlet is connected to the dryer via a pipe.

[0011] As a preferred technical solution, the liquid phase outlet of the centrifuge is connected to a third evaporator via a pipeline, the top gas phase outlet of the third evaporator is connected to a solvent recovery tank via a pipeline, and the outlet of the solvent recovery tank is connected to a second solvent tank via a pipeline.

[0012] As a preferred technical solution, the outlet of the rinsing tank is connected to the third evaporating tank via a pipeline.

[0013] As a preferred technical solution, the outlet of the 2,4-dichlorophenol tank is connected to a first purification tank via a pipeline, the inlet of the first purification tank is connected to a first ethanol tank via a pipeline, the outlet of the first purification tank is connected to a first filter via a pipeline, the solid phase outlet of the first filter is connected to a purified 2,4-dichlorophenol tank via a pipeline, and the outlet of the purified 2,4-dichlorophenol tank is connected to the reaction vessel via a pipeline.

[0014] The liquid phase outlet of the first filter is connected to a fourth evaporator via a pipeline, and the top gas phase outlet of the fourth evaporator is connected to a first ethanol recovery tank via a pipeline. The outlet of the first ethanol recovery tank is connected to the first ethanol tank via a pipeline.

[0015] As a preferred technical solution, the outlet of the 2-nitro-4-chlorophenol tank is connected to a second purification tank via a pipeline, the inlet of the second purification tank is connected to a second ethanol tank via a pipeline, the outlet of the second purification tank is connected to a second filter via a pipeline, the solid phase outlet of the second filter is connected to a purifying 2-nitro-4-chlorophenol tank via a pipeline, and the outlet of the purifying 2-nitro-4-chlorophenol tank is connected to the reaction vessel via a pipeline.

[0016] The liquid phase outlet of the second filter is connected to a fifth evaporator via a pipeline. The top gas phase outlet of the fifth evaporator is connected to a second ethanol recovery tank via a pipeline. The outlet of the second ethanol recovery tank is connected to the second ethanol tank via a pipeline.

[0017] Due to the adoption of the above technical solution, the beneficial effects of this utility model are:

[0018] This invention relates to an apparatus for preparing 2,4,4'-trichloro-2'-nitrodiphenyl ether, comprising a reaction vessel. The inlet of the reaction vessel is connected via pipes to a 2,4-dichlorophenol tank, a 2-nitro-4-chlorophenol tank, a sodium hydroxide tank, and an N,N-dimethylformamide tank. The outlet of the reaction vessel is connected via pipes to an extraction tank. The inlet of the extraction tank is connected via pipes to a deionized water tank and an ethyl acetate tank. The outlet of the extraction tank is connected via pipes to an organic phase tank. The outlet of the organic phase tank is connected via pipes to a drying tank. The inlet of the drying tank is connected via pipes to an anhydrous sodium sulfate tank. The outlet of the drying tank is connected via pipes to a vacuum distillation tank. The bottom outlet of the vacuum distillation tank is connected via pipes to a product tank. After the reaction solution enters the extraction tank, deionized water is added to allow N,N-dimethylformamide to enter the aqueous phase, while 2,4,4'-trichloro-2'-nitrodiphenyl ether dissolves in ethyl acetate and enters the organic phase. The organic phase is then dried and dehydrated before being subjected to vacuum distillation to finally obtain the 2,4,4'-trichloro-2'-nitrodiphenyl ether product. The process is simple, and the product yield and purity are high.

[0019] The bottom inlet of the reactor of this invention is connected to a nitrogen tank via a pipe. During the reaction, nitrogen is introduced into the reactor to create an inert protective atmosphere. Nitrogen effectively expels air from the reactor, preventing side reactions such as oxidation from contacting raw materials and target products with oxygen, improving reaction selectivity, and reducing impurity formation. Simultaneously, the introduction of nitrogen helps to stir and disperse the reactants, resulting in more uniform mixing of raw materials, promoting a more complete reaction, and increasing the reaction rate and product yield. Furthermore, for some oxygen-sensitive reaction conditions, nitrogen protection provides a more suitable and stable environment for the reaction, ensuring smooth reaction progress and guaranteeing product quality and production safety.

