Production system for triclosan hydrolysis reaction process
By designing a heat exchanger and a tubular hydrolysis reactor, continuous production of triclosan hydrolysis was achieved, improving hydrolysis yield and production efficiency, reducing energy consumption and side reactions, and solving the problem of low utilization rate of traditional hydrolysis reactor equipment.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- SHANDONG AOYOU BIOLOGICAL TECH CO LTD
- Filing Date
- 2025-05-20
- Publication Date
- 2026-05-12
AI Technical Summary
Existing triclosan hydrolysis processes suffer from long production cycles, low equipment utilization, high energy consumption, low hydrolysis yield, and low thermal energy utilization. Traditional equipment also presents problems such as reaction risks and frequent side reactions.
The device employs a heat exchanger and a tubular hydrolysis reactor. The precise addition of sulfuric acid and diazonium salt dilution is controlled by a metering pump. Multi-layer reaction coils and electric heating rods are used for synergistic heating. Temperature and pressure sensors are used to control reaction conditions, enabling continuous production and uniform heating, thereby reducing heat consumption and side reactions.
It improves the efficiency and yield of hydrolysis reaction, reduces reaction risk, achieves efficient utilization of thermal energy and stability of product quality, and reduces the occurrence of side reactions.
Smart Images
Figure CN224221360U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of triclosan production technology, and in particular to a production system for the triclosan hydrolysis reaction process. Background Technology
[0002] Triclosan is a safe, highly effective, and broad-spectrum antibacterial agent, widely used in the daily chemical, medical, and textile industries due to its excellent antibacterial properties. Currently, the main industrial processes both domestically and internationally primarily use dichlorophenol as a raw material, which undergoes sequential etherification, nitro reduction, diazotization, and hydrolysis with dichloronitrobenzene, followed by extraction and distillation to obtain the target product. However, the key processes determining production costs and product quality are the diazotization and hydrolysis reactions. Traditional hydrolysis processes use reaction vessels as the reaction equipment, resulting in long production cycles, low equipment utilization, and excessive energy consumption. The intermittent reaction leads to low hydrolysis yields. Furthermore, the hydrolysis reaction uses sulfuric acid as a substrate, heating it to approximately 180°C, adding a diazonium salt diluent, and then cooling the material from approximately 180°C to below 90°C before proceeding to the next production step. Separate handling of raw material heating and reactant cooling results in low thermal energy utilization. Therefore, to address these issues, it is necessary to develop a production system for the triclosan hydrolysis reaction process. Utility Model Content
[0003] The technical problem to be solved by this utility model is to provide a production system for the triclosan hydrolysis reaction process, which greatly improves the hydrolysis yield and reduces the reaction risk, 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] A production system for a triclosan hydrolysis reaction process includes a heat exchanger and a tubular hydrolysis reactor. The inlet of the heat exchanger is connected to a sulfuric acid delivery pipeline. The outlet of the heat exchanger and the diazonium salt dilution solution delivery pipeline are respectively connected to the sulfuric acid inlet pipe and the diazonium salt dilution solution inlet pipe of the tubular hydrolysis reactor. The outlet pipe of the tubular hydrolysis reactor is respectively connected to the heat medium inlet of the heat exchanger. The heat medium outlet of the heat exchanger is connected to an extraction vessel.
[0006] As an improved technical solution, the sulfuric acid conveying pipeline is connected to the inlet of the heat exchanger via a metering pump.
[0007] As an improved technical solution, the diazonium salt dilution solution delivery pipeline is connected to the tubular hydrolysis reaction device via a metering pump.
[0008] As an improved technical solution, the tubular hydrolysis reactor includes a main body, inside which are arranged multiple interconnected reaction coils. At both ends of the main body are sulfuric acid feed pipe and discharge pipe connected to the reaction coils, respectively. At the top of the main body, at a distance of 1 / 3 from the total number of reaction coil layers, is a diazonium salt dilution inlet pipe connected to the reaction coils. A heat medium inlet is provided on one side of the top of the main body, and a heat medium outlet is provided on one side of the bottom of the main body. An electric heating rod is provided between two adjacent reaction coil layers.
[0009] As an improved technical solution, the top of the main body is provided with a diazonium salt dilution inlet pipe connected to the reaction coil at 1 / 3 of the distance from the total number of reaction coil layers.
[0010] As an improved technical solution, the sulfuric acid feed pipe is provided with a purging and cleaning port, and the discharge pipe is provided with a cleaning liquid outlet.
[0011] As an improved technical solution, the body is equipped with two liquid level gauges inside, and the top of the body is also equipped with an interface that connects to the heat medium buffer tank.
[0012] As an improved technical solution, the body is equipped with a first temperature sensor, the reaction coil is equipped with a second temperature sensor, and the first temperature sensor, the second temperature sensor and the electric heating rod are electrically connected to the controller.
