A full-process precipitation crystallization device for bromine substances

By using two distillation tanks and stirring racks to rotate in the bromine-based substance precipitation and crystallization device, combined with steam heating and heat recovery technology, the problems of long process time and low heat utilization efficiency in traditional methods are solved, and the process flow is shortened and the energy is efficiently utilized.

CN120022630BActive Publication Date: 2025-07-22SHANDONG HAIWANG CHEM
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Patent Information

Application Number
CN202510459879.4
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-04-14
Publication Date
2025-07-22
Estimated Expiration
2045-04-14

AI Technical Summary

Technical Problem

During the precipitation and crystallization process of traditional bromine substances, the process time is long and the heat utilization efficiency is low, resulting in a large amount of energy consumption.

Method used

Using a device including two distillation tanks, the mixing rack rotation and steam heating are combined, using the flow and heat recovery technology of the mixed liquid to shorten the process flow and excess heat is recovered.

Benefits of technology

The process flow time has been successfully shortened, the heat recovery and utilization have been realized, and the energy utilization efficiency has been improved.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention belongs to the field of substance precipitation and crystallization, and specifically relates to a full-process precipitation and crystallization device for bromine-based substances, including two distillation tanks. A pre-storage tank is arranged between the two distillation tanks. A rotatable stirring frame is arranged in the distillation tank. A raw material pipe communicated with the stirring frame is arranged outside the distillation tank. A drain pipe communicated with the stirring frame is also arranged outside the distillation tank. The drain pipe is communicated with the pre-storage tank. A suction pipe is fixedly connected to the bottom of the pre-storage tank. The suction pipe is communicated with the inside of the distillation tank. A discharge valve is installed at the bottom of the distillation tank. An electric heating control box is installed outside the pre-storage tank. Through this setting, the heating and fusion of the mixed liquid and the heating and evaporation process of the mixed liquid are effectively combined, successfully shortening the time consumed by the process flow. At the same time, half of the heating process utilizes the excess heat that could only be dissipated outward originally, achieving the effect of energy recovery and utilization.
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Description

Technical Field

[0001] The invention belongs to the field of substance precipitation crystallization, and specifically is a full-process precipitation crystallization device for bromine-based substances. Background Art

[0002] Bromine-based substances mainly include bromine element and its compounds, such as bromides such as sodium bromide, potassium bromide, hydrogen bromide and its derivatives.

[0003] In the traditional production process of bromine-based substances, the final product is generally obtained by precipitation and crystallization. For example, bromotriazine needs to be first obtained through a synthesis reaction to obtain a crude product of bromotriazine, and then the crude product is washed with alkali and acid to remove impurities in the crude product, such as tribromophenol and hydrochloride. After that, the treated crude product and the solvent are placed in a heating tank for mixing and heating. The solvent is generally toluene or chlorobenzene to ensure that the crude product is completely dissolved. After that, the mixed solution is added to an evaporator for heating to remove the organic solvent in the mixed solution, and finally the temperature is slowly lowered to precipitate the finished product.

[0004] In the traditional precipitation process, the crude product needs to be heated first, then placed in an evaporation container for heating and stirring, and finally the finished product is cooled to room temperature or lower. The two processes are separated from each other, resulting in a longer time for the entire process, and a lot of heat is lost in the process, resulting in more energy consumption in the overall process.

[0005] To this end, the present invention provides a full-process precipitation and crystallization device for bromine-based substances. Summary of the invention

[0006] In order to make up for the deficiencies of the prior art, at least one technical problem raised in the background technology is solved.

[0007] The technical solution adopted by the present invention to solve the technical problem is as follows: a full-process precipitation crystallization device for bromine-based substances according to the present invention comprises two distillation tanks, a pre-storage tank is arranged between the two distillation tanks, a rotatable stirring rack is arranged in the distillation tank, a raw material pipe connected to the stirring rack is arranged on the outside of the distillation tank, a liquid discharge pipe connected to the stirring rack is also arranged on the outside of the distillation tank, the liquid discharge pipe is connected to the pre-storage tank, a suction pipe is fixedly connected to the bottom of the pre-storage tank, the suction pipe is connected to the inside of the distillation tank, a discharge valve is installed at the bottom of the distillation tank, and an electric heating control box is installed on the outside of the pre-storage tank;

