Whole-flow separation and crystallization device for brominated substances

Abstract

The invention belongs to the field of substance precipitation and crystallization, and particularly relates to a brominated substance whole-process precipitation and crystallization device which comprises two distillation retorts, a pre-storage tank is arranged between the two distillation retorts, a stirring frame capable of rotating is arranged in each distillation retort, and a raw material pipe communicated with the stirring frame is arranged on the outer side of each distillation retort. A liquid discharging pipe communicated with the stirring frame is further arranged on the outer side of the distillation tank, the liquid discharging pipe is communicated with a pre-storage tank, a suction pipe is fixedly connected to the bottom of the pre-storage tank, the suction pipe is communicated with the interior of the distillation tank, a discharging valve is installed at the bottom of the distillation tank, and an electric heating control box is installed on the outer side of the pre-storage tank. The heating and fusing processes of the mixed liquid and the heating and evaporating processes of the mixed liquid are effectively combined, the time consumed by the technological process is successfully shortened, meanwhile, excessive heat which can only be dissipated outwards originally is utilized in the half heating process, and the energy recycling effect is achieved.

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. 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.

[0004] To this end, the present invention provides a full-process precipitation and crystallization device for bromine-based substances. Summary of the invention

[0005] In order to make up for the deficiencies of the prior art, at least one technical problem raised in the background technology is solved.

[0006] 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; 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.

[0007] 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.

[0008] Preferably, 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, the cut-in pipe is connected to the upper mixing tank, an opening and closing 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 discharge pipe and the cut-in pipe, and since the cut-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, so that the mixed liquid will also rotate and mix permanently in the upper mixing tank, because the subsequent mixed liquid will continuously input thrust, thereby ensuring the sufficient mixing of the crude product and the solvent in the mixed liquid; when the mixed liquid in the pre-storage tank needs to be output externally, the mixed liquid is first injected into the lower transmission tank, and then the negative pressure is increased in the distillation tank, and the mixed liquid is pumped into the distillation tank in conjunction with the suction pipe.

[0009] Preferably, a plurality of heat-conducting rods are fixedly connected to the bottom of the lower transmission tank, and the plurality of heat-conducting rods are arranged equidistantly in a ring shape. The heat-conducting rods are provided with electric heating wires connected to the electric heating control box. The mixed liquid injected subsequently may have the problem of insufficient temperature, and the mixed liquid in the lower transmission tank can be heated by the heat-conducting rods. At the same time, there is a water level measuring instrument in the lower transmission tank, which can measure whether the amount of the transferred mixed liquid meets the standard. The plurality of heat-conducting rods will produce obstructions, allowing the mixed liquid to quickly return to stability, which is convenient for the measurement of the water level.

[0010] 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, the drain pipe is connected to the mixing ring one, and both the mixing ring one and the mixing ring two are connected to the stirring rack. The raw material pipe injects the crude product and the solvent into the mixing ring two, and the mixing ring two is connected to the stirring rack, thereby injecting the mixed liquid therein. The mixed liquid that fills the stirring rack and undergoes heat exchange finally enters the mixing ring one and is finally discharged from the drain pipe.

[0011] Preferably, 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 clamped with a clamping ring 1 and a clamping ring 2, the clamping ring 1 is connected to the mixing ring 1 through two connecting tubes, and the clamping ring 2 is also connected to the mixing ring 2 through two connecting tubes, and the bottom of the connecting shaft is provided with a connecting groove 2 connected to the clamping ring 2, and the bottom of the connecting shaft is also provided with a connecting groove 1 connected to the clamping ring 1, the connecting shaft is used to transmit the kinetic energy of the reduction motor, the clamping ring 1 and the clamping ring 2 are rotatably clamped on the outer side of the connecting shaft, and when the connecting shaft rotates, the two remain stationary and are supported and fixed by multiple connecting tubes, the input end of the stirring frame is connected to the clamping ring 2, and the output end is connected to the clamping ring 1, thereby completing the injection and output functions of the mixed liquid.

[0012] Preferably, a multi-way valve is fixedly connected to the top of the suction tube, a plurality of drainage holes are opened on the top of the multi-way valve, a transfer pipe is fixedly connected to the end of the drainage hole, a vertically arranged filter element is installed in the middle of the suction tube, the transfer pipe is used to inject the mixed liquid into the distillation tank, the multi-way valve can connect multiple transfer pipes, the number of distillation tanks can be increased, and one pre-storage tank can be used for multiple distillation tanks at the same time, and it is only necessary to adjust the injection speed of the mixed liquid to coordinate, and the filter element is used to filter impurities in the mixed liquid to ensure the quality of the finished product.

[0013] 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, and a connecting valve connected to 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 feed solid materials. The connecting valve is connected to the inside of the distillation tank for smoothly transferring the mixed liquid.

[0014] Preferably, 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. The mixing arms not only further increase the contact area of ​​the stirring frame, but also expand the volume of the stirring frame, thereby improving the stirring effect and heat exchange effect.