[0020] The top vapor outlet of the vacuum distillation vessel is connected to a first evaporator via a pipeline. The top vapor outlet of the first evaporator is connected to an ethyl acetate recovery tank via a pipeline, and the outlet of the ethyl acetate recovery tank is connected to the ethyl acetate tank via a pipeline. During vacuum distillation, ethyl acetate vaporizes and enters the first evaporator for further concentration, and is then collected in the ethyl acetate recovery tank. The recovered ethyl acetate can be recycled back to the ethyl acetate tank, significantly reducing the cost of using ethyl acetate and reducing solvent procurement costs. Simultaneously, it reduces ethyl acetate emissions, lowers environmental pollution, and aligns with the principles of green chemistry and sustainable development. Furthermore, a stable supply of ethyl acetate ensures the stability and consistency of the extraction process, contributing to improved product quality and production efficiency.

[0021] The outlet of the extraction tank is connected to an inorganic phase tank via a pipeline. The outlet of the inorganic phase tank is connected to a second evaporator via a pipeline. The top vapor phase outlet of the second evaporator is connected to an N,N-dimethylformamide recovery tank via a pipeline. After extraction, N,N-dimethylformamide dissolves in the aqueous phase. By introducing the inorganic phase into the second evaporator, the difference in boiling points between N,N-dimethylformamide and water is used for evaporation and separation. The vaporized N,N-dimethylformamide is collected in the N,N-dimethylformamide recovery tank. N,N-dimethylformamide is a relatively expensive organic solvent. Recycling and reusing it can significantly reduce production costs; reduce waste emissions of N,N-dimethylformamide, avoiding environmental pollution; and the recovered N,N-dimethylformamide can be reused in the reaction process, ensuring the stability of the quality and quantity of solvent in the reaction system, maintaining the continuity and stability of the reaction, and improving production efficiency.

[0022] The product tank's outlet is connected to a recrystallization tank via a pipeline. The recrystallization tank's inlet is connected to a first solvent tank via a pipeline. The recrystallization tank's outlet is connected to a centrifuge via a pipeline. The centrifuge's outlet is connected to a dryer via a pipeline. The dryer's outlet is connected to a pure product tank via a pipeline. The recrystallization tank, in conjunction with the first solvent tank, allows for the selection of a suitable solvent to recrystallize the product. Utilizing the difference in solubility between the target product and impurities at different temperatures, the target product crystallizes out, effectively removing residual impurities. The centrifuge quickly and efficiently separates the crystallized solid and liquid, improving separation efficiency. The dryer removes residual solvent from the solid surface, yielding a high-purity dried product that is stored in the pure product tank.

[0023] The centrifuge outlet is connected to a rinsing tank via a pipe, the rinsing tank inlet is connected to a second solvent tank via a pipe, and the rinsing tank outlet is connected to the dryer via a pipe. The product exiting the centrifuge may have a small amount of impurities and mother liquor adhering to its surface. Rinsing the product in the rinsing tank using the solvent provided by the second solvent tank effectively removes these residual impurities. The rinsed product then directly enters the dryer for drying, ensuring the continuity of the product processing flow and preventing secondary contamination during transfer. Furthermore, proper rinsing can reduce residual impurities on the product surface, improve the product's appearance and performance, further enhance product quality, and meet customers' high standards for product quality.

[0024] The liquid phase outlet of the centrifuge is connected to a third evaporator via a pipeline. The top vapor phase outlet of the third evaporator is connected to a solvent recovery tank via a pipeline. The outlet of the solvent recovery tank is connected to a second solvent tank via a pipeline. The liquid phase separated by the centrifuge contains the solvent used for rinsing and a small amount of dissolved impurities. It is introduced into the third evaporator for evaporation and concentration. After the solvent vaporizes, it is collected in the solvent recovery tank and then transported back to the second solvent tank for recycling. This process reduces solvent waste and lowers production costs. At the same time, it reduces the generation and discharge of waste liquid, alleviating environmental protection pressure. A stable solvent supply also ensures the continuous operation of rinsing, maintains the consistency of product cleaning effect, and helps to ensure the stability of product quality.