[0008] By setting up two distillation tanks, the crude product that has just been pickled is injected into the stirring rack, and the solvent is also injected into the stirring rack. At this time, the mixed liquid 1 is at room temperature, and the first distillation tank still stores the previous mixed liquid 2. Steam is introduced into the inner wall of the distillation tank for heating, and the mixed liquid inside the distillation tank is heated. At the same time, the stirring rack is rotated and stirred to ensure that the temperature of the mixed liquid inside the distillation tank is uniform. At this time, the room temperature mixed liquid 1 fills the stirring rack and is in a state of continuous flow, and the heated mixed liquid 2 will continuously heat the mixed liquid 1, and the discharged mixed liquid 1 will enter the pre-storage tank. When the stirring and heating of the mixed liquid 2 in the distillation tank is completed, the steam heating is turned off, and the speed of the stirring rack is reduced. At this time, the distillation tank enters the cooling stage. At this time, as the room temperature mixed liquid 1 continuously flows into the stirring rack, the temperature of the mixed liquid 2 in the distillation tank can be taken away, and because the stirring rack is rotating, the mixed liquid 2 can be cooled at a uniform speed, and the heat is transferred to the mixed liquid 1. Since the mixed liquid 1 passes through the longer stirring rack and the stirring rack is in a state of continuous rotation, the mixed liquid 1 injected into the stirring rack at the same time The crude product and solvent of the mixing rack can be well mixed, and the heat that needs to be dissipated by the previous batch of mixed liquid 2 can be used to heat itself; by adjusting the rate at which the mixed liquid 1 is introduced into the stirring rack, when the mixed liquid 2 stops, the mixed liquid 1 is just discharged into the pre-storage tank, and then the mixed and heated mixed liquid 1 is injected into another distillation tank, and starts to heat and rotate, and at the same time, the third batch of mixed liquid is injected into the stirring rack of the distillation tank, while the first distillation tank is discharging the finished product at this time, waiting for the next injection of the mixed liquid. Through this setting, the heating, fusion and heating evaporation processes of the mixed liquid are effectively combined, and the time consumed by the process flow is successfully shortened. At the same time, half of the heating process utilizes the excess heat that can only be dissipated outward, realizing the energy recovery effect; the distillation tank and the pre-storage tank are both provided with temperature measurement modules to ensure accurate temperature control, and the inner wall of the pre-storage tank is provided with an electric heating module, which is regulated by the electric heating control box to ensure that the mixed liquid can maintain the temperature in the pre-storage tank to prevent the temperature from being too low, resulting in the problem of premature precipitation of the finished product.

[0009] Preferably, the stirring rack is composed of a plurality of split tubes, which are arranged equidistantly in a ring shape; a vertically arranged reduction motor is installed on the top of the distillation tank; the output end of the reduction motor is transmission-connected to the top of the stirring rack; the plurality of split tubes divide the mixed liquid evenly, and at the same time increase the contact area of the stirring rack, thereby improving the heat exchange effect; the mixed liquid is introduced into the split tubes in the following manner: the mixed liquid is connected to two of the split tubes, and the mixed liquid is injected into the split tubes from top to bottom; then the mixed liquid moves from bottom to top through the plurality of split tubes at the bottom, and finally is discharged outwardly from the drain pipe, thereby ensuring that the stirring rack is filled with the mixed liquid; the reduction motor drives the stirring rack to rotate stably.

[0010] Preferably, the pre-storage tank includes an upper mixing tank and a lower transfer tank that are connected to each other. The output end of the drain pipe is fixedly connected with a cutting-in pipe, and the cutting-in pipe is connected to the upper mixing tank. A switching valve is installed at the bottom of the upper mixing tank. The mixed liquid discharged from the stirring frame enters the upper mixing tank through the drain pipe and the cutting-in pipe. Since the cutting-in pipe is connected to the inner wall of the upper mixing tank at a vertical angle, the mixed liquid entering the upper mixing tank will flow and rotate along the upper mixing tank. In this way, the mixed liquid will continuously rotate and mix in the upper mixing tank. Because the subsequent mixed liquid will continuously input thrust, it ensures the full mixing of the crude product and the solvent in the mixed liquid. When it is necessary to output the mixed liquid in the pre-storage tank, first inject the mixed liquid into the lower transfer tank, and then increase the negative pressure in the distillation tank and cooperate with the suction pipe to suck the mixed liquid into the distillation tank.

[0011] Preferably, a plurality of heat conduction rods are fixedly connected to the bottom of the lower transfer tank, and the plurality of heat conduction rods are arranged in an annular and equidistant manner. Electric heating wires connected to the electric heating control box are arranged in the heat conduction rods. The mixed liquid injected subsequently may have the problem of insufficient temperature. The heat conduction rods can be used to raise the temperature of the mixed liquid in the lower transfer tank. At the same time, a water level measuring instrument is provided in the lower transfer tank to measure whether the amount of the transferred mixed liquid meets the standard. The plurality of heat conduction rods will produce obstruction, making the mixed liquid quickly return to stability, which is convenient for the measurement of the water level.