[0015] Preferably, two heat transfer plates are fixedly connected to the inside of the raw material tube, the cross-section of the heat transfer plates is triangular, and the heat transfer plates are spirally arranged. The heat transfer plates are used to increase the contact surface between the mixed liquid and the raw material tube, further increasing the heat exchange effect, and the spiral arrangement allows the mixed liquid to move in a spiral inside the raw material tube, thereby improving the mixing effect of the two raw materials in the mixed liquid.

[0016] The beneficial effects of the present invention are as follows: 1. The full-process precipitation and crystallization device for bromine-based substances described in the present invention has two distillation tanks, and the crude product that has just been pickled is injected into the stirring frame, and the solvent is also injected into the stirring frame. Through this arrangement, the heating and fusion of the mixed liquid and the heating and evaporation process of the mixed liquid are effectively combined, which successfully shortens the time consumed by the process flow. At the same time, half of the heating process utilizes the excess heat that can only be dissipated outward, thereby achieving the effect of energy recovery and utilization.

[0017] 2. In the full-process precipitation and crystallization device for bromine-based substances described in the present invention, a plurality of splitting tubes divide the mixed liquid evenly, and at the same time increase the contact area of ​​the stirring frame, thereby improving the heat exchange effect; the mixed liquid is introduced into the splitting tubes in the following manner: the mixed liquid is connected to two of the splitting tubes, and the mixed liquid is injected into the splitting tubes from top to bottom, and then the mixed liquid moves from bottom to top through the plurality of splitting tubes at the bottom, and finally is discharged from the drain pipe, thereby ensuring that the stirring frame is filled with the mixed liquid; the stirring frame is driven by a reduction motor to rotate stably. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] The present invention will be further described below in conjunction with the accompanying drawings.

[0019] Figure 1 is a stereogram of the present invention; Figure 2 It is a stereoscopic diagram of the pre-storage tank and the distillation tank of the present invention; Figure 3 is a perspective view of a distillation tank of the present invention; Figure 4 is a cross-sectional view of a distillation tank of the present invention; Figure 5 is a three-dimensional diagram of the stirring frame of the present invention; Figure 6 is a cross-sectional view of the connecting shaft of the present invention; Figure 7 is a stereogram of a raw material tube of the present invention; Figure 8 It is a three-dimensional diagram of the pre-storage tank of the present invention; 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. discharge 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 plate; 25. upper mixing tank; 26. lower transfer tank; 27. opening and closing valve; 28. heat conduction rod; 29. ​​cutting pipe. DETAILED DESCRIPTION

[0020] In order to make the technical means, creative features, objectives and effects achieved by the present invention easy to understand, the present invention is further explained below in conjunction with specific implementation methods.

[0021] like Figures 1 to 8 As shown, a full-process precipitation crystallization device for bromine-based substances according to an embodiment of the present invention comprises 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 connected to the stirring frame 5 is arranged on the outside of the distillation tank 1, a drain pipe 12 connected to the stirring frame 5 is also arranged on the outside of the distillation tank 1, the drain pipe 12 is connected to 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 connected to the inside of the distillation tank 1, a discharge valve 4 is installed at the bottom of the distillation tank 1, and an electric heating control box 10 is installed on the outside of the pre-storage tank 2; By setting up two distillation tanks 1, the crude product just after pickling is injected into the stirring rack 5, and the solvent is also injected into the stirring rack 5. At this time, the mixed solution 1 is at room temperature, and the first distillation tank 1 still contains the previous mixed solution 2. Steam is introduced into the inner wall of the distillation tank 1 to heat the mixed solution inside the distillation tank 1. At the same time, the stirring rack 5 is rotated and stirred to ensure that the temperature of the mixed solution inside the distillation tank 1 is uniform. At this time, the room temperature mixed solution 1 fills the stirring rack 5 and is in a state of continuous flow, and the heated mixed solution 2 will continuously heat the mixed solution. The mixed liquid 1 is discharged, and the discharged mixed liquid 1 will enter the pre-storage tank 2. When the mixed liquid 2 in the distillation tank 1 is stirred and heated, the steam heating is turned off, and the speed of the stirring rack 5 is reduced. At this time, the distillation tank 1 enters the cooling stage. At this time, as the mixed liquid 1 at room temperature continues to flow into the stirring rack 5, the temperature of the mixed liquid 2 in the distillation tank 1 can be taken away. Since the stirring rack 5 is in a rotating state, 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 long stirring rack 5, and the stirring rack 5 is in a continuously rotating state, the mixed liquid 1 is simultaneously injected into the stirring rack 5. The crude product and solvent introduced into the stirring rack 5 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 5, when the mixed liquid 2 stops, the mixed liquid 1 is just discharged into the pre-storage tank 2, and then the mixed and heated mixed liquid 1 is injected into another distillation tank 1, and heating and rotation are started, and at the same time, the third batch of mixed liquid is injected into the stirring rack 5 of the distillation tank 1, while the first distillation tank 1 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, which successfully shortens 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, thereby achieving energy recovery and utilization effects. Both the distillation tank 1 and the pre-storage tank 2 are provided with temperature measuring modules to ensure accurate temperature control. The inner wall of the pre-storage tank 2 is provided with an electric heating module, which is regulated by the electric heating control box 10 to ensure that the temperature of the mixed liquid can be maintained in the pre-storage tank 2 to prevent the temperature from being too low, which may cause the finished product to precipitate prematurely.

