Hydrolysis reaction device for 2, 4-difluoronitrobenzene

Abstract

The utility model provides a 2, 4-difluoronitrobenzene hydrolysis reaction device, which belongs to the technical field of chemical production equipment and comprises a hydrolysis reaction kettle and a neutralization kettle, an inlet of the hydrolysis reaction kettle is connected with the washing water transfer tank and the raw material tank, an alkali inlet is connected with the alkali metering pump, and an acid inlet is connected with the acid storage tank through the acid metering pump; an outlet of the hydrolysis reaction kettle is connected with an inlet of the neutralization kettle, and an acid neutralization inlet of the neutralization kettle is connected with the acid metering pump; an upper-layer outlet of the neutralization kettle is connected with the washing kettle; a lower-layer outlet of the washing kettle is connected with the washing water transfer tank, and an upper-layer outlet is connected with the preheating kettle; the preheating kettle is connected with a film evaporator through a pipeline heater, and a product outlet of the film evaporator is connected with a product receiving tank. According to the device, the hydrolysis reaction kettle and the neutralization kettle are cooperatively used, and the hydrolysis reaction is refined, so that the problem of poor material reaction effect caused by large temperature difference between alkali addition reaction and acid addition neutralization reaction is avoided, and the hydrolysis reaction efficiency and the product quality and yield are improved.

Description

Technical Field

[0001] The utility model relates to the technical field of chemical production equipment, in particular to a 2,4-difluoronitrobenzene hydrolysis reaction device. Background Art

[0002] 2,4-Difluoronitrobenzene is a light yellow transparent liquid at room temperature and pressure. It is insoluble in water but soluble in common organic solvents. As an important organic compound, 2,4-difluoronitrobenzene has shown broad application prospects in many fields such as medicine, pesticides, liquid crystal materials and analytical reagents. 2,4-Difluoronitrobenzene can be used as an intermediate in organic synthesis and pharmaceutical chemistry, and is mostly used in the synthesis of drug molecules and bioactive molecules, such as a reactant for the preparation of 4-thiazolidinone derivatives as antibacterial agents, and as an intermediate for the drug flubendiamide. 2,4-Difluoronitrobenzene can also be used as a dye intermediate, participating in the synthesis of a series of brightly colored and stable dyes, providing important raw materials for the textile, printing and other industries.

[0003] When 2,4-difluoronitrobenzene is used as a production raw material, it needs to be hydrolyzed. Its hydrolysis product 5-fluoro-2-nitrophenol is also an organic compound widely used in the fields of medicine, dyes, pesticides, synthetic resins, etc. At present, the hydrolysis reaction of 2,4-difluoronitrobenzene is carried out in a hydrolysis reactor and is carried out under a high temperature environment. The hydrolysis reaction often requires the addition of alkali to react first, and then the addition of acid to neutralize it. The temperature and reaction system environment required for the alkali reaction and the acid neutralization reaction are different. When the existing hydrolysis reactor is used, its heating / cooling temperature adjustment method is limited, resulting in the inability to conduct heat to the reaction materials in time, and it is also easy to cause the reaction heat to be unable to be transferred out of the hydrolysis reactor in time, which is easy to cause the temperature in the hydrolysis reactor to be adjusted in time, the material reaction is uneven, and the controllability of the hydrolysis reaction is poor, which leads to an increase in by-products, affecting the product quality and yield, and at the same time resulting in low hydrolysis efficiency, poor reaction effect, and reduced production efficiency. Utility Model Content

[0004] The utility model provides a 2,4-difluoronitrobenzene hydrolysis reaction device, which is used to solve the problems that the existing hydrolysis reaction uses a hydrolysis reactor, resulting in limited temperature adjustment methods, untimely temperature adjustment in the hydrolysis reactor, uneven material reaction, and poor reaction controllability, thereby increasing by-products, affecting product quality and yield, and simultaneously resulting in low hydrolysis efficiency, thereby reducing production efficiency.