[0012] Preferably, a mixing ring one and a mixing ring two are arranged above the distillation tank. The raw material pipe is connected to the mixing ring two, and the drain pipe is connected to the mixing ring one. Both the mixing ring one and the mixing ring two are connected to the stirring frame. The raw material pipe injects the crude product and the solvent into the mixing ring two. The mixing ring two is connected to the stirring frame, thereby injecting the mixed liquid into it. The mixed liquid that fills the stirring frame and has undergone heat exchange finally enters the mixing ring one and finally discharges from the drain pipe.

[0013] Preferably, a connecting shaft is fixedly connected between the top of the stirring frame and the reduction motor. A clamping ring one and a clamping ring two are rotatably clamped on the outer side of the connecting shaft. The clamping ring one and the mixing ring one are connected by two connecting pipes, and the clamping ring two and the mixing ring two are also connected by two connecting pipes. A second connecting groove communicating with the clamping ring two is opened at the bottom of the connecting shaft, and a first connecting groove communicating with the clamping ring one is also opened at the bottom of the connecting shaft. The connecting shaft is used to transmit the kinetic energy of the reduction motor. The clamping ring one and the clamping ring two are rotatably clamped on the outer side of the connecting shaft. When the connecting shaft rotates, the two remain stationary and are supported and fixed by a plurality of connecting pipes. The input end of the stirring frame is connected to the clamping ring two, and the output end is connected to the clamping ring one, thereby completing the injection and output functions of the mixed liquid.

[0014] Preferably, a multi-way valve is fixedly connected to the top of the suction pipe. A plurality of liquid discharge holes are formed in the top of the multi-way valve. Transfer pipes are fixedly connected to the ends of the liquid discharge holes. A vertically arranged filter element is installed in the middle of the suction pipe. The transfer pipes are used to inject the mixed liquid into the distillation tank. The multi-way valve can communicate with a plurality of transfer pipes. The number of distillation tanks can be increased. It is also possible to use one pre-storage tank for multiple distillation tanks at the same time. Only the injection speed of the mixed liquid needs to be adjusted for coordination. The filter element is used to filter impurities in the mixed liquid to ensure the quality of the finished product.

[0015] Preferably, a feeding window is installed on the outer side of the distillation tank near the top. The middle part of the feeding window is made of transparent material. A communication valve communicating with the transfer pipe is fixedly connected to the rear end of the distillation tank. The feeding window is used to observe the internal situation of the distillation tank and can also be used to put solid materials. The communication valve is connected to the inside of the distillation tank to smoothly transfer the mixed liquid.

[0016] Preferably, a plurality of mixing arms are fixedly connected to the bottom of the stirring frame. The mixing arms are communicated with the stirring frame and are arranged in a bent shape. The mixing arms not only further increase the contact area of the stirring frame, but also expand the volume of the stirring frame, improving the stirring effect and the heat exchange effect.

[0017] Preferably, two heat transfer fins are fixedly connected inside the raw material pipe. The cross-section of the heat transfer fin is triangular. The heat transfer fins are arranged in a spiral shape. The heat transfer fins are used to increase the contact surface between the mixed liquid and the raw material pipe, further increasing the heat exchange effect. The spiral arrangement allows the mixed liquid to move spirally inside the raw material pipe, improving the mixing effect of the two raw materials in the mixed liquid.

[0018] The beneficial effects of the present invention are as follows:

[0019] 1. For the bromine-based substance full-process precipitation and crystallization device of the present invention, by setting two distillation tanks, the crude product just after pickling is injected into the stirring frame, and at the same time the solvent is also injected into the stirring frame. Through this setting, the heating, fusion of the mixed liquid, and the heating and evaporation process of the mixed liquid are effectively combined, successfully shortening the time consumed by the process flow. At the same time, half of the heating process utilizes the excess heat that could only be dissipated outward before, achieving the effect of energy recovery and utilization.

[0020] 2. For the bromine-based substance full-process precipitation and crystallization device of the present invention, a plurality of splitting pipes evenly divide the mixed liquid, and at the same time increase the contact area of the stirring frame to improve the heat exchange effect. The way the mixed liquid enters the splitting pipes is as follows: The mixed liquid is communicated with two of the splitting pipes, and the mixed liquid is injected into them from top to bottom. Then the mixed liquid moves from bottom to top through multiple splitting pipes at the bottom and finally is discharged out through the drain pipe, ensuring that the stirring frame is filled with the mixed liquid. The stirring frame is driven to rotate stably by a reduction motor. Description of the Drawings

[0021] The present invention will be further described below in conjunction with the accompanying drawings.

