A triclabendazole production apparatus

Abstract

This utility model discloses a triclocarban production apparatus, relating to the field of triclocarban production technology. The inlet of the reactor is connected via pipelines to a p-chloroaniline tank, a 3,4,4'-trichloroisocyanuric acid tank, a first solvent tank, and a catalyst tank. The outlet of the reactor is connected via pipelines to a filter. The liquid phase outlet of the filter is connected via pipelines to a precipitation tank. The inlet of the precipitation tank is connected via pipelines to a saturated sodium carbonate solution tank. The outlet of the precipitation tank is connected via pipelines to a first centrifuge. The solid phase outlet of the first centrifuge is connected via pipelines to a crude product tank. After the p-chloroaniline reacts with 3,4,4'-trichloroisocyanuric acid, the catalyst is removed. Then, under the action of the saturated sodium carbonate solution, triclocarban precipitates out. The first centrifuge separates the solid and liquid phases after precipitation, obtaining crude triclocarban, which is then transported to the crude product tank. The obtained product has high purity and is environmentally friendly.

Description

Technical Field

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

[0002] Triclocarban (TCC), an important antibacterial agent, is widely used in personal care products, detergents, and other fields. Currently, the production process for triclocarban mostly involves reacting 3,4-dichloroaniline and p-chlorophenyl isocyanate dissolved in toluene in a reactor for a period of time. The reaction product is then centrifuged, dried, and pulverized to obtain the triclocarban product. However, this process results in poor purity of the triclocarban product, affecting its quality. Furthermore, toluene has significant environmental and operator impacts. Summary of the Invention

[0003] The technical problem to be solved by this utility model is to provide a triclocarban production device that produces products with high purity, good quality, and environmental friendliness, addressing the shortcomings of existing technologies.

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

[0005] A triclocarban production apparatus includes a reaction vessel. The inlet of the reaction vessel is connected via pipelines to a p-chloroaniline tank, a 3,4,4'-trichloroisocyanuric acid tank, a first solvent tank, and a catalyst tank. The outlet of the reaction vessel is connected via pipelines to a filter. The liquid phase outlet of the filter is connected via pipelines to a precipitation tank. The inlet of the precipitation tank is connected via pipelines to a saturated sodium carbonate solution tank. The outlet of the precipitation tank is connected via pipelines to a first centrifuge. The solid phase outlet of the first centrifuge is connected via pipelines to a crude product tank.

[0006] As an improved technical solution, a nitrogen tank is provided at the bottom inlet of the reactor.

[0007] As an improved technical solution, the precipitation tank is equipped with an online pH sensor, and the outlet of the saturated sodium carbonate solution tank is equipped with a shut-off valve. The online pH sensor and the shut-off valve are interlocked to the control system.

[0008] As an improved technical solution, the outlet of the crude product tank is connected to a recrystallization tank via a pipeline, the inlet of the recrystallization tank is connected to a second solvent tank via a pipeline, the outlet of the recrystallization tank is connected to a second centrifuge via a pipeline, the solid phase outlet of the second centrifuge is connected to a first dryer via a pipeline, and the outlet of the first dryer is connected to a finished product tank via a pipeline.

[0009] As an improved technical solution, the liquid phase outlet of the second centrifuge is connected to the first evaporator via a pipeline, the top gas phase outlet of the first evaporator is connected to the first recovery tank via a pipeline, and the outlet of the first recovery tank is connected to the second solvent tank via a pipeline.

[0010] As an improved technical solution, the liquid phase outlet of the first centrifuge is connected to a second evaporator via a pipeline, the top gas phase outlet of the second evaporator is connected to a second recovery tank via a pipeline, and the outlet of the second recovery tank is connected to the first solvent tank via a pipeline.

[0011] As a preferred technical solution, the solid phase outlet of the filter is connected to a catalyst recovery tank via a pipeline, the outlet of the catalyst recovery tank is connected to a washing tank via a pipeline, the inlet of the washing tank is connected to a deionized water tank via a pipeline, the outlet of the washing tank is connected to a second dryer via a pipeline, and the outlet of the second dryer is connected to the catalyst tank via a pipeline.

