A device for preparing triclosan

Abstract

The utility model discloses a triclosan preparation device relates to triclosan production technical field, including first reactor, the inlet of first reactor is respectively through pipeline intercommunication with 2,4 - dichlorophenol jar, sodium hydroxide solution jar, xylene jar I and tetrabutyl ammonium bromide jar, the outlet of first reactor is through pipeline intercommunication with second reactor, the inlet of second reactor is respectively through pipeline intercommunication with 2 - chloro - 5 - nitrobenzene methyl ether jar, dilute hydrochloric acid solution jar, ZnCl2 - Al2O3 solid acid jar, nano TiO2 jar and xylene jar II, the outlet of second reactor is through pipeline intercommunication with third reactor, the inlet of third reactor is through pipeline intercommunication with acetic acid jar, the top gas phase export of third reactor is through pipeline intercommunication with first condenser, and the outlet of first condenser is through pipeline intercommunication with crude product jar, improves the yield of product.

Description

Technical Field

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

[0002] Triclosan is a broad-spectrum antibacterial agent widely used in high-efficiency medicated soaps / hygienic soaps, sanitary washes, deodorant / athlete's foot sprays, disinfectant hand sanitizers, wound disinfectant sprays, medical device disinfectants, hygienic facial cleansers / creams, air fresheners, and refrigerator deodorizers. It is also used in the finishing of sanitary textiles and the preservation and treatment of plastics. Higher purity triclosan is also widely used in toothpastes and mouthwashes for the treatment of gingivitis, periodontitis, and oral ulcers.

[0003] Chinese patent CN221359872U discloses a production device for crude triclosan etherification. By dissolving 2,4-dichlorophenol in a solvent, it eliminates the difficulty of manual powder feeding and saves labor. However, it cannot solve the problem of low reaction yield and results in waste of raw materials. Summary of the Invention

[0004] The technical problem to be solved by this utility model is to provide a triclosan preparation device that addresses the shortcomings of existing technologies, resulting in high product yield and improved raw material utilization.

[0005] To solve the above-mentioned technical problems, the technical solution of this utility model is as follows:

[0006] A triclosan preparation apparatus includes a first reactor, the inlet of which is connected via pipes to a 2,4-dichlorophenol tank, a sodium hydroxide solution tank, a xylene tank I, and a tetrabutylammonium bromide tank; the outlet of the first reactor is connected via pipes to a second reactor, the inlet of which is connected via pipes to a 2-chloro-5-nitrobenzene ether tank, a dilute hydrochloric acid solution tank, a ZnCl2-Al2O3 solid acid tank, a nano-TiO2 tank, and a xylene tank II; and the outlet of the second reactor is connected via pipes to a third reactor, the inlet of which is connected via pipes to an acetic acid tank.

[0007] The top gas phase outlet of the third reactor is connected to the first condenser via a pipeline, and the outlet of the first condenser is connected to the crude product tank via a pipeline.

[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 an ethanol tank via a pipeline, the outlet of the recrystallization tank is connected to a centrifuge via a pipeline, and the solid phase outlet of the centrifuge is connected to a finished product tank.

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

[0010] As an improved technical solution, the gas phase outlet of the third reactor is connected to a heat exchanger via a pipeline, and the material outlet of the heat exchanger is connected to the first condenser via a pipeline.

[0011] The jacket inlet and outlet of the heat exchanger are respectively connected to the jacket inlet and outlet of the first reactor via pipelines.

[0012] As an improved technical solution, the outlet of the first condenser is connected to a third condenser via a pipe, the outlet of the third condenser is connected to an evaporator via a pipe, the top vapor outlet of the evaporator is connected to a fourth condenser via a pipe, and the outlet of the fourth condenser is connected to a solvent recovery tank via a pipe.

[0013] As an improved technical solution, the outlet of the solvent recovery tank is connected to xylene tank I and xylene tank II via pipelines.

[0014] As a preferred technical solution, the outlet of the third condenser is connected to an alkaline washing tower via a pipeline. The alkaline washing tower is equipped with a circulation pump, and the top of the alkaline washing tower is equipped with a gas exhaust port.

[0015] As a preferred technical solution, the first reactor is a vertical stirred reactor, the second reactor is a horizontal multi-chamber reactor, and the third reactor is a packed tower reactor.

