Production system for triclosan diazonium reaction process

Abstract

The utility model relates to the technical field of triclosan production, in particular to a production system for a triclosan diazonium reaction process, which comprises an amino sulfate reaction kettle, a discharge port of the amino sulfate reaction kettle is communicated with a heat exchanger, and a discharge port of the heat exchanger is communicated with a first feed port of a tubular static mixer. The nitrosyl sulfuric acid conveying pipeline is communicated with a second feed port of the tubular static mixer, a discharge port of the tubular static mixer is communicated with a feed pipe of the tubular reactor, the feed pipe is provided with an external circulation inlet, and a discharge pipe of the tubular reactor is respectively communicated with the external circulation inlet and the dilution kettle. According to the production system, amino sulfate is prepared in advance through the amino sulfate reaction kettle, part of reaction heat is diluted in one step, the risk of concentrated release of the reaction heat is reduced, and the production safety is improved. The tubular reactor is adopted, so that the reaction time is shortened, side reactions are reduced, the reaction controllability and the reaction yield are improved, and the subsequent post-treatment difficulty and the production cost are reduced.

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 diazo 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. Existing technologies typically involve simultaneously adding amino compounds, sulfuric acid, and diazotizing reagents into the reaction vessel for the diazotization reaction. However, diazotization is a violently exothermic reaction; if the heat cannot be transferred in time, it can easily lead to a chain reaction. At best, the diazotizing reagent decomposes, releasing large amounts of toxic nitrous oxide, causing a "surging" or "boiler overflow" hazard; at worst, the diazonium salt decomposes, releasing large amounts of heat and gas, leading to an explosion. Therefore, to address these issues, it is necessary to develop a production system for the triclosan diazotization 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 diazo reaction process, which greatly improves the reaction 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 diazo reaction process includes an aminosulfate reactor, the outlet of which is connected to a heat exchanger, the outlet of which is connected to a first inlet of a tubular static mixer, a nitrosyl sulfuric acid conveying pipeline connected to a second inlet of the tubular static mixer, the outlet of which is connected to a feed pipe of a tubular reactor, the feed pipe having an external circulation inlet, and the outlet of the tubular reactor being connected to both the external circulation inlet and a dilution vessel.

[0006] As an improved technical solution, the outlet of the ammonium sulfate reactor is connected to the inlet of the heat exchanger via an ammonium sulfate delivery pump.

[0007] As an improved technical solution, the nitrosyl sulfuric acid conveying pipeline passes through the second inlet of the nitrosyl sulfuric acid metering pump.

[0008] As an improved technical solution, the tubular static mixer includes a body, one end of which is provided with a first inlet and a second inlet, and the other end of which is provided with a discharge outlet. The interior of the body is provided with a plurality of left-handed and right-handed guide plates alternately, and a baffle plate with a hollow structure is provided between two adjacent left-handed and right-handed guide plates.

[0009] As an improved technical solution, the left-handed guide vane is S-shaped, and the right-handed guide vane is rhomboid.

[0010] As an improved technical solution, the tubular reactor includes a body, a refrigerant inlet on one side of the bottom of the body, and a refrigerant outlet on one side of the upper part of the body; the interior of the body is provided with a rotating shaft and a material reaction coil, and the interior of the body is provided with a feed pipe and a discharge pipe connected to the material reaction coil; one end of the rotating shaft is connected to a motor, and multiple stirring components are provided on the rotating shaft.

[0011] As an improved technical solution, the plurality of stirring components are multiple stirring plates equally spaced on the rotating shaft, and the longitudinal section of each stirring plate is V-shaped.

[0012] As an improved technical solution, the feed pipe is provided with a purging and cleaning inlet, and the discharge pipe is provided with a washing liquid outlet.

[0013] As an improved technical solution, the outlet of the discharge pipe is connected to the external circulation inlet through a circulation pump and a circulation pipeline, and the circulation pipeline is connected to the dilution tank through a conveying pipeline.