[0025] The outlet of the rinsing tank is connected to the third evaporator via a pipeline. This allows the liquid containing solvent and a small amount of impurities discharged from the rinsing tank to directly enter the third evaporator for treatment, further improving the solvent recovery and recycling system. This avoids the arbitrary discharge or additional treatment of rinsing wastewater, improving the efficiency and integrity of solvent recovery; it reduces processing steps, optimizes the process flow, and lowers energy consumption and costs during production; simultaneously, it ensures the environmental friendliness of the entire production process, meeting clean production requirements and contributing to the company's sustainable development.

[0026] The outlet of the 2,4-dichlorophenol tank is connected to a first purification tank via a pipeline. The inlet of the first purification tank is connected to a first ethanol tank via a pipeline. The outlet of the first purification tank is connected to a first filter via a pipeline. The solid phase outlet of the first filter is connected to a purified 2,4-dichlorophenol tank via a pipeline. The outlet of the purified 2,4-dichlorophenol tank is connected to the reaction vessel via a pipeline. The liquid phase outlet of the first filter is connected to a fourth evaporator via a pipeline. The top gas phase outlet of the fourth evaporator is connected to a first ethanol recovery tank via a pipeline. The outlet of the first ethanol recovery tank is connected to the first ethanol tank via a pipeline. The 2,4-dichlorophenol raw material undergoes pre-purification and ethanol recovery treatment. The purification of 2,4-dichlorophenol using ethanol supplied by the first ethanol tank in the first purification tank effectively removes impurities from the raw materials, improves the purity of the raw materials, and reduces side reactions caused by impurities during the reaction process, thereby increasing product yield and purity. The first filter achieves solid-liquid separation, obtaining purified 2,4-dichlorophenol for use in the reaction, ensuring the quality of the reaction raw materials. The ethanol in the liquid phase is recovered and reused through the fourth evaporator and the first ethanol recovery tank, reducing the cost of ethanol use and raw material procurement costs. At the same time, the entire process reduces the entry of impurities into the reaction system, improves the stability and controllability of the reaction, helps to produce high-quality products, and realizes the resource recycling of the raw material purification process, which is in line with the concept of green production.

[0027] The outlet of the 2-nitro-4-chlorophenol tank is connected to a second purification tank via a pipeline. The inlet of the second purification tank is connected to a second ethanol tank via a pipeline. The outlet of the second purification tank is connected to a second filter via a pipeline. The solid phase outlet of the second filter is connected to a purified 2-nitro-4-chlorophenol tank via a pipeline. The outlet of the purified 2-nitro-4-chlorophenol tank is connected to the reaction vessel via a pipeline. The liquid phase outlet of the second filter is connected to a fifth evaporator via a pipeline. The top gas phase outlet of the fifth evaporator is connected to a second ethanol recovery tank via a pipeline. The outlet of the second ethanol recovery tank is connected to the second ethanol tank via a pipeline. Deep purification and ethanol recovery are achieved for the 2-nitro-4-chlorophenol raw material. By combining the second purification tank and the second ethanol tank, impurities in 2-nitro-4-chlorophenol are effectively removed, improving the quality of the raw materials, providing high-quality reactants for subsequent reactions, reducing side reactions, and increasing product yield and purity. The purified raw materials are separated by the second filter and fed into the reactor, ensuring the purity of the reaction raw materials. Ethanol in the liquid phase is recovered and reused through the fifth evaporator and the second ethanol recovery tank, reducing production costs and minimizing resource waste. In addition, a stable supply of high-quality raw materials helps optimize reaction conditions, improve the stability of the production process and the consistency of product quality, enhance the product's competitiveness in the market, and simultaneously achieve green and sustainable production in the raw material processing stage. Attached Figure Description

[0028] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0029] Figure 1 This is a structural schematic diagram of an embodiment of the present utility model;

