A device for increasing the yield of triclosan

CN224686885UActive Publication Date: 2026-08-28SHANDONG AOYOU BIOLOGICAL TECH CO LTD
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Patent Information

Application Number
CN202522282844.6
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2025-10-28
Publication Date
2026-08-28
Estimated Expiration
2035-10-28

AI Technical Summary

Technical Problem

然而,现有三氯生的生产工艺中存在收率低、副反应多、传质传热效率不高以及废气处理不彻底等问题,制约了产品质量和生产效率的提升

Benefits of technology

[0017]本实用新型提供了一种提高三氯生收率的装置,包括连通的成盐反应罐、重氮化反应罐、水解罐;成盐反应罐与重氮化反应罐的连接管道上设有预混合器;水解罐的出液口连通萃取罐,萃取罐的有机相出口依次连通精馏塔、第一冷凝器和产品储罐;成盐反应罐、重氮化反应罐以及水解罐的夹套内均设有螺旋导流板;预混合器内设有冷却盘管,成盐反应罐、重氮化反应罐、水解罐内均设有搅拌装置,搅拌装置包括搅拌轴,搅拌轴的一端连接搅拌电机,搅拌轴的上部设有螺带式搅拌浆叶,搅拌轴的底部设有螺旋桨叶,螺旋浆叶的外侧套设有与搅拌轴连接的多孔扰流筒,多孔扰流筒的内壁以及外壁均设有多个导流槽。本装置通过螺带式搅拌浆叶与底部螺旋桨叶组合,并配合多孔扰流筒,能显著提升反应物料的混合效率,确保热量和物质传递更均匀。预混合器的设置能让物料在进入重氮化反应罐前预先混合并控制温度,使主反应更平稳。

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Abstract

The utility model discloses a device of improving triclosan yield, including salification reaction tank, diazotization reaction tank, hydrolysis tank, be equipped with premixer on the connecting pipeline of salification reaction tank and diazotization reaction tank, the liquid outlet intercommunication extraction tank of hydrolysis tank, the organic phase export intercommunication rectifying column, first condenser and product storage tank of extraction tank, be equipped with helical guide vane in the jacket of salification reaction tank, diazotization reaction tank, hydrolysis tank, be equipped with cooling coil in premixer, be equipped with stirring device in salification reaction tank, diazotization reaction tank, hydrolysis tank, and stirring device includes stirring shaft, and one end of stirring shaft is connected stirring motor, and the upper portion of stirring shaft is equipped with screw ribbon type stirring paddle, and the bottom of stirring shaft is equipped with propeller blade, and the outside of propeller blade is equipped with the porous spoiler of sleeve, and the inner wall and the outer wall of porous spoiler all are equipped with a plurality of guide grooves. The device not only production efficiency is high, and can carry out effective treatment to the waste gas in production process, avoids the secondary pollution to the environment.
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Description

Technical Field

[0001] This utility model relates to chemical production equipment, specifically to an apparatus for improving the yield of triclosan. Background Technology

[0002] Triclosan, chemically known as 2,4,4'-trichloro-2'-hydroxydiphenyl ether, is a broad-spectrum antibacterial agent widely used in daily chemical products, medical disinfection, and plastic products. However, existing triclosan production processes suffer from low yield, numerous side reactions, low mass and heat transfer efficiency, and incomplete waste gas treatment, hindering improvements in product quality and production efficiency.

[0003] In traditional triclosan production facilities, insufficient mixing of reactants, localized overheating, or uneven concentration can easily lead to the formation of byproducts, reducing the yield of the target product. Furthermore, if acidic gases and volatile organic compounds generated during the reaction are not effectively treated, they can cause environmental pollution and equipment corrosion.

[0004] Therefore, there is an urgent need for a production device that integrates high production efficiency and multi-stage waste gas treatment to improve the reaction yield and product quality of triclosan, while achieving clean production and efficient resource utilization. Utility Model Content

[0005] The technical problem to be solved by this utility model is to provide a device for improving the yield of triclosan, which not only has high production efficiency, but also can effectively treat the waste gas in the production process and avoid secondary pollution to the environment.

[0006] To solve the above-mentioned technical problems, the technical solution of this utility model is as follows:

[0007] An apparatus for improving the yield of triclosan includes a salt-forming reaction tank, a diazotization reaction tank, and a hydrolysis tank connected in series; a premixer is provided on the connecting pipe between the salt-forming reaction tank and the diazotization reaction tank; the outlet of the hydrolysis tank is connected to an extraction tank, and the organic phase outlet of the extraction tank is sequentially connected to a distillation column, a first condenser, and a product storage tank.