[0013] As an improved technical solution, pressure sensors are respectively provided at the inlet and outlet ends of the reaction coil, and the pressure sensors are electrically connected to the controller.
[0014] After adopting the above technical solution, the beneficial effects of this utility model are:
[0015] The production system used in the triclosan hydrolysis reaction process includes a heat exchanger and a tubular hydrolysis reactor. The heat exchanger's inlet is connected to a sulfuric acid delivery pipeline, and its outlet, along with the diazonium salt dilution delivery pipeline, is connected to the sulfuric acid inlet and diazonium salt dilution inlet of the tubular hydrolysis reactor, respectively. The tubular hydrolysis reactor's outlet is connected to the heat medium inlet of the heat exchanger, and the heat medium outlet of the heat exchanger is connected to the extraction vessel. In actual production, at the beginning of the hydrolysis reaction, sulfuric acid and diazonium salt dilution are delivered to the tubular hydrolysis reactor at a certain flow rate and ratio. The high-temperature material after the hydrolysis reaction enters the heat exchanger. The next batch of sulfuric acid for the hydrolysis reaction enters the heat exchanger, undergoes heat exchange, and then enters the tubular hydrolysis reactor. Simultaneously, the diazonium salt dilution participating in the hydrolysis reaction enters the tubular hydrolysis reactor at a certain flow rate and a specified ratio with sulfuric acid for hydrolysis. The hydrolyzed material after heat exchange enters the extraction vessel for extraction, and then the extracted triclosan undergoes further processing. The aforementioned production system is rationally designed, achieving sufficient heat exchange between the reaction raw material (sulfuric acid) and the hydrolysis reaction product liquid through a heat exchanger, thereby reducing heat energy consumption. The tubular hydrolysis reactor allows for continuous production, significantly improving reaction efficiency and overall production efficiency.
[0016] The sulfuric acid delivery pipeline is connected to the inlet of the heat exchanger via a metering pump. The metering pump allows for precise control of the amount of sulfuric acid added during the hydrolysis reaction, ensuring accurate feeding.
[0017] The diazonium salt dilution solution is delivered through a pipeline connected to the tubular hydrolysis reactor via a metering pump. The metering pump allows control over the amount of diazonium salt dilution solution added during the hydrolysis reaction.
[0018] The tubular hydrolysis reactor consists of a main body containing multiple interconnected reaction coils. Both ends of the main body are connected to the reaction coils via a sulfuric acid feed pipe and a discharge pipe, respectively. The top of the main body has a diazonium salt dilution inlet pipe connected to the reaction coils. A heat transfer medium inlet is located on one side of the top of the main body, and a heat transfer medium outlet is located on one side of the bottom. Electric heating rods are installed between adjacent reaction coils. In actual production, sulfuric acid and diazonium salt dilution enter the reaction coils through the sulfuric acid feed pipe and diazonium salt dilution inlet pipe, respectively. The heat transfer medium (heat transfer oil) and electric heating rods work together to heat the materials inside the reaction coils, resulting in more uniform heating of the reactants. The entire process meets both the reaction time requirements and the requirement for precise material proportioning, achieving continuous production while ensuring controllable and stable product quality.
[0019] Because the top of the reactor body has a diazonium salt dilution inlet pipe connected to the reaction coil at one-third of the distance from the total number of reaction coil layers, the diazonium salt dilution inlet pipe is located at one-third of the distance from the total number of reaction coil layers. Instead of being mixed with the hydrolyzed sulfuric acid before entering the tubular hydrolysis reactor, this placement ensures that the sulfuric acid is sufficiently heated, reducing the time it takes for the diazonium salt dilution to reach the reaction temperature from a low temperature. This reduces side reactions, increases product yield, and lowers the difficulty of post-processing purification and the generation of pollution sources.
[0020] The sulfuric acid feed pipe is equipped with a purge and cleaning port, and the discharge pipe is equipped with a cleaning solution outlet. The purge and cleaning port facilitates the purging and cleaning of materials on the inner wall of the reaction coil, and the cleaning solution is discharged from the cleaning solution outlet.
[0021] The main body is equipped with two level gauges inside, and an interface connecting to the heat transfer oil buffer tank is located on its top. The level gauges allow for real-time monitoring of heat transfer oil loss and timely replenishment, preventing the reaction coils from drying out. The interface connecting to the heat transfer oil buffer tank ensures the reaction unit remains filled with heat transfer oil during thermal expansion and contraction, preventing oil leakage.