[0005] The utility model provides a hydrolysis reaction device for 2,4-difluoronitrobenzene, comprising: a hydrolysis reaction kettle and a neutralization kettle; the material inlet of the hydrolysis reaction kettle is respectively connected with the outlets of a water washing water transfer tank and a raw material tank, the alkali inlet of the hydrolysis reaction kettle is connected with the outlet of an alkali metering pump, and the acid inlet of the hydrolysis reaction kettle is connected with the outlet of an acid storage tank through an acid metering pump; the material outlet of the hydrolysis reaction kettle is connected with the inlet of the neutralization kettle, and the acid neutralization inlet of the neutralization kettle is connected with the outlet of the acid metering pump through a pipeline; the lower layer outlet of the neutralization kettle is connected with a wastewater treatment unit, and the upper layer outlet of the neutralization kettle is connected with the inlet of a water washing kettle; the lower layer outlet of the water washing kettle is connected with the inlet of the water washing water transfer tank, and the upper layer outlet of the water washing kettle is connected with the inlet of a preheating kettle; the outlet of the preheating kettle is connected with the inlet of a thin film evaporator through a pipeline heater, the product outlet of the thin film evaporator is connected with a product receiving tank, and the remaining material outlet of the thin film evaporator is connected with a heavy component receiving kettle.

[0006] Preferably, the inlet of the alkali metering pump is connected with the outlet of an alkali transfer kettle, the inlet of the alkali transfer kettle is connected with the outlet of an alkali preparation kettle, and the inlet of the alkali preparation kettle is respectively connected with the outlets of an alkali preparation water tank and a tube chain conveyor.

[0007] Preferably, the hydrolysis reaction kettle comprises a kettle body, the top of the kettle body is connected with a kettle cover, the kettle cover is respectively provided with a material inlet, an alkali inlet and an acid inlet, and the bottom of the kettle body is provided with a material outlet; the alkali inlet and the acid inlet are respectively connected with an alkali inlet pipe and an acid inlet pipe inside the kettle body, and Tesla valves corresponding to the alkali inlet and the acid inlet are arranged in both the alkali inlet pipe and the acid inlet pipe; a heat exchange jacket is further arranged on the outer side of the kettle body; a thermometer and a pH meter are also arranged in the kettle body; a stirring mechanism is further arranged in the hydrolysis reaction kettle.

[0008] Preferably, a plurality of heat exchange fins are arranged on the inner wall of the kettle body, the cross-sectional shape of the heat exchange fins is set as a sector, and the apex angles of the sector heat exchange fins all point to the vertical central axis of the kettle body.

[0009] Preferably, the stirring mechanism comprises a fixed cover arranged on the kettle cover, a motor is arranged on one side of the fixed cover, and the output end of the motor is fixedly connected with a first bevel gear arranged on one side inside the fixed cover; a second bevel gear is arranged above the first bevel gear, and a third bevel gear is arranged below the first bevel gear. The second bevel gear and the third bevel gear are respectively meshed and connected with the first bevel gear; the second bevel gear and the third bevel gear are both rotatably connected with the inner wall of the fixed cover; a rotating rod is connected below the second bevel gear, and the rotating rod penetrates through the center position of the third bevel gear; a rotating shaft is connected below the third bevel gear, and the rotating shaft is sleeved on the outer side of the rotating rod; both the rotating rod and the rotating shaft penetrate through the bottom wall of the fixed cover and the kettle cover and extend into the kettle body, and a plurality of stirring paddles are arranged on the outer sides of the rotating rod and the rotating shaft.

[0010] Preferably, the length of the rotating rod is greater than the length of the rotating shaft, and the bottom of the rotating shaft is rotatably and sealingly connected with the outer side of the rotating rod.

[0011] Preferably, a first spiral blade is arranged above the stirring paddle of the rotating rod, and the first spiral blade is used to drive the materials above to move downward.

[0012] Preferably, a second spiral blade is arranged below the stirring paddle of the rotating rod, and the second spiral blade is used to drive the materials below to move upward.

[0013] The 2,4-difluoronitrobenzene hydrolysis reaction device provided by the present utility model cooperatively uses a hydrolysis reaction kettle and a neutralization kettle to refine the hydrolysis reaction operation. The hydrolysis reaction kettle and the neutralization kettle are used to distinguish and separately control the temperature, reaction system environment, etc. required for the alkali addition reaction and the acid addition neutralization reaction, so that the adjustability and controllability of the hydrolysis reaction are increased, and the hydrolysis reaction can operate more safely and stably. It avoids the problems of poor material reaction effect and increased by-products caused by untimely temperature adjustment in the hydrolysis reaction kettle and large temperature difference between the alkali addition reaction and the acid addition neutralization reaction, thereby improving the product quality and yield, as well as the hydrolysis reaction efficiency and production efficiency.