[0016] Due to the adoption of the above technical solution, the beneficial effects of this utility model are:

[0017] This invention discloses a triclosan preparation apparatus, comprising a first reactor. The inlet of the first reactor is connected via pipes to a 2,4-dichlorophenol tank, a sodium hydroxide solution tank, a xylene tank I, and a tetrabutylammonium bromide tank. The outlet of the first reactor is connected via pipes to a second reactor. The inlet of the second reactor is connected via pipes to a 2-chloro-5-nitrobenzene ether tank, a dilute hydrochloric acid solution tank, a ZnCl2-Al2O3 solid acid tank, a nano-TiO2 tank, and a xylene tank II. The outlet of the second reactor is connected via pipes to a third reactor, the inlet of which is connected via pipes to an acetic acid tank. The top gas phase outlet of the third reactor is connected via pipes to a first condenser, and the outlet of the first condenser is connected via pipes to a crude product tank. Sodium hydroxide solution is added to the first reactor to maintain its pH at 11-12. Then, tetrabutylammonium bromide is added as a phase transfer catalyst to convert 2,4-dichlorophenol into phenol oxide anions, improving the utilization rate of raw materials for subsequent condensation reactions, reducing unreacted phenol residues, and significantly increasing the yield of subsequent products. The synergistic effect of solid acid catalyst (ZnCl2-Al2O3) and nano-TiO2 co-catalyst improves the selectivity of the condensation reaction, greatly reduces by-products, significantly increases the conversion rate of the raw material 2-chloro-5-nitrobenzyl ether, and promotes the isomerization of the product into highly active β-triclosan by acetic acid, further improving the yield.

[0018] The crude product tank of this invention has its outlet connected to a recrystallization tank via a pipeline, the inlet of the recrystallization tank connected to an ethanol tank via a pipeline, and the outlet of the recrystallization tank connected to a centrifuge via a pipeline. The solid phase outlet of the centrifuge is connected to a finished product tank. Ethanol recrystallization further purifies the product, removing trace isomers and solvent residues, resulting in a finished product purity >99.5%. Furthermore, the mother liquor can be recycled, increasing the overall utilization rate of raw materials by 12%.

[0019] The liquid phase outlet of the centrifuge is connected to a distillation tank via a pipeline. The top gas phase outlet of the distillation tank is connected to a second condenser via a pipeline. The outlet of the second condenser is connected to an ethanol recovery tank via a pipeline. The outlet of the ethanol recovery tank is connected to the ethanol tank via a pipeline. The ethanol recovery rate is >95%, and it is recycled for the recrystallization process, reducing the consumption of fresh solvent and significantly reducing production costs.

[0020] The gas phase outlet of the third reactor is connected to a heat exchanger via a pipeline, and the material outlet of the heat exchanger is connected to the first condenser via a pipeline. The jacket inlet and outlet of the heat exchanger are respectively connected to the jacket inlet and outlet of the first reactor via pipelines. This cascaded utilization of thermal energy reduces steam consumption by 30%, while stabilizing the initial temperature of the first reactor (80±2℃), ensuring consistent reaction rates and minimal yield fluctuations.

[0021] The outlet of the first condenser is connected to a third condenser via a pipeline. The outlet of the third condenser is connected to an evaporator via a pipeline. The top vapor outlet of the evaporator is connected to a fourth condenser via a pipeline. The outlet of the fourth condenser is connected to a solvent recovery tank via a pipeline. The outlet of the solvent recovery tank is connected to xylene tank I and xylene tank II via pipelines, respectively. Deep xylene recovery (recovery rate > 97%) reduces VOC emissions, while solvent reuse improves the accuracy of raw material dosing, and the reaction molar ratio control error is < 0.5%.

[0022] The outlet of the third condenser is connected to an alkaline scrubbing tower via a pipeline. The alkaline scrubbing tower is equipped with a circulation pump, and a gas exhaust port is located at the top of the tower. This effectively absorbs acidic gases such as HCl, protecting the environment while recovering sodium chloride as a byproduct, thus improving the utilization rate of the raw material chlorine.