[0012] As a preferred technical solution, the inlet of the washing tank is connected to an ethanol tank via a pipeline.

[0013] Due to the adoption of the above technical solution, the beneficial effects of this utility model are:

[0014] This invention relates to a triclocarban production apparatus, comprising a reaction vessel. The inlet of the reaction vessel is connected via pipelines to a p-chloroaniline tank, a 3,4,4'-trichloroisocyanuric acid tank, a first solvent tank, and a catalyst tank. The outlet of the reaction vessel is connected via a filter via a pipeline. The liquid phase outlet of the filter is connected via a pipeline to a precipitation tank. The inlet of the precipitation tank is connected via a pipeline to a saturated sodium carbonate solution tank. The outlet of the precipitation tank is connected via a pipeline to a first centrifuge. The solid phase outlet of the first centrifuge is connected via a pipeline to a crude product tank. After the p-chloroaniline reacts with 3,4,4'-trichloroisocyanuric acid, the catalyst is removed. Then, under the action of the saturated sodium carbonate solution, triclocarban precipitates out. The first centrifuge separates the solid and liquid phases after precipitation, obtaining crude triclocarban, which is then transported to the crude product tank. The obtained product has high purity and is environmentally friendly.

[0015] The reactor of this invention is equipped with a nitrogen tank at the bottom inlet. This forms a protective gas layer at the bottom of the reaction system, more effectively expelling air from the reactor and preventing the oxidation of raw materials such as p-chloroaniline, as well as intermediate and final products such as triclocarban generated during the reaction. This ensures that the reaction proceeds smoothly in an oxygen-free environment, thereby improving the purity and yield of the product.

[0016] The precipitation tank is equipped with an online pH sensor, and the outlet of the saturated sodium carbonate solution tank is equipped with a shut-off valve. The online pH sensor and the shut-off valve are interlocked to the control system. The online pH sensor monitors the pH value of the solution in the precipitation tank in real time and feeds the data back to the control system. When the pH value reaches 8-9, the control system automatically closes the shut-off valve of the saturated sodium carbonate solution tank, stopping the addition of saturated sodium carbonate solution. This automated control method can precisely control the pH value of the solution, ensuring that triclocarban precipitates completely, avoiding the precipitation effect caused by adding too much or too little sodium carbonate solution, improving the product yield and quality stability, while reducing manual monitoring and operation, and lowering labor intensity.

[0017] The outlet of the crude product tank is connected to a recrystallization tank via a pipeline. The inlet of the recrystallization tank is connected to a second solvent tank via a pipeline. The outlet of the recrystallization tank is connected to a second centrifuge via a pipeline. The solid phase outlet of the second centrifuge is connected to a first dryer via a pipeline. The outlet of the first dryer is connected to a finished product tank via a pipeline. The crude product is transported from the crude product tank to the recrystallization tank and mixed with the second solvent for recrystallization, which further removes impurities from the crude product and improves product purity. Through the sequential processing of the second centrifuge, the first dryer, and other equipment, continuous production of solid-liquid separation and solid drying after recrystallization is achieved, ensuring that the final triclocarban product has high quality and stability. The entire process is highly automated, improving production efficiency.

[0018] The liquid phase outlet of the second centrifuge is connected to the first evaporator via a pipeline. The top vapor phase outlet of the first evaporator is connected to the first recovery tank via a pipeline. The outlet of the first recovery tank is connected to the second solvent tank via a pipeline. The liquid phase separated by the second centrifuge contains incompletely dissolved triclocarban and a second solvent. The solvent is evaporated in the first evaporator, and the vaporized solvent is condensed and recovered in the first recovery tank before being transported to the second solvent tank for reuse. This design achieves solvent recycling, reduces production costs, minimizes solvent waste and environmental pollution, and aligns with the principles of green chemistry and sustainable development.