[0014] By arranging heat exchange fins in the hydrolysis reaction kettle of the device, the heat transfer efficiency and heat utilization rate are improved, the problem of local high temperature in the reaction system is solved, and the material reaction is more uniform, thereby improving the hydrolysis efficiency and product quality.

[0015] The stirring mechanism in the hydrolysis reaction kettle uses rotating rods and rotating rods with opposite rotation directions to intensify the turbulence degree inside the materials, so that the materials can be mixed more uniformly, the reaction rate is increased, and the heat transfer between the materials can also be accelerated, improving the problem of uneven temperature distribution inside the materials. At the same time, a first spiral blade and a second spiral blade are arranged on the rotating rod and the rotating rod, strengthening the mass transfer and heat transfer efficiency of the materials in the vertical direction, improving the hydrolysis reaction efficiency and heat conduction efficiency, and being beneficial to improving the hydrolysis reaction effect. Description of the Drawings

[0016] In order to more clearly illustrate the technical solutions in the embodiments of the present utility model or the prior art, the following will briefly introduce the drawings required for use in the description of the embodiments or the prior art. Obviously, the drawings in the following description are some embodiments of the present utility model. For those of ordinary skill in the art, other drawings can be obtained based on these drawings without creative efforts.

[0017] Figure 1 It is a schematic structural diagram of a 2,4-difluoronitrobenzene hydrolysis reaction device provided by an embodiment of the present utility model;

[0018] Figure 2 It is a schematic structural diagram of a hydrolysis reaction kettle provided by an embodiment of the present utility model;

[0019] Figure 3 A schematic plan view of a heat exchange fin provided by an embodiment of the present utility model;

[0020] Figure 4 A schematic structural view of a stirring mechanism provided by an embodiment of the present utility model.

[0021] Explanation of reference numerals:

[0022] 1 - hydrolysis reaction kettle, 2 - neutralization kettle, 3 - raw material tank, 4 - water washing water transfer tank, 5 - acid storage tank, 6 - product receiving tank, 7 - heavy component receiving kettle, 11 - material inlet, 12 - alkali inlet, 13 - acid inlet, 14 - material outlet, 15 - kettle body, 16 - kettle cover, 17 - heat exchange jacket, 51 - acid metering pump, 81 - water washing kettle, 82 - preheating kettle, 83 - pipeline heater, 84 - thin film evaporator, 91 - alkali metering pump, 92 - alkali transfer kettle, 93 - alkali preparation kettle, 94 - tube chain conveyor, 95 - alkali preparation water tank, 121 - alkali inlet pipe, 122 - Tesla valve, 131 - acid inlet pipe, 171 - heat exchange fin, 181 - fixing cover, 182 - motor, 183 - first bevel gear, 184 - second bevel gear, 185 - third bevel gear, 186 - stirring paddle, 1841 - rotating rod, 1842 - second helical blade, 1851 - rotating rod, 1852 - first helical blade. Detailed implementation manners

[0023] To make the objectives, technical solutions, and advantages of the embodiments of the present utility model clearer, the technical solutions in the embodiments of the present utility model will be described clearly and completely below. Apparently, the described embodiments are some, but not all, of the embodiments of the present utility model. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present utility model without creative efforts also belong to the scope of protection of the present utility model.

[0024] Embodiment 1

[0025] As Figure 1 and Figure 2, a hydrolysis reaction device for 2,4-difluoronitrobenzene provided by the utility model includes a hydrolysis reaction kettle 1 and a neutralization kettle 2; the material inlet 11 of the hydrolysis reaction kettle 1 is respectively connected to the outlets of the water washing water transfer tank 4 and the raw material tank 3, the alkali inlet 12 of the hydrolysis reaction kettle 1 is connected to the outlet of the alkali metering pump 91, and the acid inlet 13 of the hydrolysis reaction kettle 1 is connected to the outlet of the acid storage tank 5 through the acid metering pump 51; the material outlet 14 of the hydrolysis reaction kettle 1 is connected to the inlet of the neutralization kettle 2, and the acid neutralization inlet of the neutralization kettle 2 is connected to the outlet of the acid metering pump 51 through a pipeline; the lower layer outlet of the neutralization kettle 2 is connected to the wastewater treatment unit, and the upper layer outlet of the neutralization kettle 2 is connected to the inlet of the water washing kettle 81; the lower layer outlet of the water washing kettle 81 is connected to the inlet of the water washing water transfer tank 4, and the upper layer outlet of the water washing kettle 81 is connected to the inlet of the preheating kettle 82; the outlet of the preheating kettle 82 is connected to the inlet of the thin film evaporator 84 through the pipeline heater 83, the product outlet of the thin film evaporator 84 is connected to the product receiving tank 6, and the remaining material outlet of the thin film evaporator 84 is connected to the heavy component receiving kettle 7.