[0022] Figure 1 is a perspective view of the present invention;

[0023] Figure 2 is a perspective view of the pre-storage tank and the distillation tank of the present invention;

[0024] Figure 3 is a perspective view of the distillation tank of the present invention;

[0025] Figure 4 is a sectional view of the distillation tank of the present invention;

[0026] Figure 5 is a perspective view of the stirring frame of the present invention;

[0027] Figure 6 is a sectional view of the connecting shaft of the present invention;

[0028] Figure 7 is a perspective view of the raw material pipe of the present invention;

[0029] Figure 8 is a perspective view of the pre-storage tank of the present invention;

[0030] In the figure: 1, distillation tank; 2, pre-storage tank; 3, feeding window; 4, discharge valve; 5, stirring frame; 6, transfer pipe; 7, multi-way valve; 8, suction pipe; 9, filter element; 10, electric heating control box; 11, raw material pipe; 12, drain pipe; 13, mixing ring 1; 14, reduction motor; 15, mixing ring 2; 16, mixing arm; 17, splitting pipe; 18, connecting pipe; 19, clamping ring 1; 20, clamping ring 2; 21, connecting groove 2; 22, connecting groove 1; 23, connecting shaft; 24, heat transfer fin; 25, upper mixing tank; 26, lower transmission tank; 27, opening and closing valve; 28, heat conduction rod; 29, cutting-in pipe. Specific embodiments

[0031] In order to make the technical means, creative features, achieved purposes and effects of the present invention easy to understand, the present invention will be further described below in conjunction with specific embodiments.

[0032] Such as Figures 1 to 8As shown in the figure, a full-process precipitation crystallization device for bromine-based substances according to an embodiment of the present invention includes two distillation tanks 1. A pre-storage tank 2 is arranged between the two distillation tanks 1. A rotatable stirring frame 5 is arranged in the distillation tank 1. A raw material pipe 11 communicating with the stirring frame 5 is arranged outside the distillation tank 1. A drain pipe 12 communicating with the stirring frame 5 is also arranged outside the distillation tank 1. The drain pipe 12 is communicated with the pre-storage tank 2. A suction pipe 8 is fixedly connected to the bottom of the pre-storage tank 2. The suction pipe 8 is communicated with the inside of the distillation tank 1. A discharge valve 4 is installed at the bottom of the distillation tank 1. An electric heating control box 10 is installed outside the pre-storage tank 2.

[0033] By arranging two distillation tanks 1, the crude product just after pickling is injected into the stirring frame 5, and at the same time, the solvent is also injected into the stirring frame 5. At this time, the first mixed liquid is at room temperature, and the second mixed liquid from the previous batch is still stored in the first distillation tank 1. Steam is introduced into the inner wall of the distillation tank 1 for heating to raise the temperature of the mixed liquid inside the distillation tank 1. At the same time, the stirring frame 5 rotates and stirs to ensure that the temperature of the mixed liquid inside the distillation tank 1 is uniform. At this time, the room-temperature first mixed liquid fills the stirring frame 5 and is in a continuously flowing state. The heated second mixed liquid will continuously heat the first mixed liquid, and the discharged first mixed liquid will enter the pre-storage tank 2. When the stirring and heating of the second mixed liquid in the distillation tank 1 are completed, the steam heating is turned off, and at the same time, the rotation speed of the stirring frame 5 is reduced. At this time, the distillation tank 1 enters the cooling stage. At this time, as the room-temperature first mixed liquid continuously flows into the stirring frame 5, it can take away the temperature of the second mixed liquid in the distillation tank 1. And because the stirring frame 5 is rotating, it can evenly cool the second mixed liquid. At the same time, the heat is transferred to the first mixed liquid. Since the first mixed liquid passes through the relatively long stirring frame 5 and the stirring frame 5 is in a continuously rotating state, the crude product and the solvent injected into the stirring frame 5 at the same time can be well mixed. At the same time, the heat that the previous batch of the second mixed liquid needs to dissipate is used to heat itself. By regulating the rate at which the first mixed liquid enters the stirring frame 5, when the second mixed liquid stops moving, the first mixed liquid just drains into the pre-storage tank 2. Then, the well-mixed and heated first mixed liquid is injected into another distillation tank 1 and heating and rotation start. At the same time, the third batch of mixed liquid is injected into the stirring frame 5 of this distillation tank 1, while the first distillation tank 1 is discharging the finished product at this time, waiting for the injection of the next batch of mixed liquid. Through this setting, the heating, fusion of the mixed liquid, and the heating and evaporation process of the mixed liquid are effectively combined, successfully shortening the time consumed by the process flow. At the same time, half of the heating process utilizes the excess heat that could only be dissipated outward originally, achieving the effect of energy recovery and utilization. Temperature measurement modules are provided inside both the distillation tank 1 and the pre-storage tank 2 to ensure precise temperature control. An electric heating module is arranged on the inner wall of the pre-storage tank 2 and is regulated through the electric heating control box 10 to ensure that the mixed liquid can maintain its temperature in the pre-storage tank 2 and prevent the problem of premature precipitation of the finished product due to too low temperature.