[0019] The liquid phase outlet of the first centrifuge is connected to a second evaporator via a pipeline. The top vapor phase outlet of the second evaporator is connected to a second recovery tank via a pipeline. The outlet of the second recovery tank is connected to the first solvent tank via a pipeline. The first solvent in the liquid phase separated by the first centrifuge is evaporated in the second evaporator, recovered in the second recovery tank, and then returned to the first solvent tank for recycling. This not only saves production costs but also reduces waste liquid discharge and improves the resource utilization rate and environmental benefits of the entire production process.

[0020] The solid phase outlet of the filter is connected to a catalyst recovery tank via a pipeline. The outlet of the catalyst recovery tank is connected to a washing tank via a pipeline. The inlet of the washing tank is connected to a deionized water tank via a pipeline. The outlet of the washing tank is connected to a second dryer via a pipeline. The outlet of the second dryer is connected to the catalyst tank via a pipeline. The solid catalyst separated by the filter sequentially enters the catalyst recovery tank, washing tank, and second dryer via pipelines, and finally returns to the catalyst tank. This process realizes automated catalyst recovery and treatment. Impurities on the catalyst surface are removed by washing with deionized water, and the catalyst activity is restored by drying, allowing the catalyst to be reused, reducing production costs, and minimizing the environmental impact of catalyst waste, demonstrating the advantages of green production.

[0021] The inlet of the washing tank is connected to an ethanol tank via a pipe. In addition to deionized water, ethanol can also be used to wash the catalyst. Ethanol can more effectively dissolve residual organic impurities on the catalyst surface, further improving the cleanliness and activity of the catalyst, ensuring that the catalyst maintains a good catalytic effect during repeated use, thereby improving the production efficiency and product quality of triclocarban. Attached Figure Description

[0022] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0023] Figure 1 This is a structural schematic diagram of an embodiment of the present utility model;

[0024] The components include: 1. Reactor; 2. p-Chloroaniline tank; 3. 3,4,4'-Trichloroisocyanuric acid tank; 4. First solvent tank; 5. Catalyst tank; 6. Filter; 7. Precipitation tank; 8. Saturated sodium carbonate solution tank; 9. First centrifuge; 10. Crude product tank; 11. Nitrogen tank; 12. Online pH sensor; 13. Shut-off valve; 14. Recrystallization tank; 15. Second solvent tank; 16. Second centrifuge; 17. First dryer; 18. Finished product tank; 19. First evaporator; 20. First recovery tank; 21. Second evaporator; 22. Second recovery tank; 23. Catalyst recovery tank; 24. Washing tank; 25. Deionized water tank; 26. Second dryer; 27. Ethanol tank; 28. Crushing tank. Detailed Implementation

[0025] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0026] like Figure 1As shown, a triclocarban production apparatus includes a reaction vessel 1. The inlet of the reaction vessel 1 is connected via pipelines to a p-chloroaniline tank 2, a 3,4,4'-trichloroisocyanuric acid tank 3, a first solvent tank 4, and a catalyst tank 5. The outlet of the reaction vessel 1 is connected via a filter 6. The liquid phase outlet of the filter 6 is connected via a pipeline to a precipitation tank 7. The inlet of the precipitation tank 7 is connected via a pipeline to a saturated sodium carbonate solution tank 8. The outlet of the precipitation tank 7 is connected via a pipeline to a first centrifuge 9. The solid phase outlet of the first centrifuge 9 is connected via a pipeline to a crude product tank 10. After the p-chloroaniline reacts with 3,4,4'-trichloroisocyanuric acid, the catalyst is removed. Then, under the action of the saturated sodium carbonate solution, triclocarban precipitates out. The first centrifuge 9 separates the solid and liquid phases after precipitation to obtain crude triclocarban, which is then transported to the crude product tank 10. The obtained product has high purity and is environmentally friendly. In this embodiment, the first solvent tank 4 contains an ethanol-water mixed solvent. Ethanol dissolves p-chloroaniline, while water promotes the ionization of 3,4,4'-trichloroisocyanuric acid (Cl+ release). Simultaneously, adjusting the polarity may benefit intermediate stability. Furthermore, compared to toluene, it is more environmentally friendly and offers higher operational safety. The catalyst in this embodiment is a chitosan composite catalyst supported on nano-titanium dioxide. This catalyst is prepared by uniformly loading nano-titanium dioxide onto chitosan. The preparation method is as follows: chitosan is dissolved in an acetic acid solution, nano-titanium dioxide powder is added, and after thorough stirring, it is obtained by freeze-drying.