[0023] The first reactor is a vertical stirred tank reactor, the second reactor is a horizontal multi-chamber reactor, and the third reactor is a packed tower reactor. By matching the reaction characteristics of each stage, the overall reaction time is shortened, the production capacity is increased, and the optimized interstage mass transfer efficiency greatly improves the overall yield. Attached Figure Description

[0024] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0025] Figure 1 This is a structural schematic diagram of an embodiment of the present utility model;

[0026] The reactor is composed of: 1. First reactor; 2. 2,4-Dichlorophenol tank; 3. Sodium hydroxide solution tank; 4. Xylene tank I; 5. Tetrabutylammonium bromide tank; 6. Second reactor; 7. 2-Chloro-5-nitrobenzene ether tank; 8. Dilute hydrochloric acid solution tank; 9. ZnCl2-Al2O3 solid acid tank; 10. Nano-TiO2 tank; 11. Xylene tank II; 12. Third reactor; 13. Acetic acid tank; 14. First condenser; 15. Crude product tank; 16. Recrystallization tank; 17. Ethanol tank; 18. Centrifuge; 19. Finished product tank; 20. Distillation tank; 21. Second condenser; 22. Ethanol recovery tank; 23. Heat exchanger; 24. Third condenser; 25. Evaporator; 26. Fourth condenser; 27. Solvent recovery tank; 28. Alkali washing tower; 29. ​​Circulation pump; 30. Gas outlet. Detailed Implementation

[0027] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0028] like Figure 1As shown, a triclosan preparation apparatus includes a first reactor 1. The inlet of the first reactor 1 is connected via pipes to a 2,4-dichlorophenol tank 2, a sodium hydroxide solution tank 3, a xylene tank I 4, and a tetrabutylammonium bromide tank 5. The outlet of the first reactor 1 is connected via pipes to a second reactor 6. The inlet of the second reactor 6 is connected via pipes to a 2-chloro-5-nitrobenzene ether tank 7, a dilute hydrochloric acid solution tank 8, a ZnCl2-Al2O3 solid acid tank 9, a nano-TiO2 tank 10, and a xylene tank II 11. The outlet of the second reactor 6 is connected via pipes to a third reactor 12. The inlet of the third reactor 12 is connected via pipes to an acetic acid tank 13. The top gas phase outlet of the third reactor 12 is connected via pipes to a first condenser 14. The outlet of the first condenser 14 is connected via pipes to a crude product tank 15. Sodium hydroxide solution was added to reactor 1 to maintain its pH at 11-12. Then, tetrabutylammonium bromide was added as a phase-transfer catalyst to convert 2,4-dichlorophenol into phenoxy anions, improving the utilization rate of raw materials in subsequent condensation reactions, reducing unreacted phenol residues, and significantly increasing the yield of subsequent products. Furthermore, the synergistic effect of a solid acid catalyst (ZnCl2-Al2O3) and a nano-TiO2 co-catalyst improved the selectivity of the condensation reaction, significantly reduced byproducts, greatly increased the conversion rate of the raw material 2-chloro-5-nitrobenzene, and acetic acid promoted the isomerization of the product to highly active β-triclosan, further improving the yield.

[0029] The outlet of the crude product tank 15 is connected to a recrystallization tank 16 via a pipeline. The inlet of the recrystallization tank 16 is connected to an ethanol tank 17 via a pipeline. The outlet of the recrystallization tank 16 is connected to a centrifuge 18 via a pipeline. The solid phase outlet of the centrifuge 18 is connected to a finished product tank 19. Ethanol recrystallization further purifies the product, removing trace isomers and solvent residues. The purity of the finished product is >99.5%, and the mother liquor can be recycled, increasing the overall utilization rate of raw materials by 12%.

[0030] The liquid phase outlet of the centrifuge 18 is connected to a distillation tank 20 via a pipeline. The top gas phase outlet of the distillation tank 20 is connected to a second condenser 21 via a pipeline. The outlet of the second condenser 21 is connected to an ethanol recovery tank 22 via a pipeline. The outlet of the ethanol recovery tank 22 is connected to the ethanol tank 17 via a pipeline. The ethanol recovery rate is >95%, and it is recycled for the recrystallization process, reducing the consumption of fresh solvent and significantly reducing production costs.

[0031] The gas phase outlet of the third reactor 12 is connected to a heat exchanger 23 via a pipeline, and the material outlet of the heat exchanger 23 is connected to the first condenser 14 via a pipeline. The jacket inlet and outlet of the heat exchanger 23 are respectively connected to the jacket inlet and outlet of the first reactor 1 via pipelines. The cascade utilization of thermal energy reduces steam consumption by 30%, while stabilizing the initial temperature of the first reactor 1 (80±2℃), ensuring consistent reaction rate and small yield fluctuations.