[0030] The tank consists of: 1. Reactor; 2. 2,4-Dichlorophenol tank; 3. 2-Nitro-4-chlorophenol tank; 4. Sodium hydroxide tank; 5. N,N-Dimethylformamide tank; 6. Extraction tank; 7. Deionized water tank; 8. Ethyl acetate tank; 9. Organic phase tank; 10. Drying tank; 11. Anhydrous sodium sulfate tank; 12. Vacuum distillation tank; 13. Product tank; 14. Nitrogen tank; 15. First evaporator; 16. Ethyl acetate recovery tank; 17. Inorganic phase tank; 18. Second evaporator; 19. N,N-Dimethylformamide recovery tank; 20. Recrystallization tank; 1. First solvent tank; 22. Centrifuge; 23. Dryer; 24. Pure product tank; 25. Washing tank; 26. Second solvent tank; 27. Third evaporator; 28. Solvent recovery tank; 29. ​​First purification tank; 30. First ethanol tank; 31. First filter; 32. Purified 2,4-dichlorophenol tank; 33. Fourth evaporator; 34. First ethanol recovery tank; 35. Second purification tank; 36. Second ethanol tank; 37. Second filter; 38. Purified 2-nitro-4-chlorophenol tank; 39. Fifth evaporator; 40. Second ethanol recovery tank. Detailed Implementation

[0031] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0032] like Figure 1As shown, an apparatus for preparing 2,4,4'-trichloro-2'-nitrodiphenyl ether includes a reaction vessel 1. The inlet of the reaction vessel 1 is connected via pipes to a 2,4-dichlorophenol tank 2, a 2-nitro-4-chlorophenol tank 3, a sodium hydroxide tank 4, and an N,N-dimethylformamide tank 5. The outlet of the reaction vessel 1 is connected via pipes to an extraction tank 6. The inlet of the extraction tank 6 is connected via pipes to a deionized water tank 7 and an ethyl acetate tank 8. The outlet of the extraction tank 6 is connected via pipes to an organic phase tank 9. The outlet of the organic phase tank 9 is connected via pipes to a drying tank 10. The inlet of the drying tank 10 is connected via pipes to an anhydrous sodium sulfate tank 11. The outlet of the drying tank 10 is connected via pipes to a vacuum distillation tank 12. The bottom outlet of the vacuum distillation tank 12 is connected via pipes to a product tank 13. After the reaction solution enters the extraction tank 6, deionized water is added to allow N,N-dimethylformamide to enter the aqueous phase, while 2,4,4'-trichloro-2'-nitrodiphenyl ether dissolves in ethyl acetate and enters the organic phase. The organic phase is then dried and dehydrated before being subjected to vacuum distillation to finally obtain the 2,4,4'-trichloro-2'-nitrodiphenyl ether product. The process is simple, and the product yield and purity are high.

[0033] The bottom inlet of the reactor 1 is connected to a nitrogen tank 14 via a pipe. During the reaction, nitrogen is introduced into the reactor 1 to create an inert protective atmosphere. Nitrogen effectively removes air from the reactor 1, preventing side reactions such as oxidation from contacting raw materials and target products with oxygen, improving reaction selectivity, and reducing impurity formation. Simultaneously, the introduction of nitrogen helps to stir and disperse the reactants, resulting in more uniform mixing of raw materials, promoting a more complete reaction, and increasing the reaction rate and product yield. Furthermore, for some oxygen-sensitive reaction conditions, nitrogen protection provides a more suitable and stable environment for the reaction, ensuring smooth reaction progress and guaranteeing product quality and production safety.

[0034] The top vapor outlet of the vacuum distillation tank 12 is connected to a first evaporator 15 via a pipeline. The top vapor outlet of the first evaporator 15 is connected to an ethyl acetate recovery tank 16 via a pipeline. The outlet of the ethyl acetate recovery tank 16 is connected to the ethyl acetate tank 8 via a pipeline. During vacuum distillation, ethyl acetate vaporizes and enters the first evaporator 15 for further concentration, and is then collected in the ethyl acetate recovery tank 16. The recovered ethyl acetate can be recycled back to the ethyl acetate tank 8, significantly reducing the cost of using ethyl acetate and reducing solvent procurement costs. Simultaneously, it reduces ethyl acetate emissions, lowers environmental pollution, and aligns with the principles of green chemistry and sustainable development. Furthermore, a stable supply of ethyl acetate ensures the stability and consistency of the extraction process, contributing to improved product quality and production efficiency.