[0034] The stirring frame 5 is composed of a plurality of split tubes 17, and the plurality of split tubes 17 are arranged at equal intervals in a ring shape. A vertical reduction motor 14 is installed at the top of the distillation tank 1, and the output end of the reduction motor 14 is in transmission connection with the top of the stirring frame 5;

[0035] During operation, the plurality of split tubes 17 evenly divide the mixed liquid, and at the same time increase the contact area of the stirring frame 5 to improve the heat exchange effect; the way the mixed liquid enters the split tubes 17 is as follows: the mixed liquid is communicated with two of the split tubes 17, and the mixed liquid is injected into them from top to bottom. After that, the mixed liquid moves from bottom to top through multiple split tubes 17 at the bottom and is finally discharged out through the drain pipe 12, ensuring that the stirring frame 5 is filled with the mixed liquid; the reduction motor 14 drives the stirring frame 5 to rotate stably.

[0036] The pre-storage tank 2 includes an upper mixing tank 25 and a lower transmission tank 26 that are communicated with each other. The output end of the drain pipe 12 is fixedly connected with a cutting-in pipe 29, and the cutting-in pipe 29 is communicated with the upper mixing tank 25. An opening and closing valve 27 is installed at the bottom of the upper mixing tank 25;

[0037] During operation, the mixed liquid discharged from the stirring frame 5 enters the upper mixing tank 25 through the drain pipe 12 and the cutting-in pipe 29. Since the cutting-in pipe 29 is connected to the inner wall of the upper mixing tank 25 at a vertical angle, the mixed liquid entering the upper mixing tank 25 will flow and rotate along the upper mixing tank 25. In this way, the mixed liquid will also continuously rotate and mix in the upper mixing tank 25 because the subsequent mixed liquid will continuously input thrust, ensuring the full mixing of the crude product and the solvent in the mixed liquid; when it is necessary to output the mixed liquid in the pre-storage tank 2, the mixed liquid is first injected into the lower transmission tank 26, and then the negative pressure is increased in the distillation tank 1, and the mixed liquid is sucked into the distillation tank 1 in cooperation with the suction pipe 8.

[0038] A plurality of heat conduction rods 28 are fixedly connected to the bottom of the lower transmission tank 26, and the plurality of heat conduction rods 28 are arranged at equal intervals in a ring shape. Electric heating wires communicated with the electric heating control box 10 are arranged in the heat conduction rods 28;

[0039] During operation, the subsequent injected mixed liquid may have the problem of insufficient temperature. The mixed liquid in the lower transmission tank 26 can be heated by the heat conduction rods 28. At the same time, a water level measuring instrument is provided in the lower transmission tank 26 to measure whether the amount of the transferred mixed liquid meets the standard. The plurality of heat conduction rods 28 will produce a blockage to make the mixed liquid quickly return to a stable state, facilitating the measurement of the water level.

[0040] A mixing ring one 13 and a mixing ring two 15 are arranged above the distillation tank 1. The raw material pipe 11 is communicated with the mixing ring two 15, the drain pipe 12 is communicated with the mixing ring one 13, and both the mixing ring one 13 and the mixing ring two 15 are communicated with the stirring frame 5;

[0041] During operation, the raw material pipe 11 injects the crude product and the solvent into the mixing loop two 15. The mixing loop two 15 is connected to the stirring frame 5, thereby injecting the mixed liquid into it. The mixed liquid that fills the stirring frame 5 and has undergone heat exchange finally enters the mixing loop one 13 and is finally discharged from the drain pipe 12.