[0014] After adopting the above technical solution, the beneficial effects of this utility model are:

[0015] The production system used in the triclosan diazo reaction process includes an ammonium sulfate reactor. The outlet of the ammonium sulfate reactor is connected to a heat exchanger, and the outlet of the heat exchanger is connected to the first inlet of a tubular static mixer. The nitrosyl sulfuric acid conveying pipeline is connected to the second inlet of the tubular static mixer. The outlet of the tubular static mixer is connected to the feed pipe of the tubular reactor, which has an external circulation inlet. The outlet pipe of the tubular reactor is connected to both the external circulation inlet and a dilution vessel. In actual production, the workers first add the ammonium sulfate material and sulfuric acid to the ammonium sulfate reactor. After the reaction, the ammonium sulfate enters the heat exchanger for cooling and then enters the tubular static mixer. At the same time, the nitrosyl sulfuric acid inside the nitrosyl sulfuric acid conveying pipeline also enters the tubular static mixer. After mixing, the material enters the tubular reactor, and the temperature required for the reaction is controlled. During the reaction, the material circulates through the tubular reactor via external circulation to promote a complete reaction. After the reaction, the material enters the dilution vessel for dilution and then proceeds to the next processing step. The aforementioned production system is rationally designed. By pre-mixing aminosulfate in the aminosulfate reactor, some of the reaction heat is diluted, reducing the risk of concentrated heat release and improving production safety. The use of a tubular reactor reduces reaction time, minimizes side reactions, improves reaction controllability and yield, and lowers the difficulty of subsequent post-processing and production costs.

[0016] The outlet of the ammonium sulfate reactor is connected to the inlet of the heat exchanger via an ammonium sulfate transfer pump. This design facilitates the delivery of ammonium sulfate to the interior of the heat exchanger for cooling.

[0017] Because the nitrosyl sulfuric acid delivery pipeline passes through the second inlet of the nitrosyl sulfuric acid metering pump, this design facilitates the rapid delivery of the nitrosyl sulfuric acid through the nitrosyl flow metering pump into the interior of the tubular static mixer.

[0018] The tubular static mixer comprises a main body with a first and second inlet at one end and an outlet at the other. The interior of the main body is alternately equipped with multiple left-handed and right-handed guide vanes, with perforated baffles between adjacent left-handed and right-handed guide vanes. Cooled aminosulfate enters the main body through the first inlet, while nitrosylsulfuric acid enters through the second inlet. Through the synergistic action of the left-handed guide vanes, baffles, and right-handed guide vanes, the two materials are ensured to fully contact and mix.

[0019] Because the left-hand guide vane is S-shaped and the right-hand guide vane is rhomboid, the two materials first come into contact with the S-shaped left-hand guide vane after entering the main body. The S-shaped and rhomboid designs increase the contact area between the material and the left-hand and right-hand guide vanes, which helps to disperse and mix the material evenly.

[0020] The tubular reactor comprises a main body with a refrigerant inlet on one side of the bottom and a refrigerant outlet on one side of the top. Inside the main body are a rotating shaft and a material reaction coil, with a feed pipe and a discharge pipe connected to the material reaction coil. One end of the rotating shaft is connected to a motor, and multiple stirring components are mounted on the shaft. In actual production, the liquid mixture, after being mixed by the tubular static mixer, enters the material reaction coil through the feed pipe. Once the motor starts, it drives the rotating shaft and multiple stirring components to agitate the refrigerant inside the main body, promoting uniform cooling of the liquid mixture within the material reaction coil. This tubular reactor structure is rationally designed, significantly reducing reaction time and the occurrence of side reactions, thus improving reaction efficiency.

[0021] Because the multiple stirring components consist of multiple stirring plates evenly spaced on the rotating shaft, and each stirring plate has a V-shaped longitudinal section, this structure of stirring components can achieve thorough stirring of the refrigerant, promote uniform heating of the materials inside the reaction coil, and further facilitate a complete reaction.

[0022] The feed pipe is equipped with a purging and cleaning inlet, and the discharge pipe is equipped with a washing liquid outlet. The residual liquid inside the reaction coil can be purged through the purging and cleaning inlet, and the inner wall of the reaction coil can also be cleaned. The washing liquid after cleaning is discharged from the washing liquid outlet.