[0035] The outlet of the extraction tank 6 is connected to the inorganic phase tank 17 via a pipeline. The outlet of the inorganic phase tank 17 is connected to the second evaporator 18 via a pipeline. The top gas phase outlet of the second evaporator 18 is connected to the N,N-dimethylformamide recovery tank 19 via a pipeline. After extraction, N,N-dimethylformamide dissolves in the aqueous phase. By introducing the inorganic phase into the second evaporator 18, the difference in boiling points between N,N-dimethylformamide and water is used for evaporation and separation. The vaporized N,N-dimethylformamide is collected in the N,N-dimethylformamide recovery tank 19. N,N-dimethylformamide is a relatively expensive organic solvent. Recycling and reusing it can significantly reduce production costs; reduce the waste discharge of N,N-dimethylformamide and avoid environmental pollution; and the recovered N,N-dimethylformamide can be reused in the reaction process, ensuring the stability of the quality and quantity of solvent in the reaction system, maintaining the continuity and stability of the reaction, and improving production efficiency.

[0036] The outlet of the product tank 13 is connected to a recrystallization tank 20 via a pipeline. The inlet of the recrystallization tank 20 is connected to a first solvent tank 21 via a pipeline. The outlet of the recrystallization tank 20 is connected to a centrifuge 22 via a pipeline. The outlet of the centrifuge 22 is connected to a dryer 23 via a pipeline. The outlet of the dryer 23 is connected to a pure product tank 24 via a pipeline. The recrystallization tank 20, in conjunction with the first solvent tank 21, allows for the selection of a suitable solvent to recrystallize the product. By utilizing the difference in solubility between the target product and impurities at different temperatures, the target product crystallizes out, thereby effectively removing residual small amounts of impurities. The centrifuge 22 can quickly and efficiently separate the crystallized solid and liquid, improving separation efficiency. The dryer 23 can remove residual solvent from the surface of the solid, obtaining a high-purity dried product, which is then stored in the pure product tank 24. In this embodiment, the first solvent tank 21 contains a mixed solvent of toluene and n-hexane in a volume ratio of 3:2.

[0037] The centrifuge 22 has its outlet connected to a rinsing tank 25 via a pipe. The rinsing tank 25 has its inlet connected to a second solvent tank 26 via a pipe. The rinsing tank 25 has its outlet connected to the dryer 23 via a pipe. The product exiting the centrifuge 22 may have a small amount of impurities and mother liquor adhering to its surface. The rinsing tank 25 uses the solvent provided by the second solvent tank 26 to rinse the product, effectively removing these residual impurities. The rinsed product directly enters the dryer 23 for drying, ensuring the continuity of the product processing flow and preventing secondary contamination during transfer. Furthermore, proper rinsing can reduce residual impurities on the product surface, improve the product's appearance and performance, further enhance product quality, and meet customers' high standards for product quality. In this embodiment, the second solvent tank 26 contains a low-temperature mixed solvent of toluene and n-hexane in a volume ratio of 3:2.

[0038] The liquid phase outlet of the centrifuge 22 is connected to a third evaporator 27 via a pipeline. The top vapor phase outlet of the third evaporator 27 is connected to a solvent recovery tank 28 via a pipeline. The outlet of the solvent recovery tank 28 is connected to a second solvent tank 26 via a pipeline. The liquid phase separated by the centrifuge 22 contains the solvent used for rinsing and a small amount of dissolved impurities. It is introduced into the third evaporator 27 for evaporation and concentration. After the solvent vaporizes, it is collected in the solvent recovery tank 28 and then transported back to the second solvent tank 26 for recycling. This process reduces solvent waste and lowers production costs. At the same time, it reduces the generation and discharge of waste liquid, alleviating the pressure on environmental protection. A stable solvent supply also ensures the continuous operation of rinsing, maintains the consistency of product cleaning effect, and helps to ensure the stability of product quality.

[0039] The outlet of the rinsing tank 25 is connected to the third evaporator 27 via a pipeline. This allows the liquid containing solvent and a small amount of impurities discharged from the rinsing tank 25 to directly enter the third evaporator 27 for treatment, further improving the solvent recovery and recycling system. This avoids the arbitrary discharge or additional treatment of rinsing wastewater, improving the efficiency and integrity of solvent recovery; it reduces processing steps, optimizes the process flow, and lowers energy consumption and costs during production; simultaneously, it ensures the environmental friendliness of the entire production process, meeting clean production requirements and contributing to the company's sustainable development.