[0008] The jackets of the salt-forming reaction tank, diazotization reaction tank, and hydrolysis tank are all equipped with spiral guide plates; the premixer is equipped with a cooling coil; the salt-forming reaction tank, diazotization reaction tank, and hydrolysis tank are all equipped with stirring devices, each stirring device including a stirring shaft, one end of which is connected to a stirring motor; the upper part of the stirring shaft is equipped with a ribbon-type stirring blade; the bottom of the stirring shaft is equipped with a propeller blade; a porous baffle cylinder connected to the stirring shaft is fitted around the outside of the propeller blade; and multiple guide grooves are provided on both the inner and outer walls of the porous baffle cylinder.

[0009] Preferably, the connecting pipe between the salt formation reaction vessel and the diazotization reaction vessel is equipped with a first buffer tank with a jacket.

[0010] Preferably, a jacketed second buffer tank is provided on the connecting pipe between the diazotization reaction vessel and the hydrolysis vessel.

[0011] Preferably, the spiral guide plate is provided with turbulence holes.

[0012] Preferably, the gas outlets of the salt formation reaction tank, the diazotization reaction tank, and the hydrolysis tank are all connected to the tail gas treatment mechanism; the tail gas treatment mechanism includes a second condenser, a primary alkali absorption tower, an oxidation absorption tower, a secondary alkali absorption tower, an activated carbon adsorption tower, an induced draft fan, and an exhaust stack.

[0013] Preferably, a demister is provided at the top of the first condenser, the first-stage alkaline absorption tower, the oxidation absorption tower, and the second-stage alkaline absorption tower.

[0014] Preferably, the inner walls of the primary alkali absorption tower, the oxidation absorption tower, and the secondary alkali absorption tower are provided with multiple porous diversion plates.

[0015] Preferably, the holes on adjacent perforated flow dividers are arranged in an alternating pattern.

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

[0017] This invention provides an apparatus for improving the yield of triclosan, comprising a connected salt-forming reaction tank, a diazotization reaction tank, and a hydrolysis tank; a premixer is installed on the connecting pipe between the salt-forming reaction tank and the diazotization reaction tank; the outlet of the hydrolysis tank is connected to an extraction tank, and the organic phase outlet of the extraction tank is sequentially connected to a distillation column, a first condenser, and a product storage tank; spiral guide plates are installed in the jackets of the salt-forming reaction tank, the diazotization reaction tank, and the hydrolysis tank; a cooling coil is installed in the premixer; and a stirring device is installed in each of the salt-forming reaction tank, the diazotization reaction tank, and the hydrolysis tank. The stirring device includes a stirring shaft, one end of which is connected to a stirring motor; a ribbon-type stirring blade is installed at the upper part of the stirring shaft; a propeller blade is installed at the bottom of the stirring shaft; and a porous baffle tube connected to the stirring shaft is fitted around the outside of the propeller blade. Multiple guide grooves are provided on the inner and outer walls of the porous baffle tube. This apparatus, through the combination of the ribbon-type stirring blade and the bottom propeller blade, and in conjunction with the porous baffle tube, can significantly improve the mixing efficiency of the reactants, ensuring more uniform heat and mass transfer. The premixer allows materials to be premixed and the temperature controlled before entering the diazotization reactor, resulting in a more stable main reaction.

[0018] The combined use of spiral guide plates and turbulence holes in this device significantly improves the flow of the heat exchange medium within the jacket, breaks down the boundary layer, enhances heat transfer efficiency, and enables more precise and faster reaction temperature control. The cooling coils within the premixer promptly remove any heat generated during mixing, preventing localized overheating and potential side reactions.

[0019] The gas outlets of the salt formation reaction tank, diazotization reaction tank, and hydrolysis tank in this unit are all connected to the tail gas treatment mechanism. The tail gas treatment mechanism includes a first condenser, a primary alkali absorption tower, an oxidation absorption tower, a secondary alkali absorption tower, an activated carbon adsorption tower, an induced draft fan, and an exhaust stack. Demisters are installed at the top of the first condenser, the primary alkali absorption tower, the oxidation absorption tower, and the secondary alkali absorption tower. This setup effectively treats and ensures the emission of harmful gases in compliance with environmental protection requirements. The demisters reduce liquid entrainment, improve absorption efficiency, and protect downstream equipment.