[0032] The outlet of the first condenser 14 is connected to a third condenser 24 via a pipeline. The outlet of the third condenser 24 is connected to an evaporator 25 via a pipeline. The top vapor outlet of the evaporator 25 is connected to a fourth condenser 26 via a pipeline. The outlet of the fourth condenser 26 is connected to a solvent recovery tank 27 via a pipeline. The outlet of the solvent recovery tank 27 is connected to xylene tank I4 and xylene tank II11 via pipelines, respectively. Deep xylene recovery (recovery rate > 97%) reduces VOC emissions, while solvent reuse improves the accuracy of raw material feeding, and the reaction molar ratio control error is < 0.5%.

[0033] The outlet of the third condenser 24 is connected to an alkaline washing tower 28 via a pipeline. The alkaline washing tower 28 is equipped with a circulation pump 29, and a gas exhaust port 30 is located at the top of the alkaline washing tower 28. This effectively absorbs acidic gases such as HCl, protecting the environment while recovering sodium chloride byproducts, thus improving the utilization rate of the raw material chlorine.

[0034] The first reactor 1 is a vertical stirred tank reactor, the second reactor 6 is a horizontal multi-chamber reactor, and the third reactor 12 is a packed tower reactor. By matching the reaction characteristics of each stage, the overall reaction time is shortened, the production capacity is increased, and the optimized interstage mass transfer efficiency greatly improves the overall yield.

[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 device for the preparation of triclosan, characterized by: The reactor includes a first reactor, whose inlet is connected via pipes to a 2,4-dichlorophenol tank, a sodium hydroxide solution tank, a xylene tank I, and a tetrabutylammonium bromide tank. The outlet of the first reactor is connected via pipes to a second reactor, whose inlet is connected via pipes to a 2-chloro-5-nitrobenzene ether tank, a dilute hydrochloric acid solution tank, a ZnCl2-Al2O3 solid acid tank, a nano-TiO2 tank, and a xylene tank II. The outlet of the second reactor is connected via pipes to a third reactor, whose inlet is connected via pipes to an acetic acid tank. The top gas phase outlet of the third reactor is connected to the first condenser via a pipeline, and the outlet of the first condenser is connected to the crude product tank via a pipeline.

2. A device for the preparation of triclosan according to 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 an ethanol tank via a pipeline, the outlet of the recrystallization tank is connected to a centrifuge via a pipeline, and the solid phase outlet of the centrifuge is connected to a finished product tank.

3. A device for the preparation of triclosan as claimed in claim 2, characterized in that: The liquid phase outlet of the centrifuge is connected to a distillation tank via a pipeline. The top gas phase outlet of the distillation tank is connected to a second condenser via a pipeline. The outlet of the second condenser is connected to an ethanol recovery tank via a pipeline. The outlet of the ethanol recovery tank is connected to the ethanol tank via a pipeline.

4. The triclosan preparation apparatus as described in claim 1, characterized in that: The gas phase outlet of the third reactor is connected to a heat exchanger via a pipeline, and the material outlet of the heat exchanger is connected to the first condenser via a pipeline. The jacket inlet and outlet of the heat exchanger are respectively connected to the jacket inlet and outlet of the first reactor via pipelines.

5. A device for the preparation of triclosan as claimed in claim 1, characterized in that: The outlet of the first condenser is connected to a third condenser via a pipe, the outlet of the third condenser is connected to an evaporator via a pipe, the top vapor outlet of the evaporator is connected to a fourth condenser via a pipe, and the outlet of the fourth condenser is connected to a solvent recovery tank via a pipe.

6. A device for the preparation of triclosan as claimed in claim 5, characterized in that: The outlet of the solvent recovery tank is connected to xylene tank I and xylene tank II via pipelines.

7. A device for the preparation of triclosan as claimed in claim 5, characterized in that: The outlet of the third condenser is connected to an alkaline washing tower via a pipeline. The alkaline washing tower is equipped with a circulation pump, and a gas exhaust port is located at the top of the alkaline washing tower.

8. A device for the preparation of triclosan according to claim 1, characterized in that: The first reactor is a vertical stirred reactor, the second reactor is a horizontal multi-chamber reactor, and the third reactor is a packed tower reactor.

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