[0026] When hydrolyzing 2,4-difluoronitrobenzene, 2,4-difluoronitrobenzene and water are respectively added into the hydrolysis reaction kettle 1 through the raw material tank 3 and the water washing water transfer tank 4, and then the temperature is heated up to 60 °C. The pre-prepared potassium hydroxide solution is pumped in by the alkali metering pump 91, and the temperature in the hydrolysis reaction kettle 1 is controlled at 60-65 °C during the dropping of the potassium hydroxide solution. After the dropping is completed, it is kept warm for 1 h. After the heat preservation is completed, the temperature is controlled at 55-65 °C and hydrochloric acid is dropped through the acid metering pump 51 to adjust the pH value of the material to 7. Then the material is transferred to the neutralization kettle 2, and hydrochloric acid is continuously pumped in to adjust the pH value of the material to 2-3. Stir for 0.5 h, stand for 0.5 h, and layer. The lower saline layer goes to the wastewater treatment unit to recover potassium salts, and the upper organic layer is transferred to the water washing kettle 81. Water is added and the temperature is controlled at 40-50 °C. Stir for 0.5 h, stand for 0.5 h, and layer. The lower layer of water is transferred into the water washing water transfer tank 4 and reused in the hydrolysis reaction kettle 1, and the upper organic layer is transferred into the preheating kettle 82. It is preheated to 60-85 °C in the preheating kettle 82, and then continuously heated to 90-140 °C through the pipeline heater 83 and enters the thin film evaporator 84. The product is removed and enters the product receiving tank 6, and the remaining material of the thin film evaporator 84 enters the heavy component receiving kettle 7.

[0027] This device uses the hydrolysis reaction kettle 1 and the neutralization kettle 2 in cooperation to refine the hydrolysis reaction operation. The hydrolysis reaction kettle 1 and the neutralization kettle 2 are used to distinguish and separately control the temperature, reaction system environment, etc. required for the alkali addition reaction and the acid addition and neutralization reaction, increasing the adjustability and controllability of the hydrolysis reaction, enabling the hydrolysis reaction to operate more safely and stably, and avoiding problems such as poor material reaction effect and increased by-products caused by untimely temperature adjustment in the hydrolysis reaction kettle 1 and large temperature difference between the alkali addition reaction and the acid addition and neutralization reaction. Thereby, the product quality and yield are improved, and the hydrolysis reaction efficiency and production efficiency are also increased.

[0028] As Figure 1 , preferably, the inlet of the alkali metering pump 91 is connected to the outlet of the alkali intermediate kettle 92, the inlet of the alkali intermediate kettle 92 is connected to the outlet of the alkali preparation kettle 93, and the inlets of the alkali preparation kettle 93 are respectively connected to the alkali preparation water tank 95 and the outlet of the tube chain conveyor 94. The alkali used in the alkali addition reaction needs to be prepared into an alkali solution in advance and then quantitatively added dropwise to the hydrolysis reaction kettle 1, otherwise it is easy to cause the local temperature to not reach the standard and affect the hydrolysis process. Therefore, taking the potassium hydroxide solution as an example, before the reaction starts, water from the alkali preparation water tank 95 is first added to the alkali preparation kettle 93. After starting the stirring, the potassium hydroxide is quantitatively input into the alkali preparation kettle 93 by the tube chain conveyor 94, and the temperature is controlled ≤85°C and stirred. After the feeding is completed, the material is transferred to the alkali intermediate kettle 92, and stirring is continued, and the temperature is controlled between 55 - 65°C. After all the potassium hydroxide is dissolved, the prepared potassium hydroxide solution is obtained for use.