[0040] The outlet of the 2,4-dichlorophenol tank 2 is connected to a first purification tank 29 via a pipeline. The inlet of the first purification tank 29 is connected to a first ethanol tank 30 via a pipeline. The outlet of the first purification tank 29 is connected to a first filter 31 via a pipeline. The solid phase outlet of the first filter 31 is connected to a purified 2,4-dichlorophenol tank 32 via a pipeline. The outlet of the purified 2,4-dichlorophenol tank 32 is connected to the reaction vessel 1 via a pipeline. The liquid phase outlet of the first filter 31 is connected to a fourth evaporator 33 via a pipeline. The top gas phase outlet of the fourth evaporator 33 is connected to a first ethanol recovery tank 34 via a pipeline. The outlet of the first ethanol recovery tank 34 is connected to the first ethanol tank 30 via a pipeline. The 2,4-dichlorophenol raw material has undergone pre-purification and ethanol recovery treatment. The purification of 2,4-dichlorophenol using ethanol supplied by the first ethanol tank 30 in the first purification tank 29 effectively removes impurities from the raw materials, improves the purity of the raw materials, and reduces side reactions caused by impurities in the raw materials during the reaction process, thereby increasing the product yield and purity. The first filter 31 achieves solid-liquid separation, and the purified 2,4-dichlorophenol is used in the reaction, ensuring the quality of the reaction raw materials. The ethanol in the liquid phase is recovered and reused through the fourth evaporator 33 and the first ethanol recovery tank 34, reducing the cost of using ethanol and reducing raw material procurement costs. At the same time, the entire process reduces the entry of impurities into the reaction system, improves the stability and controllability of the reaction, helps to produce high-quality products, and realizes the resource recycling of the raw material purification process, which is in line with the concept of green production.

[0041] The outlet of the 2-nitro-4-chlorophenol tank 3 is connected to a second purification tank 35 via a pipeline. The inlet of the second purification tank 35 is connected to a second ethanol tank 36 via a pipeline. The outlet of the second purification tank 35 is connected to a second filter 37 via a pipeline. The solid phase outlet of the second filter 37 is connected to a purified 2-nitro-4-chlorophenol tank 38 via a pipeline. The outlet of the purified 2-nitro-4-chlorophenol tank 38 is connected to the reaction vessel 1 via a pipeline. The liquid phase outlet of the second filter 37 is connected to a fifth evaporator 39 via a pipeline. The top gas phase outlet of the fifth evaporator 39 is connected to a second ethanol recovery tank 40 via a pipeline. The outlet of the second ethanol recovery tank 40 is connected to the second ethanol tank 36 via a pipeline. Deep purification and ethanol recovery are achieved for the 2-nitro-4-chlorophenol raw material. The second purification tank 35 and the second ethanol tank 36 work together to effectively remove impurities from 2-nitro-4-chlorophenol, improve the quality of raw materials, provide high-quality reactants for subsequent reactions, reduce side reactions, and improve product yield and purity. The second filter 37 separates the purified raw materials and sends them into the reaction vessel 1 to ensure the purity of the reaction raw materials. Ethanol in the liquid phase is recovered and reused through the fifth evaporator 39 and the second ethanol recovery tank 40, reducing production costs and minimizing resource waste. In addition, a stable supply of high-quality raw materials helps to optimize reaction conditions, improve the stability of the production process and the consistency of product quality, enhance the competitiveness of the product in the market, and realize green and sustainable production in the raw material processing stage.

[0042] It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the present invention. Furthermore, it should be understood that after reading the teachings of this invention, those skilled in the art can make various alterations or modifications to the invention, and these equivalent forms also fall within the scope defined by the appended claims.

Claims

1. An apparatus for the preparation of 2,4,4'-trichloro-2'-nitrodiphenyl ether comprising a reaction vessel, characterized in that: The inlet of the reactor is connected via pipes to a 2,4-dichlorophenol tank, a 2-nitro-4-chlorophenol tank, a sodium hydroxide tank, and an N,N-dimethylformamide tank. The outlet of the reactor is connected via pipes to an extraction tank. The inlet of the extraction tank is connected via pipes to a deionized water tank and an ethyl acetate tank. The outlet of the extraction tank is connected via pipes to an organic phase tank. The outlet of the organic phase tank is connected via pipes to a drying tank. The inlet of the drying tank is connected via pipes to an anhydrous sodium sulfate tank. The outlet of the drying tank is connected via pipes to a vacuum distillation tank. The bottom outlet of the vacuum distillation tank is connected via pipes to a product tank.