[0020] The inner walls of the primary alkali absorption tower, oxidation absorption tower, and secondary alkali absorption tower of this device are equipped with multiple porous flow dividers. The holes on adjacent porous flow dividers are staggered. The porous flow dividers and their staggered holes increase the gas-liquid contact area and path, prevent gas flow deviation, and ensure thorough treatment of waste gas. Attached Figure Description

[0021] To more clearly illustrate the technical solutions in the embodiments of this utility model or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0022] Figure 1 This is a schematic diagram of the structure of Embodiment 1 of this utility model;

[0023] Figure 2 yes Figure 1 Enlarged structural diagram at point A;

[0024] Figure 3 This is a schematic diagram of the porous baffle tube in Example 1;

[0025] In the diagram, 1. Salt formation reaction vessel; 2. Diazotization reaction vessel; 3. Hydrolysis vessel; 4. Premixer; 5. Extraction vessel; 6. Distillation column; 7. First condenser; 8. Product storage tank; 9. First buffer tank; 10. Second buffer tank; 11. Spiral guide plate; 12. Turbulence hole; 13. Cooling coil; 14. Stirring shaft; 15. Stirring motor; 16. Ribbon-type stirring blade; 17. Propeller blade; 18. Porous turbulence cylinder; 19. Guide channel; 20. Second condenser; 21. Primary alkali absorption tower; 22. Oxidation absorption tower; 23. Secondary alkali absorption tower; 24. Activated carbon adsorption tower; 25. Exhaust fan; 26. Discharge cylinder; 27. Demister; 28. Diverter plate. Detailed Implementation

[0026] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present utility model.

[0027] Example 1

[0028] like Figures 1 to 3 As shown, an apparatus for improving the yield of triclosan includes a salt-forming reaction tank 1, a diazotization reaction tank 2, and a hydrolysis tank 3 connected in series. A premixer 4 is provided on the connecting pipe between the salt-forming reaction tank 1 and the diazotization reaction tank 2. The outlet of the hydrolysis tank 3 is connected to an extraction tank 5, and the organic phase outlet of the extraction tank 5 is sequentially connected to a distillation column 6, a first condenser 7, and a product storage tank 8. A first buffer tank 9 with a jacket is provided on the connecting pipe between the salt-forming reaction tank 1 and the diazotization reaction tank 2. A second buffer tank 10 with a jacket is provided on the connecting pipe between the diazotization reaction tank 2 and the hydrolysis tank 3. This apparatus premixes the aminosulfate feed solution and nitrosylsulfuric acid, the raw materials for the diazotization reaction, through the premixer 4, thereby ensuring sufficient contact and temperature control of the reaction raw materials before they enter the diazotization reaction tank 2, thus improving the efficiency of the diazotization reaction and reducing the occurrence of side reactions.

[0029] The jackets of the salt-forming reaction tank 1, the diazotization reaction tank 2, and the hydrolysis tank 3 are all equipped with spiral guide plates 11; the spiral guide plates 11 are provided with turbulence holes 12; the spiral guide plates 11 can extend the flow path of the cooling medium and increase the heat exchange time; while the design of the turbulence holes 12 further disrupts the laminar flow of the cooling medium and forms turbulence, which greatly improves the heat transfer coefficient and heat exchange efficiency of the jacket, and improves the reaction efficiency to a certain extent.

[0030] The premixer 4 is equipped with a cooling coil 13. The salt-forming reaction tank 1, diazotization reaction tank 2, and hydrolysis tank 3 are all equipped with stirring devices. Each stirring device includes a stirring shaft 14, one end of which is connected to a stirring motor 15. The upper part of the stirring shaft 14 is equipped with a ribbon-type stirring blade 16, and the bottom of the stirring shaft 14 is equipped with a propeller blade 17. A porous baffle cylinder 18, connected to the stirring shaft 14, is fitted around the outside of the propeller blade. The inner and outer walls of the porous baffle cylinder 18 are equipped with multiple guide grooves 19. The stirring device of this apparatus, through the combination of the ribbon-type stirring blade 16 and the propeller blade 17, along with the baffle cylinder 18 and the guide grooves 19, generates strong axial and radial circulation during the stirring process. This ensures that the materials achieve a high degree of uniform mixing at both the macroscopic and microscopic scales, avoiding excessively high local concentrations or uneven temperatures, making the reaction more complete and thorough, thereby improving the reaction conversion rate and yield.

[0031] The gas outlets of the salt-forming reaction tank 1, the diazotization reaction tank 2, and the hydrolysis tank 3 are all connected to a tail gas treatment mechanism. This tail gas treatment mechanism includes a second condenser 20, a primary alkali absorption tower 21, an oxidation absorption tower 22, a secondary alkali absorption tower 23, an activated carbon adsorption tower 24, an induced draft fan 25, and an exhaust stack 26. This device collects the tail gas from the reaction process and treats it through multiple stages, achieving high treatment efficiency and avoiding secondary air pollution.