[0022] The main body is equipped with a first temperature sensor, and the reaction coil is equipped with a second temperature sensor. The first and second temperature sensors, along with the electric heating rod, are electrically connected to the controller. The first temperature sensor detects the temperature of the heating medium and the electric heating rod. When these temperatures exceed a set value, the controller cuts off heating by the electric heating rod or discharges the heating medium (guide oil), stopping the heating of the material inside the reaction coil. Similarly, when the second temperature sensor detects that the material temperature exceeds a set value, the controller also cuts off heating by the electric heating rod or discharges the heating medium. This design allows for precise control of the material temperature inside the reaction coil, which is more conducive to the hydrolysis reaction and reduces the occurrence of side reactions.
[0023] Pressure sensors are installed at both the inlet and outlet of the reaction coil, and these sensors are electrically connected to the controller. The pressure sensors can detect the pressure inside the reaction coil. When the pressure exceeds the set pressure, the operator determines whether pipeline cleaning and purging are necessary. Attached Figure Description
[0024] Figure 1 This is a schematic diagram of the production system used in the triclosan hydrolysis reaction process according to this utility model;
[0025] Among them, 1-heat exchanger, 2-tubular hydrolysis reaction device, 20-sulfuric acid feed pipe, 200-purge and cleaning port, 21-diazonium salt dilution solution inlet pipe, 22-reaction coil, 23-discharge pipe, 230-cleaning solution outlet, 24-heating medium inlet, 25-heating medium outlet, 26-electric heating rod, 27-interface, 3-sulfuric acid conveying pipeline, 4, 6-metering pump, 5-diazonium salt dilution solution conveying pipeline, 7-extraction vessel, 8-level gauge, 9-heating medium buffer tank, 10-first temperature sensor, 11-second temperature sensor, 12-controller, 13-pressure sensor, 14-flow meter. Detailed Implementation
[0026] To make the objectives, technical solutions, and advantages of this utility model clearer, the present utility model will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present utility model and are not intended to limit the present utility model.
[0027] A production system for a triclosan hydrolysis reaction process, such as Figure 1 As shown, the apparatus includes a heat exchanger 1 (rolled plate heat exchanger) and a tubular hydrolysis reactor 2. A sulfuric acid delivery pipeline 3 (equipped with a flow meter 14) is connected to the inlet of the heat exchanger 1 via a metering pump 4. The outlet of the heat exchanger 1 is connected to the sulfuric acid feed pipe 20 of the tubular hydrolysis reactor 2. A diazonium salt dilution delivery pipeline 5 is connected to the diazonium salt dilution inlet pipe 21 of the tubular hydrolysis reactor 2 via a metering pump 6. The outlet pipe of the tubular hydrolysis reactor 2 is connected to the heat medium inlet of the heat exchanger 1. The heat medium outlet of the heat exchanger 1 is connected to the extraction vessel 7. The tubular hydrolysis reactor 2 includes a main body, inside which are multiple interconnected reaction coils 22. At both ends of the main body are sulfuric acid feed pipes 20 and discharge pipes 23 connected to the reaction coils 22, respectively. At the top of the main body is a diazonium salt dilution inlet pipe 21 connected to the reaction coils 22. A heat medium inlet 24 is provided on one side of the top of the main body, and a heat medium outlet 25 is provided on one side of the bottom of the main body. An electric heating rod 26 is provided between two adjacent reaction coils 22.
[0028] In actual production, the hydrolysis reaction begins with a metering pump delivering diluted sulfuric acid and diazonium salt solution to the reaction pipes of the tubular hydrolysis reactor at a specific flow rate and ratio. A heat transfer medium (heat transfer oil) and electric heating rods work together to heat the hydrolysate, providing the necessary temperature for the reaction. The high-temperature hydrolysis product solution, after hydrolysis, enters a heat exchanger as the heat medium. The next batch of sulfuric acid enters the heat exchanger and, after heat exchange, enters the tubular hydrolysis reactor. Simultaneously, the next batch of diluted diazonium salt solution, also participating in the hydrolysis reaction, enters the reactor at a specific flow rate and ratio with sulfuric acid for further hydrolysis. The hydrolysate, after heat exchange, enters an extraction vessel for extraction, followed by further processing of the extracted triclosan. Throughout the hydrolysis process, the hydrolysate is heated more uniformly. The multi-layer reaction coil design ensures that the reaction time requirements are met, and the metering pump allows for precise material proportioning, achieving continuous production while maintaining controllable and stable product quality.
[0029] The top of the main body, at one-third of the distance from the total number of reaction coil layers, has a diazonium salt dilution inlet pipe 21 connected to the reaction coil 22. The diazonium salt dilution inlet pipe is located at one-third of the distance from the total number of reaction coil layers, rather than being mixed with the hydrolyzed sulfuric acid before entering the tubular hydrolysis reactor. This allows the sulfuric acid to be sufficiently heated, reducing the time it takes for the diazonium dilution to reach the reaction temperature from a low temperature, thereby reducing side reactions, increasing product yield, and lowering the difficulty of post-processing purification and the generation of pollution sources.