[0027] The outlets of p-chloroaniline tank 2 and 3,4,4'-trichloroisocyanuric acid tank 3 are respectively connected to crushing tanks 28, which improves reaction efficiency and product quality by crushing the raw materials.

[0028] The bottom inlet of the reactor 1 is equipped with a nitrogen tank 11. This can form a protective gas layer at the bottom of the reaction system, more effectively expelling air from the reactor 1 and preventing the oxidation of raw materials such as p-chloroaniline, as well as intermediate and final products such as triclocarban generated during the reaction. This ensures that the reaction proceeds smoothly in an oxygen-free environment, thereby improving the purity and yield of the product.

[0029] The precipitation tank 7 is equipped with an online pH sensor 12, and the outlet of the saturated sodium carbonate solution tank 8 is equipped with a shut-off valve 13. The online pH sensor 12 and the shut-off valve 13 are interlocked to the control system. The online pH sensor 12 monitors the pH value of the solution in the precipitation tank 7 in real time and feeds the data back to the control system. When the pH value reaches 8-9, the control system automatically closes the shut-off valve 13 of the saturated sodium carbonate solution tank 8, stopping the addition of saturated sodium carbonate solution. This automated control method can accurately control the pH value of the solution, ensuring that triclocarban is fully precipitated and avoiding the precipitation effect caused by adding too much or too little sodium carbonate solution, thus improving the product yield and quality stability, while reducing manual monitoring and operation, and lowering labor intensity.

[0030] The outlet of the crude product tank 10 is connected to a recrystallization tank 14 via a pipeline. The inlet of the recrystallization tank 14 is connected to a second solvent tank 15 via a pipeline. The outlet of the recrystallization tank 14 is connected to a second centrifuge 16 via a pipeline. The solid phase outlet of the second centrifuge 16 is connected to a first dryer 17 via a pipeline. The outlet of the first dryer 17 is connected to a finished product tank 18 via a pipeline. The crude product is transported from the crude product tank 10 to the recrystallization tank 14, where it is mixed with the second solvent for recrystallization. This further removes impurities from the crude product and improves its purity. Through the sequential processing of the second centrifuge 16, the first dryer 17, and other equipment, continuous production of solid-liquid separation and solid drying after recrystallization is achieved, ensuring that the final triclocarban product has high quality and stability. Furthermore, the entire process is highly automated, improving production efficiency. In this embodiment, the second solvent tank 15 contains a methanol-water mixed solvent, which is environmentally friendly, making the triclocarban refining and purification process more efficient, green, and economical.

[0031] The liquid phase outlet of the second centrifuge 16 is connected to the first evaporator 19 via a pipeline. The top vapor phase outlet of the first evaporator 19 is connected to the first recovery tank 20 via a pipeline. The outlet of the first recovery tank 20 is connected to the second solvent tank 15 via a pipeline. The liquid phase separated by the second centrifuge 16 contains incompletely dissolved triclocarban and a second solvent. The solvent is evaporated in the first evaporator 19, and the vapor phase solvent is condensed and recovered in the first recovery tank 20, and then transported to the second solvent tank 15 for reuse. This design realizes the recycling of solvents, reduces production costs, reduces solvent waste and environmental pollution, and conforms to the concepts of green chemistry and sustainable development.

[0032] The liquid phase outlet of the first centrifuge 9 is connected to a second evaporator 21 via a pipeline. The top gas phase outlet of the second evaporator 21 is connected to a second recovery tank 22 via a pipeline. The outlet of the second recovery tank 22 is connected to the first solvent tank 4 via a pipeline. The first solvent in the liquid phase separated by the first centrifuge 9 is evaporated by the second evaporator 21, recovered by the second recovery tank 22, and then returned to the first solvent tank 4 for recycling. This not only saves production costs but also reduces waste liquid discharge and improves the resource utilization rate and environmental benefits of the entire production process.