[0032] Furthermore, in this embodiment, the top of the first condenser 20, the primary alkaline absorption tower 21, the oxidation absorption tower 22, and the secondary alkaline absorption tower 23 are equipped with demisters 27, which can effectively capture liquid droplets entrained in the exhaust gas, preventing material loss and corrosion of subsequent equipment.

[0033] Furthermore, in this embodiment, the inner walls of the primary alkaline absorption tower 21, the oxidation absorption tower 22, and the secondary alkaline absorption tower 23 are provided with multiple porous flow dividers 28; the holes on adjacent porous flow dividers 28 are staggered. This arrangement can greatly increase the contact area and contact time between the gas and liquid phases, thereby improving the absorption efficiency.

[0034] The working principle of this device is as follows:

[0035] In the preparation of triclosan, the reactants 2,4,4'-trichloro-2'-aminodiphenyl ether and sulfuric acid are mixed and reacted in a salt-forming reaction tank 1. After the reaction, the resulting aminosulfate solution is cooled in a first buffer tank 9 and then enters a premixer 4 to be mixed evenly with nitrosyl sulfuric acid before entering a diazotization reaction tank 2 for further reaction. After the diazotization reaction, the resulting solution is diluted in a second buffer tank 10 and then enters a hydrolysis tank 3 to be mixed with sulfuric acid for hydrolysis. After the hydrolysis, the solution enters an extraction tank 5 for cooling, extraction, and separation. The resulting organic phase enters a distillation column 6 for distillation to recover the target product. The waste gas generated in the salt-forming reaction tank 1, the diazotization reaction tank 2, and the hydrolysis tank 3 during the above reaction process is condensed in a second condenser 20 and then sequentially treated by a primary alkali absorption tower 21, an oxidation absorption tower 22, a secondary alkali absorption tower 23, and an activated carbon adsorption tower 24. After meeting the standards, the waste gas is discharged into the atmosphere through an exhaust stack 26 by an induced draft fan 25.

[0036] The above description of the disclosed embodiments enables those skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. An apparatus for improving the yield of triclosan, characterized in that: It includes a connected salt-forming reaction tank, a diazotization reaction tank, and a hydrolysis tank; a premixer is provided on the connecting pipe between the salt-forming reaction tank and the diazotization reaction tank; the outlet of the hydrolysis tank is connected to an extraction tank, and the organic phase outlet of the extraction tank is sequentially connected to a distillation column, a first condenser, and a product storage tank; The jackets of the salt-forming reaction tank, diazotization reaction tank, and hydrolysis tank are all equipped with spiral guide plates; the premixer is equipped with a cooling coil; the salt-forming reaction tank, diazotization reaction tank, and hydrolysis tank are all equipped with stirring devices, each stirring device including a stirring shaft, one end of which is connected to a stirring motor; the upper part of the stirring shaft is equipped with a ribbon-type stirring blade; the bottom of the stirring shaft is equipped with a propeller blade; a porous baffle cylinder connected to the stirring shaft is fitted around the outside of the propeller blade; and multiple guide grooves are provided on both the inner and outer walls of the porous baffle cylinder.

2. The apparatus for improving the yield of triclosan according to claim 1, characterized in that: The connecting pipe between the salt formation reaction vessel and the diazotization reaction vessel is equipped with a first buffer tank with a jacket.

3. The apparatus for improving the yield of triclosan according to claim 1, characterized in that: The connecting pipe between the diazotization reaction vessel and the hydrolysis vessel is equipped with a second buffer tank with a jacket.

4. The apparatus for improving the yield of triclosan according to claim 1, characterized in that: The spiral guide plate is provided with turbulence holes.

5. The apparatus for improving the yield of triclosan according to claim 1, characterized in that: The gas outlets of the salt formation reaction tank, the diazotization reaction tank, and the hydrolysis tank are all connected to the tail gas treatment mechanism; the tail gas treatment mechanism includes a second condenser, a primary alkali absorption tower, an oxidation absorption tower, a secondary alkali absorption tower, an activated carbon adsorption tower, an induced draft fan, and an exhaust stack.

6. The apparatus for improving the yield of triclosan according to claim 5, characterized in that: Demisters are installed at the top of the first condenser, the first-stage alkali absorption tower, the oxidation absorption tower, and the second-stage alkali absorption tower.

7. The apparatus for improving the yield of triclosan according to claim 5, characterized in that: The inner walls of the primary alkali absorption tower, the oxidation absorption tower, and the secondary alkali absorption tower are equipped with multiple porous diversion plates.

8. The apparatus for improving the yield of triclosan according to claim 7, characterized in that: The holes on adjacent perforated flow dividers are arranged in an alternating pattern.