[0029] Example 2

[0030] Based on the above embodiment, this embodiment further includes: As Figure 2 , the hydrolysis reaction kettle 1 includes a kettle body 15, the top of the kettle body 15 is connected with a kettle cover 16, and a material inlet 11, an alkali inlet 12, and an acid inlet 13 are respectively opened on the kettle cover 16. A material outlet 14 is opened at the bottom of the kettle body 15; the alkali inlet 12 and the acid inlet 13 are respectively connected to an alkali inlet pipe 121 and an acid inlet pipe 131 inside the kettle body 15, and Tesla valves 122 corresponding to the alkali inlet 12 and the acid inlet 13 are arranged in both the alkali inlet pipe 121 and the acid inlet pipe 131; a heat exchange jacket 17 is further arranged outside the kettle body 15; a thermometer and a pH meter (conventional settings, not shown in the drawings) are also arranged in the kettle body 15; a stirring mechanism is further arranged in the hydrolysis reaction kettle 1.

[0031] In actual application, the heat exchange jacket 17 of the hydrolysis reaction kettle 1 is connected to an external hot water or cold water supply device, so as to heat, cool, or keep warm the material inside the kettle body 15. Coils and other devices can also be arranged in the heat exchange jacket 17 according to production needs to provide the temperatures at each stage of the hydrolysis reaction, reduce the time required for hydrolysis, and improve production efficiency. The thermometer in the kettle body 15 can monitor and feedback the temperature of the material in real time, facilitating temperature control adjustment, and the pH meter can monitor the pH value of the material, which has a guiding nature for the kettle transfer operation in the acid addition and neutralization reaction. The stirring mechanism can stir and mix the material in the kettle body 15, promote the reaction, facilitate heat transfer, and at the same time prevent the reaction heat from being concentratedly generated, reducing the generation of high-temperature side reactions.

[0032] An alkali inlet pipe 121 is connected to the alkali inlet 12 of the hydrolysis reactor 1, and an acid inlet pipe 131 is connected to the acid inlet 13. Tesla valves 122 are provided in the alkali inlet pipe 121 and the acid inlet pipe 131. The structure of the Tesla valves 122 enables the alkali or acid to enter the materials in the kettle body 15 at a lower rate when adding alkali and acid, controlling the input rate of the alkali or acid, providing a certain flexible space for temperature regulation, facilitating the stable progress of the reaction, improving the hydrolysis safety, and also being conducive to improving the product quality and yield.

[0033] Such as Figure 3 , preferably, a plurality of heat exchange fins 171 are provided on the inner wall of the kettle body 15. The cross-sectional shape of the heat exchange fins 171 is set as a sector, and the apex angles of the sector heat exchange fins 171 all point to the vertical central axis of the kettle body 15. In order to improve the heat exchange efficiency and effect, heat exchange fins 171 are provided on the inner wall of the kettle body 15. When the heat in the heat exchange jacket 17 is conducted to the inner wall of the kettle body 15, it is not only conducted through the materials in contact with the inner wall of the kettle body 15, but also through the heat transfer by first conducting to the heat exchange fins 171 and then to the materials not in contact with the inner wall of the kettle body 15. The same conduction principle applies during cooling. Through the heat exchange fins 171, the heat transfer efficiency and heat utilization rate can be improved, the problem of local high temperature in the reaction system can be solved, the materials can react more evenly, and thus the hydrolysis efficiency and product quality can be improved. The arc-shaped sides of the sector heat exchange fins 171 have a large contact area with the inner wall of the kettle body 15, and the two radius sides of the sector can also increase the contact area with the materials, improving the heat exchange efficiency. Moreover, the heat exchange fins 171 are detachably installed on the inner wall of the kettle body 15 and are prevented from contacting the stirring mechanism. Of course, the heat exchange fins 171 can also use other common shapes in the field (such as square, triangular, etc.).