[0023] The outlet of the discharge pipe is connected to the external circulation inlet via a circulation pump and circulation pipeline, and the circulation pipeline is connected to the dilution vessel via a conveying pipeline. The material inside the reaction coil enters the external circulation inlet through the circulation pump and circulation pipeline, thus realizing the circulation and mixing of the material. After the reaction is completed, the liquid is sent to the dilution vessel for dilution through the conveying pipeline. Attached Figure Description

[0024] Figure 1 This is a schematic diagram of the production system used in the triclosan diazo reaction process according to this utility model;

[0025] Among them, 1-Aminosulfate reactor, 2-Aminosulfate transfer pump, 3-Heat exchanger, 4-Tube static mixer, 40-First feed inlet, 41-Second feed inlet, 42-Discharge outlet, 43-Left-handed guide plate, 44-Baffle plate, 45-Right-handed guide plate, 5-Nitrosylsulfuric acid transfer pipeline, 6-Nitrosylsulfuric acid metering pump, 7-Flow meter, 8-Tube reactor, 80-Feed pipe, 800-External circulation inlet, 801-Purge and cleaning inlet, 81-Discharge pipe, 810-Washing liquid outlet, 82-Refrigerant inlet, 83-Refrigerant outlet, 84-Material reaction coil, 85-Rotating shaft, 86-Motor, 87-Stirring component, 9-Circulation pump, 10-Circulation pipeline, 11-Transfer pipeline, 12-Dilution vessel. 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 diazo reaction process, such as Figure 1 As shown, the reactor includes an aminosulfate reactor 1. The outlet of the aminosulfate reactor 1 is connected to a heat exchanger 3 (a shell-and-tube heat exchanger) via an aminosulfate transfer pump 2. The outlet of the heat exchanger 3 is connected to the first inlet of a tubular static mixer 4 (a flow meter 7 is installed on the pipe connecting the outlet of the heat exchanger and the tubular static mixer). A nitrosyl sulfuric acid transfer pipe 5 is connected to the second inlet of the tubular static mixer 4 via a nitrosyl sulfuric acid metering pump 6. The outlet of the tubular static mixer 4 is connected to the feed pipe 80 of a tubular reactor 8. An external circulation inlet 80 is provided on the feed pipe 80. The outlet of the discharge pipe 81 of the tubular reactor 8 is connected to the external circulation inlet 800 via a circulation pump 9 and a circulation pipe 10. The circulation pipe 9 is connected to a dilution vessel 12 via a transfer pipe 11. The tubular reactor 8 includes a body, with a refrigerant inlet 82 on one side of the bottom of the body and a refrigerant outlet 83 on one side of the upper part of the body; the body is equipped with a rotating shaft 85 and a material reaction coil 84 inside, and the body is also equipped with a feed pipe 80 and a discharge pipe 81 connected to the material reaction coil 84. One end of the rotating shaft 85 is connected to a motor 86, and multiple stirring components 87 are provided on the rotating shaft 85.

[0028] In actual production, the workers first add amino materials and sulfuric acid to the ammonium sulfate reactor. After the reaction, the ammonium sulfate is pumped into the heat exchanger and then cooled before entering the tubular static mixer. At the same time, the nitrosyl sulfuric acid in the nitrosyl sulfuric acid delivery pipeline is also pumped into the tubular static mixer via the nitrosyl sulfuric acid metering pump. After being mixed, the material enters the material reaction coil of the tubular reactor through the feed pipe. Meanwhile, the refrigerant enters the main body of the tubular reactor. After the motor starts, it drives the rotating shaft and multiple stirring components to stir the refrigerant inside the main body, which promotes uniform cooling of the liquid inside the reaction coil. During the reaction, the material inside the reaction coil enters the reaction coil from the external circulation inlet through the circulation pump and circulation pipeline, realizing the circulation and thorough mixing of the material, which helps the material to react fully. After the reaction is completed, the material enters the dilution tank through the conveying pipeline and then enters the next processing step.