[0033] The solid phase outlet of filter 6 is connected to catalyst recovery tank 23 via a pipeline. The outlet of catalyst recovery tank 23 is connected to washing tank 24 via a pipeline. The inlet of washing tank 24 is connected to deionized water tank 25 via a pipeline. The outlet of washing tank 24 is connected to second dryer 26 via a pipeline. The outlet of second dryer 26 is connected to catalyst tank 5 via a pipeline. The solid catalyst separated by filter 6 enters catalyst recovery tank 23, washing tank 24, and second dryer 26 sequentially via pipelines, and finally returns to catalyst tank 5. This process realizes automated catalyst recovery and treatment. Impurities on the catalyst surface are removed by washing with deionized water, and the catalyst activity is restored by drying, enabling the catalyst to be reused, reducing production costs, and minimizing the environmental impact of catalyst waste, demonstrating the advantages of green production.

[0034] The inlet of the washing tank 24 is connected to an ethanol tank 27 via a pipe. In addition to deionized water, ethanol can also be used to wash the catalyst. Ethanol can more effectively dissolve residual organic impurities on the catalyst surface, further improving the cleanliness and activity of the catalyst, ensuring that the catalyst maintains a good catalytic effect during repeated use, thereby improving the production efficiency and product quality of triclocarban.

[0035] 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. A triclocarban production apparatus, comprising a reaction vessel, characterized in that: The inlet of the reactor is connected via pipes to a p-chloroaniline tank, a 3,4,4'-trichloroisocyanuric acid tank, a first solvent tank, and a catalyst tank. The outlet of the reactor is connected via pipes to a filter. The liquid phase outlet of the filter is connected via pipes to a precipitation tank. The inlet of the precipitation tank is connected via pipes to a saturated sodium carbonate solution tank. The outlet of the precipitation tank is connected via pipes to a first centrifuge. The solid phase outlet of the first centrifuge is connected via pipes to a crude product tank.

2. The triclocarban production apparatus as described in claim 1, characterized in that: The bottom inlet of the reactor is equipped with a nitrogen tank.

3. The triclocarban production apparatus as described in claim 1, characterized in that: The precipitation tank is equipped with an online pH sensor, and the outlet of the saturated sodium carbonate solution tank is equipped with a shut-off valve. The online pH sensor and the shut-off valve are interlocked to the control system.

4. A triclocarban production apparatus as described in claim 1, characterized in that: The outlet of the crude product tank is connected to a recrystallization tank via a pipeline. The inlet of the recrystallization tank is connected to a second solvent tank via a pipeline. The outlet of the recrystallization tank is connected to a second centrifuge via a pipeline. The solid phase outlet of the second centrifuge is connected to a first dryer via a pipeline. The outlet of the first dryer is connected to a finished product tank via a pipeline.

5. A triclocarban production apparatus as described in claim 4, characterized in that: The liquid phase outlet of the second centrifuge is connected to the first evaporator via a pipeline, the top gas phase outlet of the first evaporator is connected to the first recovery tank via a pipeline, and the outlet of the first recovery tank is connected to the second solvent tank via a pipeline.

6. A triclocarban production apparatus as described in claim 1, characterized in that: The liquid phase outlet of the first centrifuge is connected to a second evaporator via a pipeline, the top gas phase outlet of the second evaporator is connected to a second recovery tank via a pipeline, and the outlet of the second recovery tank is connected to the first solvent tank via a pipeline.

7. A triclocarban production apparatus as described in claim 1, characterized in that: The solid phase outlet of the filter is connected to a catalyst recovery tank via a pipeline. The outlet of the catalyst recovery tank is connected to a washing tank via a pipeline. The inlet of the washing tank is connected to a deionized water tank via a pipeline. The outlet of the washing tank is connected to a second dryer via a pipeline. The outlet of the second dryer is connected to the catalyst tank via a pipeline.

8. A triclocarban production apparatus as described in claim 7, characterized in that: The inlet of the washing tank is connected to an ethanol tank via a pipe.

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