[0034] Example 3

[0035] Based on the above embodiments, this embodiment further includes: Such as Figure 4, the stirring mechanism includes a fixed cover 181 provided on the kettle cover 16. One side of the fixed cover 181 is provided with a motor 182, and the output end of the motor 182 is fixedly connected to a first bevel gear 183 provided on one side inside the fixed cover 181; above the first bevel gear 183 is provided a second bevel gear 184, and below the first bevel gear 183 is provided a third bevel gear 185. The second bevel gear 184 and the third bevel gear 185 are respectively meshed and connected with the first bevel gear 183; the second bevel gear 184 and the third bevel gear 185 are both rotatably connected to the inner wall of the fixed cover 181; below the second bevel gear 184 is connected a rotating rod 1841, and the rotating rod 1841 penetrates through the center position of the third bevel gear 185; below the third bevel gear 185 is connected a rotating rod 1851, and the rotating rod 1851 is sleeved outside the rotating rod 1841; the rotating rod 1841 and the rotating rod 1851 both penetrate through the bottom wall of the fixed cover 181 and the kettle cover 16 and extend into the kettle body 15, and a plurality of stirring paddles 186 are provided on the outside of the rotating rod 1841 and the rotating rod 1851.

[0036] In order to improve the stirring efficiency of the stirring mechanism and the material mixing effect, a second bevel gear 184 and a third bevel gear 185 are respectively meshed and connected above and below the first bevel gear 183, so that the rotation directions of the second bevel gear 184 and the third bevel gear 185 are opposite. Thus, while respectively driving the rotating rod 1841 and the rotating rod 1851 to rotate, the rotation directions of the rotating rod 1841 and the rotating rod 1851 are also opposite, driving the stirring paddles 186 thereon to rotate in the reverse direction. Furthermore, the materials inside the kettle body 15 also receive a reverse stirring force, intensifying the turbulence degree inside the materials, making the materials mix more evenly, improving the reaction rate, and also enabling the heat transfer between the materials to be accelerated, and improving the problem of uneven temperature distribution inside the materials.

[0037] The styles of the stirring paddles 186 on the rotating rod 1841 and the rotating rod 1851 can be the same or different. The specific styles of the stirring paddles 186 are not limited herein, which belong to the conventional settings in the art and can meet the stirring requirements. They can be selected and designed by those skilled in the art.

[0038] Preferably, the length of the rotating rod 1841 is greater than that of the rotating lever 1851, and the bottom of the rotating lever 1851 is rotationally and sealingly connected to the outer side of the rotating rod 1841. Since the rotating rod 1841 is sleeved inside the rotating lever 1851, the length of the rotating rod 1841 should be greater than that of the rotating lever 1851 so that its lower part can extend below the bottom of the rotating lever 1851, facilitating the separate rotation of the rotating rod 1841 and the rotating lever 1851. In addition, in order to prevent materials from entering the gap between the rotating rod 1841 and the rotating lever 1851, a rotational sealing structure (such as a rotating sealing ring, a common device in the art) is used to sealingly connect the bottom of the rotating lever 1851 to the outer side of the rotating rod 1841.

[0039] Example 4

[0040] Based on the above embodiments, this embodiment further includes: as Figure 4 , above the stirring paddle 186 of the rotating lever 1851, a first spiral blade 1852 is provided, and the first spiral blade 1852 is used to drive the materials above downward. The stirring paddle 186 of a conventional stirring mechanism can only rotate and stir the materials inside the kettle body 15 in the horizontal direction, and its mixing effect is slightly lacking. Therefore, by providing the first spiral blade 1852 on the rotating lever 1851, the materials above the rotating lever 1851 and in the upper part of the kettle body 15 can be guided and mixed downward, increasing the mixing degree of the materials in the vertical direction, which is beneficial to improving the hydrolysis reaction effect.

[0041] As Figure 4 , preferably, below the stirring paddle 186 of the rotating rod 1841, a second spiral blade 1842 is provided, and the second spiral blade 1842 is used to drive the materials below upward. For the same purpose, the second spiral blade 1842 can guide and mix the materials below the rotating rod 1841 and in the lower part of the kettle body 15 upward, increasing the mixing degree of the materials in the vertical direction, which is beneficial to improving the hydrolysis reaction effect. By the combined action of the first spiral blade 1852 and the second spiral blade 1842, the materials in the upper and bottom parts of the kettle body 15 move downward and upward respectively, strengthening the mass transfer and heat transfer efficiency of the materials in the vertical direction, improving the hydrolysis reaction efficiency and heat conduction efficiency, and being beneficial to improving the hydrolysis reaction effect.