[0029] The tubular static mixer 4 includes a main body, with a first inlet 40 and a second inlet 41 at one end and an outlet 42 at the other end. Multiple left-handed and right-handed guide plates 43 and 44 are alternately arranged inside the main body. A perforated baffle plate 45 is provided between adjacent left-handed and right-handed guide plates 43 (fixed on a baffle plate). Cooled aminosulfate enters the main body through the first inlet, while nitrosylsulfuric acid enters through the second inlet. Through the synergistic effect of the left-handed, right-handed, and left-handed guide plates, the two materials are fully contacted and mixed.

[0030] The left-hand guide plate 43 is S-shaped, and the right-hand guide plate 44 is rhomboid. After the two materials enter the body, they first come into contact with the S-shaped left-hand guide plate. The S-shaped and rhomboid designs increase the contact area between the materials and the left-hand and right-hand guide plates, which helps to disperse and mix the materials evenly.

[0031] The multiple stirring components 87 consist of several stirring plates evenly spaced on the rotating shaft, with each stirring plate having a V-shaped longitudinal section. This structure allows for thorough stirring of the refrigerant, ensuring uniform heating of the materials inside the reaction coil and promoting a more complete reaction.

[0032] The feed pipe 80 is equipped with a purge and cleaning inlet 801, and the discharge pipe 81 is equipped with a washing liquid outlet 810. The residual liquid inside the reaction coil can be purged through the purge and cleaning inlet, and the inner wall of the reaction coil can also be cleaned. The washing liquid after cleaning is discharged from the washing liquid outlet.

[0033] 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 diazo reaction process, characterized in that, The apparatus includes an aminosulfate reaction vessel, the outlet of which is connected to a heat exchanger, the outlet of which is connected to a first inlet of a tubular static mixer, a nitrosyl sulfuric acid conveying pipeline connected to a second inlet of the tubular static mixer, the outlet of which is connected to a feed pipe of a tubular reactor, the feed pipe having an external circulation inlet, and the outlet of the tubular reactor being connected to both the external circulation inlet and a dilution vessel.

2. The production system for the triclosan diazo reaction process according to claim 1, characterized in that, The outlet of the ammonium sulfate reactor is connected to the inlet of the heat exchanger via an ammonium sulfate delivery pump.

3. The production system for the triclosan diazo reaction process according to claim 1, characterized in that, The nitrosyl sulfuric acid delivery pipeline passes through the second inlet of the nitrosyl sulfuric acid metering pump.

4. The production system for the triclosan diazo reaction process according to claim 1, characterized in that, The tubular static mixer includes a body, one end of which is provided with a first inlet and a second inlet, and the other end of which is provided with a discharge outlet. The interior of the body is provided with a plurality of left-handed and right-handed guide plates alternately, and a hollow baffle is provided between two adjacent left-handed and right-handed guide plates.

5. The production system for the triclosan diazo reaction process according to claim 4, characterized in that, The left-handed guide vane is S-shaped, and the right-handed guide vane is rhomboid.

6. The production system for a triclosan diazo reaction process according to claim 1, characterized in that, The tubular reactor includes a main body, with a refrigerant inlet on one side of the bottom and a refrigerant outlet on one side of the top. Inside the main body, there is a rotating shaft and a material reaction coil. Inside the main body, there are a feed pipe and a discharge pipe connected to the material reaction coil. One end of the rotating shaft is connected to a motor, and multiple stirring components are provided on the rotating shaft.

7. The production system for a triclosan diazo reaction process according to claim 6, characterized in that, The multiple stirring components are multiple stirring plates arranged at equal intervals on the rotating shaft, and the longitudinal section of each stirring plate is V-shaped.

8. The production system for a triclosan diazo reaction process according to claim 6, characterized in that, The feed pipe is provided with a purging and cleaning inlet, and the discharge pipe is provided with a washing liquid outlet.

9. The production system for a triclosan diazo reaction process according to claim 6, characterized in that, The outlet of the discharge pipe is connected to the external circulation inlet via a circulation pump and a circulation pipeline, and the circulation pipeline is connected to the dilution vessel via a conveying pipeline.

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