[0042] The top of the stirring frame 5 is fixedly connected to the reduction motor 14 by a connecting shaft 23. The outer side of the connecting shaft 23 is rotationally clamped with a clamping ring one 19 and a clamping ring two 20. The clamping ring one 19 and the mixing loop one 13 are connected by two connecting pipes 18. The clamping ring two 20 and the mixing loop two 15 are also connected by two connecting pipes 18. The bottom of the connecting shaft 23 is provided with a communication groove two 21 communicating with the clamping ring two 20, and the bottom of the connecting shaft 23 is also provided with a communication groove one 22 communicating with the clamping ring one 19;

[0043] During operation, the connecting shaft 23 is used to transmit the kinetic energy of the reduction motor 14. The clamping ring one 19 and the clamping ring two 20 are rotationally clamped on the outer side of the connecting shaft 23. When the connecting shaft 23 rotates, the two remain stationary and are supported and fixed by multiple connecting pipes 18. The input end of the stirring frame 5 is connected to the clamping ring two 20, and the output end is connected to the clamping ring one 19, thereby completing the injection and output functions of the mixed liquid.

[0044] The top of the suction pipe 8 is fixedly connected to a multi-way valve 7. The top of the multi-way valve 7 is provided with multiple drain holes, and the ends of the drain holes are fixedly connected to transfer pipes 6. A vertically arranged filter element 9 is installed in the middle of the suction pipe 8;

[0045] During operation, the transfer pipe 6 is used to inject the mixed liquid into the distillation tank 1. The multi-way valve 7 can connect multiple transfer pipes 6. The number of distillation tanks 1 can be increased. It is also possible to use a single storage tank 2 for multiple distillation tanks 1, and only the injection speed of the mixed liquid needs to be adjusted for coordination. The filter element 9 is used to filter impurities in the mixed liquid to ensure the quality of the finished product.

[0046] A feeding window 3 is installed on the outer side of the distillation tank 1 near the top. The middle of the feeding window 3 is made of a transparent material. The rear end of the distillation tank 1 is fixedly connected to a communication valve communicating with the transfer pipe 6;

[0047] During operation, the feeding window 3 is used to observe the internal situation of the distillation tank 1 and can also be used to put in solid materials. The communication valve is connected to the inside of the distillation tank 1 and is used to smoothly transfer the mixed liquid.

[0048] The bottom of the stirring frame 5 is fixedly connected to multiple mixing arms 16. The mixing arms 16 are connected to the stirring frame 5 and are arranged in a bent shape;

[0049] During operation, the mixing arm 16 not only further increases the contact area of the stirring frame 5, but also expands the volume of the stirring frame 5, improving the stirring effect and heat exchange effect.

[0050] Two heat transfer fins 24 are fixedly connected inside the raw material pipe 11. The cross-section of the heat transfer fin 24 is triangular, and the heat transfer fin 24 is arranged in a spiral shape.

[0051] During operation, the heat transfer fin 24 is used to increase the contact surface between the mixed liquid and the raw material pipe 11, further enhancing the heat exchange effect. The spiral arrangement allows the mixed liquid to move spirally inside the raw material pipe 11, improving the mixing effect of the two raw materials in the mixed liquid.

[0052] During operation, by setting up two distillation tanks 1, the crude product just after pickling is injected into the stirring rack 5, and at the same time the solvent is also injected into the stirring rack 5. At this time, the first mixture is at room temperature, and the second mixture from the previous time is still stored in the first distillation tank 1. Steam is introduced into the inner wall of the distillation tank 1 for heating to raise the temperature of the mixture inside the distillation tank 1. At the same time, the stirring rack 5 rotates and stirs to ensure that the temperature of the mixture inside the distillation tank 1 is uniform. At this time, the room-temperature first mixture fills the stirring rack 5 and is in a continuously flowing state, and the heated second mixture will continuously heat the first mixture. The discharged first mixture will enter the pre-storage tank 2. When the stirring and heating of the second mixture in the distillation tank 1 are completed, the steam heating is turned off, and at the same time the rotation speed of the stirring rack 5 is reduced. At this time, the distillation tank 1 enters the cooling stage. At this time, as the room-temperature first mixture continuously flows into the stirring rack 5, it can take away the temperature of the second mixture in the distillation tank 1. And because the stirring rack 5 is rotating, it can evenly cool the second mixture. At the same time, the heat is transferred to the first mixture. Since the first mixture passes through the relatively long stirring rack 5 and the stirring rack 5 is in a continuous rotating state, the crude product and the solvent injected into the stirring rack 5 at the same time can be well mixed. At the same time, the heat that the previous batch of the second mixture needs to dissipate is used to heat itself. By regulating the rate at which the first mixture enters the stirring rack 5, when the second mixture stops stirring, the first mixture just drains into the pre-storage tank 2. Then the well-mixed and heated first mixture is injected into another distillation tank 1 and heating and rotation start. At the same time, the third batch of the mixture is injected into the stirring rack 5 of this distillation tank 1, while the first distillation tank 1 is discharging the finished product at this time, waiting for the injection of the next mixture. Through this setting, the heating, fusion of the mixture, and the heating and evaporation process of the mixture are effectively combined, successfully shortening the time consumed by the process flow. At the same time, half of the heating process utilizes the excess heat that could only be dissipated outward originally, achieving the effect of energy recovery and utilization. Temperature measurement modules are provided inside both the distillation tank 1 and the pre-storage tank 2 to ensure precise temperature control. An electric heating module is provided on the inner wall of the pre-storage tank 2 and is regulated through the electric heating control box 10 to ensure that the mixture can maintain its temperature in the pre-storage tank 2 and prevent the problem of premature precipitation of the finished product due to too low temperature.