[0042] In summary, for the 2,4-difluoronitrobenzene hydrolysis reaction device of the present utility model, during specific operation, first, water from the alkali preparation water tank 95 is added to the alkali preparation kettle 93. After starting the stirring, potassium hydroxide is quantitatively input into the alkali preparation kettle 93 by the tube chain conveyor 94, the temperature is controlled ≤ 85°C and stirred. After the feeding is completed, the materials are transferred to the alkali intermediate kettle 92, and stirring is continued, and the temperature is controlled between 55 - 65°C. After all the potassium hydroxide is dissolved, the prepared potassium hydroxide solution is obtained for later use.

[0043] Add 2,4-difluoronitrobenzene and water into the hydrolysis reactor 1 through the raw material tank 3 and the water washing intermediate tank 4 respectively. Start the stirring mechanism, and heat up the hydrolysis reactor 1 through the heat exchange jacket 17 and the heat exchange fins 171 on the inner wall of the reactor body 15. Heat up to 60 °C, pump in the pre-prepared potassium hydroxide solution with the alkali metering pump 91, and drip the potassium hydroxide solution into the reactor body 15 through the Tesla valve 122 of the alkali inlet pipe 121. During the dripping of the potassium hydroxide solution, control the temperature in the hydrolysis reactor 1 at 60-65 °C. After the dripping is completed, keep warm for 1 h. After the heat preservation is over, control the temperature through the heat exchange jacket 17 and the heat exchange fins 171, control the temperature at 55-65 °C, and drip hydrochloric acid into the reactor body 15 through the acid metering pump 51 and the Tesla valve 122 of the acid inlet pipe 131 to adjust the pH value of the material to 7. Then transfer the material to the neutralization reactor 2, and continue to pump in hydrochloric acid to adjust the pH value of the material to 2-3. Stir for 0.5 h, stand for 0.5 h, and separate the layers. The lower saline water layer goes to the wastewater treatment unit to recover potassium salts. The upper organic layer is transferred to the water washing kettle 81, add water and control the temperature at 40-50 °C, stir for 0.5 h, stand for 0.5 h, and separate the layers. The lower layer of water is transferred into the water washing intermediate tank 4 and recycled to the hydrolysis reactor 1. The upper organic layer is transferred into the preheating kettle 82. Preheat to 60-85 °C in the preheating kettle 82, and then continue to heat to 90-140 °C through the pipeline heater 83, enter the thin film evaporator 84, the product is stripped out and enters the product receiving tank 6, and the remaining material in the thin film evaporator 84 enters the heavy component receiving kettle 7.

[0044] When the stirring mechanism of the hydrolysis reactor 1 is working, the motor 182 drives the first bevel gear 183 to rotate. The first bevel gear 183 drives the second bevel gear 184 and the third bevel gear 185 to rotate in the opposite direction through meshing. Correspondingly, the rotating rod 1841 and the rotating rod 1851 are also driven to rotate in the opposite direction, driving the stirring paddle 186 thereon to rotate in the opposite direction, so that the material inside the reactor body 15 also receives an opposite stirring force, intensifying the turbulence degree inside the material. At the same time, the first spiral blade 1852 and the second spiral blade 1842 arranged on the rotating rod 1841 and the rotating rod 1851 make the materials located at the upper and bottom inside the reactor body 15 move downward and upward respectively, strengthening the mass transfer and heat transfer efficiency of the material in the vertical direction, improving the hydrolysis reaction efficiency and heat conduction efficiency, and enhancing the hydrolysis reaction effect.

[0045] It should be noted that in the present utility model, the detailed structures of some devices are not described in detail, but belong to the prior art known to those skilled in the art, so they will not be elaborated here. In addition, the parts not involved in this device are the same as the prior art or can be implemented by using the prior art.

[0046] It should be noted that pressure sensors, flow meters or temperature sensors are provided on the conveying pipelines inside the device between different units and equipment, and different valves are also provided, such as pressure relief valves, pressure regulating valves, safety valves, etc., which are used to adjust and stabilize the pressure of the entire system.