2. A device for the preparation of 2,4,4'-trichloro-2'-nitro-diphenyl ether according to claim 1, characterized in that: The bottom inlet of the reactor is connected to a nitrogen tank via a pipe.

3. A device for the preparation of 2,4,4'-trichloro-2'-nitro diphenyl ether according to claim 1, characterized in that: The top gas phase outlet of the vacuum distillation vessel is connected to a first evaporator via a pipeline, and the top gas phase outlet of the first evaporator is connected to an ethyl acetate recovery tank via a pipeline. The outlet of the ethyl acetate recovery tank is connected to the ethyl acetate tank via a pipeline.

4. The apparatus for preparing 2,4,4'-trichloro-2'-nitrodiphenyl ether as described in claim 1, characterized in that: The outlet of the extraction tank is connected to the inorganic phase tank via a pipeline, and the outlet of the inorganic phase tank is connected to the second evaporator via a pipeline. The top gas phase outlet of the second evaporator is connected to the N,N-dimethylformamide recovery tank via a pipeline.

5. A device for the preparation of 2,4,4'-trichloro-2'-nitro diphenyl ether according to claim 1, characterized in that: The product tank's outlet is connected to a recrystallization tank via a pipeline, the recrystallization tank's inlet is connected to a first solvent tank via a pipeline, the recrystallization tank's outlet is connected to a centrifuge via a pipeline, the centrifuge's outlet is connected to a dryer via a pipeline, and the dryer's outlet is connected to a pure product tank via a pipeline.

6. A device for the preparation of 2,4,4'-trichloro-2'-nitro-diphenyl ether according to claim 5, characterized in that: The centrifuge outlet is connected to a rinsing tank via a pipe, the rinsing tank inlet is connected to a second solvent tank via a pipe, and the rinsing tank outlet is connected to the dryer via a pipe.

7. A device for the preparation of 2,4,4'-trichloro-2'-nitro-diphenyl ether according to claim 6, characterized in that: The liquid phase outlet of the centrifuge is connected to a third evaporator via a pipe, and the top gas phase outlet of the third evaporator is connected to a solvent recovery tank via a pipe. The outlet of the solvent recovery tank is connected to a second solvent tank via a pipe.

8. A device for the preparation of 2,4,4'-trichloro-2'-nitro-diphenyl ether according to claim 7, characterized in that: The outlet of the rinsing tank is connected to the third evaporating tank via a pipe.

9. The apparatus for preparing 2,4,4'-trichloro-2'-nitrodiphenyl ether as described in claim 1, characterized in that: The outlet of the 2,4-dichlorophenol tank is connected to a first purification tank via a pipeline. The inlet of the first purification tank is connected to a first ethanol tank via a pipeline. The outlet of the first purification tank is connected to a first filter via a pipeline. The solid phase outlet of the first filter is connected to a purifying 2,4-dichlorophenol tank via a pipeline. The outlet of the purifying 2,4-dichlorophenol tank is connected to the reaction vessel via a pipeline. The liquid phase outlet of the first filter is connected to a fourth evaporator via a pipeline, and the top gas phase outlet of the fourth evaporator is connected to a first ethanol recovery tank via a pipeline. The outlet of the first ethanol recovery tank is connected to the first ethanol tank via a pipeline.

10. A plant for the preparation of 2,4,4'-trichloro-2'-nitro-diphenyl ether according to claim 1, characterized in that: The outlet of the 2-nitro-4-chlorophenol tank is connected to a second purification tank via a pipeline. The inlet of the second purification tank is connected to a second ethanol tank via a pipeline. The outlet of the second purification tank is connected to a second filter via a pipeline. The solid phase outlet of the second filter is connected to a purifying 2-nitro-4-chlorophenol tank via a pipeline. The outlet of the purifying 2-nitro-4-chlorophenol tank is connected to the reaction vessel via a pipeline. The liquid phase outlet of the second filter is connected to a fifth evaporator via a pipeline. The top gas phase outlet of the fifth evaporator is connected to a second ethanol recovery tank via a pipeline. The outlet of the second ethanol recovery tank is connected to the second ethanol tank via a pipeline.

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