[0053] Multiple splitting tubes 17 divide the mixture evenly, and at the same time increase the contact area of the stirring rack 5 to improve the heat exchange effect. The way the mixture enters the splitting tubes 17 is as follows: The mixture is connected to two of the splitting tubes 17, and the mixture is injected into them from top to bottom. Then the mixture moves from bottom to top through multiple splitting tubes 17 at the bottom and finally discharges outward through the drain pipe 12, ensuring that the stirring rack 5 is filled with the mixture. The stirring rack 5 is stably rotated by the reduction motor 14.

[0054] The mixed liquid discharged from the stirring frame 5 enters the upper mixing tank 25 through the discharge pipe 12 and the cut-in pipe 29. Since the cut-in pipe 29 is connected to the inner wall of the upper mixing tank 25 at a vertical angle, the mixed liquid entering the upper mixing tank 25 will flow and rotate along the upper mixing tank 25, so that the mixed liquid will also be rotated and mixed in the upper mixing tank 25 for a long time, because the subsequent mixed liquid will continuously input thrust, thereby ensuring the full mixing of the crude product and the solvent in the mixed liquid; when the mixed liquid in the pre-storage tank 2 needs to be outputted, the mixed liquid is first injected into the lower transmission tank 26, and then the negative pressure is increased in the distillation tank 1, and the mixed liquid is pumped into the distillation tank 1 in cooperation with the suction pipe 8;

[0055] The mixed liquid injected subsequently may have a problem of insufficient temperature. The mixed liquid in the lower transmission tank 26 can be heated by the heat-conducting rod 28. At the same time, there is a water level measuring instrument in the lower transmission tank 26 to measure whether the amount of the mixed liquid transferred meets the standard. Multiple heat-conducting rods 28 will create obstacles, allowing the mixed liquid to quickly return to stability, which is convenient for water level measurement;

[0056] The raw material pipe 11 injects the crude product and the solvent into the mixing ring 2 15, and the mixing ring 2 15 is connected to the stirring frame 5, so that the mixed liquid is injected therein, and the mixed liquid that fills the stirring frame 5 and undergoes heat exchange finally enters the mixing ring 1 13, and finally is discharged from the drain pipe 12;

[0057] The connecting shaft 23 is used to transmit the kinetic energy of the reduction motor 14. The clamping ring 19 and the clamping ring 20 are rotatably clamped on the outside of the connecting shaft 23. When the connecting shaft 23 rotates, the two remain stationary and are supported and fixed by a plurality of connecting pipes 18. The input end of the stirring frame 5 is connected to the clamping ring 20, and the output end is connected to the clamping ring 19, thereby completing the injection and output functions of the mixed liquid;

[0058] The transfer pipe 6 is used to inject the mixed liquid into the distillation tank 1. The multi-way valve 7 can connect multiple transfer pipes 6. The number of distillation tanks 1 can be increased. It is also possible to use one pre-storage tank 2 for multiple distillation tanks 1 at the same time. It is only necessary to adjust the injection speed of the mixed liquid to coordinate. The filter element 9 is used to filter impurities in the mixed liquid to ensure the quality of the finished product.

[0059] The feeding window 3 is used to observe the internal situation of the distillation tank 1, and can also be used to feed solid materials. The connecting valve is connected to the inside of the distillation tank 1 for smoothly transferring the mixed liquid;

[0060] The mixing arm 16 not only further increases the contact area of the stirring frame 5, but also expands the volume of the stirring frame 5, thereby improving the stirring effect and heat exchange effect;

[0061] The heat transfer fin 24 is used to increase the contact area between the mixed liquid and the raw material pipe 11, further enhancing the heat exchange effect. The spiral configuration enables the mixed liquid to move spirally inside the raw material pipe 11, improving the mixing effect of the two raw materials in the mixed liquid.