[0047] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than limiting it; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that they can still modify the technical solutions described in the foregoing embodiments, or perform equivalent replacements on some or all of the technical features; and these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A hydrolysis reaction device for 2,4-difluoronitrobenzene, characterized in that, Including: A hydrolysis reactor and a neutralization kettle; the material inlet of the hydrolysis reactor is respectively connected to the outlets of the water washing intermediate tank and the raw material tank, the alkali inlet of the hydrolysis reactor is connected to the outlet of the alkali metering pump, and the acid inlet of the hydrolysis reactor is connected to the outlet of the acid storage tank through the acid metering pump; the material outlet of the hydrolysis reactor is connected to the inlet of the neutralization kettle, and the acid neutralization inlet of the neutralization kettle is connected to the outlet of the acid metering pump through a pipeline; the lower layer outlet of the neutralization kettle is connected to the wastewater treatment unit, and the upper layer outlet of the neutralization kettle is connected to the inlet of the water washing kettle; the lower layer outlet of the water washing kettle is connected to the inlet of the water washing intermediate tank, and the upper layer outlet of the water washing kettle is connected to the inlet of the preheating kettle; the outlet of the preheating kettle is connected to the inlet of the thin film evaporator through a pipeline heater, the product outlet of the thin film evaporator is connected to the product receiving tank, and the residue outlet of the thin film evaporator is connected to the heavy component receiving kettle.

2. The 2,4-difluoronitrobenzene hydrolysis reaction device according to claim 1, characterized in that, The inlet of the alkali metering pump is connected to the outlet of the alkali intermediate kettle, the inlet of the alkali intermediate kettle is connected to the outlet of the alkali preparation kettle, and the inlet of the alkali preparation kettle is respectively connected to the outlets of the alkali preparation water tank and the tube chain conveyor.

3. The 2,4-difluoronitrobenzene hydrolysis reaction device according to claim 1 or 2, characterized in that, The hydrolysis reactor includes a kettle body, the top of the kettle body is connected with a kettle cover, the kettle cover is respectively provided with a material inlet, an alkali inlet and an acid inlet, and the bottom of the kettle body is provided with a material outlet; the alkali inlet and the acid inlet are respectively connected to the alkali inlet pipe and the acid inlet pipe inside the kettle body, and Tesla valves corresponding to the alkali inlet and the acid inlet are arranged in both the alkali inlet pipe and the acid inlet pipe; a heat exchange jacket is also arranged outside the kettle body; a thermometer and a pH meter are also arranged in the kettle body; a stirring mechanism is also arranged in the hydrolysis reactor.

4. The 2,4-difluoronitrobenzene hydrolysis reaction device according to claim 3, characterized in that, A plurality of heat exchange fins are arranged on the inner wall of the kettle body, the cross-sectional shape of the heat exchange fins is set as a sector, and the top angles of the fan-shaped heat exchange fins all point to the vertical central axis of the kettle body.

5. The 2,4-difluoronitrobenzene hydrolysis reaction device according to claim 3, wherein The stirring mechanism includes a fixed cover arranged on the kettle cover, a motor is arranged on one side of the fixed cover, and the output end of the motor is fixedly connected with a first bevel gear arranged on one side inside the fixed cover; a second bevel gear is arranged above the first bevel gear, and a third bevel gear is arranged below the first bevel gear, and the second bevel gear and the third bevel gear are respectively meshed and connected with the first bevel gear; the second bevel gear and the third bevel gear are both rotatably connected to the inner wall of the fixed cover; a rotating rod is connected below the second bevel gear, and the rotating rod penetrates through the center position of the third bevel gear; a rotating shaft is connected below the third bevel gear, and the rotating shaft is sleeved outside the rotating rod; both the rotating rod and the rotating shaft penetrate through the bottom wall of the fixed cover and the kettle cover and extend into the kettle body, and a plurality of stirring paddles are arranged on the outer sides of the rotating rod and the rotating shaft.

6. The 2,4-difluoronitrobenzene hydrolysis reaction device according to claim 5, wherein, The length of the rotating rod is greater than the length of the rotating shaft, and the bottom of the rotating shaft is rotationally and hermetically connected to the outside of the rotating rod.

7. The 2,4-difluoronitrobenzene hydrolysis reaction device according to claim 5, characterized in that, A first spiral blade is arranged above the stirring paddle of the rotating shaft, and the first spiral blade is used to drive the material above to move downward.

8. The 2,4-difluoronitrobenzene hydrolysis reaction device according to claim 5, characterized in that, A second spiral blade is arranged below the stirring paddle of the rotating rod, and the second spiral blade is used to drive the materials below to move upward.

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