[0030] The sulfuric acid feed pipe 20 is equipped with a purge and cleaning port 200, and the discharge pipe 23 is equipped with a cleaning liquid outlet 230. The purge and cleaning port facilitates the purging and cleaning of materials on the inner wall of the reaction coil, and the cleaning liquid is discharged from the cleaning liquid outlet.
[0031] The main body is equipped with two level gauges 8 (electrically connected to the controller), and the top of the main body also has an interface 27 that connects to the heat transfer medium buffer tank 9. The level gauges allow observation of the heat transfer medium (heat transfer oil) level within the reaction device, facilitating timely replenishment. The interface ensures that the heat transfer oil remains full and does not overflow when the heat transfer oil expands or contracts due to temperature changes.
[0032] The reactor body is equipped with a first temperature sensor 10, and the reaction coil 22 is equipped with a second temperature sensor 11. The first temperature sensor 10, the second temperature sensor 11, and the electric heating rod 26 are electrically connected to the controller 12. The first temperature sensor detects the temperature of the heating medium and the electric heating rod. When the temperature exceeds the set value, the controller cuts off the heating of the electric heating rod or discharges the heating medium (guide oil), stopping the heating of the material in the reaction coil. When the second temperature sensor detects that the material temperature exceeds the set value, the controller also cuts off the heating of the electric heating rod or discharges the heating medium. This design can accurately control the temperature of the material in the reaction coil, which is more conducive to the hydrolysis reaction and reduces the occurrence of side reactions.
[0033] Pressure sensors 13 are installed at the inlet and outlet of the reaction coil 22, respectively, and the pressure sensors 13 are electrically connected to the controller 12. The pressure sensors can detect the pressure inside the reaction coil. When the pressure exceeds the set pressure, the operator can determine whether pipeline cleaning and purging is required.
[0034] The above description is only a preferred embodiment of the present utility model and is not intended to limit the present utility model. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present utility model should be included within the protection scope of the present utility model.
Claims
1. A production system for a triclosan hydrolysis reaction process, characterized in that, The device includes a heat exchanger and a tubular hydrolysis reactor. The inlet of the heat exchanger is connected to a sulfuric acid delivery pipeline. The outlet of the heat exchanger and the diazonium salt dilution solution delivery pipeline are respectively connected to the sulfuric acid inlet pipe and the diazonium salt dilution solution inlet pipe of the tubular hydrolysis reactor. The outlet pipe of the tubular hydrolysis reactor is respectively connected to the heat medium inlet of the heat exchanger. The heat medium outlet of the heat exchanger is connected to the extraction vessel.
2. The production system for the triclosan hydrolysis reaction process according to claim 1, characterized in that, The sulfuric acid delivery pipeline is connected to the inlet of the heat exchanger via a metering pump.
3. The production system for the triclosan hydrolysis reaction process according to claim 1, characterized in that, The diazonium salt dilution solution delivery pipeline is connected to the tubular hydrolysis reaction device via a metering pump.
4. The production system for the triclosan hydrolysis reaction process according to claim 1, characterized in that, The tubular hydrolysis reactor includes a main body, inside which are arranged multiple interconnected reaction coils. At both ends of the main body are sulfuric acid feed pipes and discharge pipes connected to the reaction coils, respectively. At the top of the main body, at a distance of 1 / 3 from the total number of reaction coil layers, is a diazonium salt dilution inlet pipe connected to the reaction coils. A heat medium inlet is provided on one side of the top of the main body, and a heat medium outlet is provided on one side of the bottom of the main body. An electric heating rod is provided between two adjacent reaction coil layers.
5. The production system for the triclosan hydrolysis reaction process according to claim 4, characterized in that, The top of the main body has a diazonium salt dilution inlet pipe connected to the reaction coil at a distance of 1 / 3 from the total number of reaction coil layers.
6. The production system for the triclosan hydrolysis reaction process according to claim 4, characterized in that, The sulfuric acid feed pipe is equipped with a purging and cleaning port, and the discharge pipe is equipped with a cleaning liquid outlet.
7. The production system for the triclosan hydrolysis reaction process according to claim 4, characterized in that, The body is equipped with two liquid level gauges inside, and the top of the body is also equipped with an interface that connects to the heat medium buffer tank.
8. The production system for the triclosan hydrolysis reaction process according to claim 4, characterized in that, The main body is equipped with a first temperature sensor, and the reaction coil is equipped with a second temperature sensor. The first temperature sensor, the second temperature sensor, and the electric heating rod are electrically connected to the controller.
9. The production system for the triclosan hydrolysis reaction process according to claim 4, characterized in that, Pressure sensors are respectively installed at the inlet and outlet of the reaction coil, and the pressure sensors are electrically connected to the controller.