[0062] The foregoing has shown and described the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited by the above embodiments, and what is described in the above embodiments and the specification is only to illustrate the principle of the present invention. Without departing from the spirit and scope of the present invention, the present invention will have various changes and improvements, and these changes and improvements all fall within the scope of the present invention claimed. The scope of the present invention claimed is defined by the appended claims and their equivalents.

Claims

1. A full-process precipitation crystallization device for bromine-based substances, characterized in that: It comprises two distillation tanks, a pre-storage tank is arranged between the two distillation tanks, a rotatable stirring frame is arranged in the distillation tank, a raw material pipe connected to the stirring frame is arranged on the outside of the distillation tank, a liquid discharge pipe connected to the stirring frame is also arranged on the outside of the distillation tank, the liquid discharge pipe is connected to the pre-storage tank, a suction pipe is fixedly connected to the bottom of the pre-storage tank, the suction pipe is connected to the inside of the distillation tank, a discharge valve is installed at the bottom of the distillation tank, and an electric heating control box is installed on the outside of the pre-storage tank; The stirring frame is composed of a plurality of split tubes, which are arranged in a circular shape with equal spacing. A vertically arranged reduction motor is installed on the top of the distillation tank, and the output end of the reduction motor is transmission-connected to the top of the stirring frame; A plurality of mixing arms are fixedly connected to the bottom of the stirring frame, the mixing arms are connected to the stirring frame, and the mixing arms are arranged in a bent shape; A mixing ring 1 and a mixing ring 2 are arranged above the distillation tank, the raw material pipe is connected to the mixing ring 2, the drain pipe is connected to the mixing ring 1, and the mixing ring 1 and the mixing ring 2 are both connected to the stirring frame; The top of the stirring frame is fixedly connected to the reduction motor with a connecting shaft, and the outer side of the connecting shaft is rotatably connected with a clamping ring 1 and a clamping ring 2, the clamping ring 1 is connected with the mixing ring 1 through two connecting pipes, and the clamping ring 2 is also connected with the mixing ring 2 through two connecting pipes, and the bottom of the connecting shaft is provided with a connecting groove 2 connected with the clamping ring 2, and the bottom of the connecting shaft is also provided with a connecting groove 1 connected with the clamping ring 1; Among them, as the mixed liquid 1 at room temperature continuously flows into the stirring rack, it takes away the temperature of the mixed liquid 2 in the distillation tank. At the same time, the stirring rack rotates and stirs, which can cool the mixed liquid 2 at a uniform speed. At the same time, the heat is transferred to the mixed liquid 1, combining the heating, fusion and heating evaporation processes of the mixed liquid, thereby shortening the time consumed by the process.

2. The crystallization device for the whole-process precipitation of bromine-based substances according to claim 1, wherein: The pre-storage tank includes an upper mixing tank and a lower transmission tank which are interconnected. The output end of the discharge pipe is fixedly connected with a cut-in pipe which is connected with the upper mixing tank. An opening and closing valve is installed at the bottom of the upper mixing tank.

3. The crystallization device for the whole process precipitation of bromine substances according to claim 2, characterized in that: A plurality of heat-conducting rods are fixedly connected to the bottom of the lower transmission tank. The plurality of heat-conducting rods are arranged in a ring shape with equal spacing. The heat-conducting rods are provided with electric heating wires connected to the electric heating control box.

4. A crystallization device for the whole-process precipitation of bromine-based substances according to claim 3, characterized in that: A multi-way valve is fixedly connected to the top of the suction pipe, a plurality of drainage holes are opened on the top of the multi-way valve, transfer pipes are fixedly connected to the ends of the drainage holes, and a vertically arranged filter element is installed in the middle of the suction pipe.

5. The crystallization device for the whole process precipitation of bromine-based substances according to claim 4, characterized in that: A feeding window is installed on the outer side of the distillation tank near the top, the middle part of the feeding window is made of transparent material, and a connecting valve connected with the transfer pipe is fixedly connected to the rear end of the distillation tank.

6. The crystallization device for the whole process precipitation of bromine-based substances according to claim 5, wherein: Two heat transfer sheets are fixedly connected inside the raw material tube. The cross-section of the heat transfer sheet is triangular and the heat transfer sheet is spirally arranged.

Citation Information

Patent Citations

  • DTB evaporation crystallizer

    CN212594089U

  • Medicinal acid crystallization kettle

    CN218608119U