[0022] The stirring frame 5 is composed of a plurality of split tubes 17, which are arranged in a circular shape and at equal intervals. A vertically arranged reduction motor 14 is installed on the top of the distillation tank 1, and the output end of the reduction motor 14 is transmission-connected to the top of the stirring frame 5; During operation, the multiple split tubes 17 divide the mixed liquid evenly, and at the same time increase the contact area of ​​the stirring frame 5, thereby improving the heat exchange effect; the mixed liquid is introduced into the split tubes 17 in the following manner: the mixed liquid is connected to two of the split tubes 17, and the mixed liquid is injected into the split tubes from top to bottom, and then the mixed liquid moves from the bottom multiple split tubes 17 from bottom to top, and finally is discharged from the drain pipe 12, thereby ensuring that the stirring frame 5 is filled with the mixed liquid; the stirring frame 5 is driven to rotate stably by the reduction motor 14.

[0023] The pre-storage tank 2 includes an upper mixing tank 25 and a lower transmission tank 26 which are connected to each other. The output end of the discharge pipe 12 is fixedly connected with a cut-in pipe 29, and the cut-in pipe 29 is connected with the upper mixing tank 25. An opening and closing valve 27 is installed at the bottom of the upper mixing tank 25. During operation, 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. In this way, the mixed liquid will also rotate and mix permanently in the upper mixing tank 25, because the subsequent mixed liquid will continuously input thrust, thereby ensuring the sufficient 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 output to the outside, 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 with the help of the suction pipe 8.

[0024] A plurality of heat-conducting rods 28 are fixedly connected to the bottom of the lower transmission tank 26. The plurality of heat-conducting rods 28 are arranged in a ring-shaped manner with equal spacing. The heat-conducting rods 28 are provided with electric heating wires connected to the electric heating control box 10. During operation, the subsequently 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-conducting rod 28. At the same time, there is a water level measuring instrument in the lower transmission tank 26, which can measure whether the amount of the transferred mixed liquid meets the standard. Multiple heat-conducting rods 28 will create obstacles, allowing the mixed liquid to quickly return to stability, making it convenient to measure the water level.

[0025] A mixing ring 13 and a mixing ring 2 15 are arranged above the distillation tank 1, the raw material pipe 11 is connected to the mixing ring 2 15, the discharge pipe 12 is connected to the mixing ring 13, and the mixing ring 13 and the mixing ring 2 15 are both connected to the stirring frame 5; During operation, 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 is finally discharged from the drain pipe 12.

[0026] The top of the stirring frame 5 is fixedly connected to the reduction motor 14 with a connecting shaft 23, and the outer side of the connecting shaft 23 is rotatably connected with a clamping ring 19 and a clamping ring 20, the clamping ring 19 is connected with the mixing ring 13 through two connecting pipes 18, and the clamping ring 20 is also connected with the mixing ring 15 through two connecting pipes 18. The bottom of the connecting shaft 23 is provided with a connecting groove 21 connected with the clamping ring 20, and the bottom of the connecting shaft 23 is also provided with a connecting groove 22 connected with the clamping ring 19; During operation, 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 multiple connecting tubes 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.

[0027] 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 a plurality of drainage holes, the ends of the drainage holes are fixedly connected to a transfer pipe 6, and a vertically arranged filter element 9 is installed in the middle of the suction pipe 8; 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 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.

[0028] A feeding window 3 is installed on the outside of the distillation tank 1 near the top, the middle part of the feeding window 3 is made of transparent material, and a connecting valve connected to the transfer pipe 6 is fixedly connected to the rear end of the distillation tank 1; During operation, 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.

[0029] A plurality of mixing arms 16 are fixedly connected to the bottom of the stirring frame 5, the mixing arms 16 are connected to the stirring frame 5, and the mixing arms 16 are arranged in a bent shape; When working, 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.

[0030] Two heat transfer sheets 24 are fixedly connected to the inside of the raw material tube 11. The cross section of the heat transfer sheet 24 is triangular and the heat transfer sheet 24 is spirally arranged. During operation, the heat transfer sheet 24 is used to increase the contact surface between the mixed liquid and the raw material tube 11, further increasing the heat exchange effect, and the spiral arrangement allows the mixed liquid to move in a spiral inside the raw material tube 11, thereby improving the mixing effect of the two raw materials in the mixed liquid.

[0031] During operation, two distillation tanks 1 are set up, and the crude product just after pickling is injected into the stirring rack 5, and the solvent is also injected into the stirring rack 5. At this time, the mixed solution 1 is at room temperature, and the first distillation tank 1 still contains the previous mixed solution 2. Steam is introduced into the inner wall of the distillation tank 1 to heat the mixed solution inside the distillation tank 1. At the same time, the stirring rack 5 is rotated and stirred to ensure that the temperature of the mixed solution inside the distillation tank 1 is uniform. At this time, the room temperature mixed solution 1 fills the stirring rack 5 and is in a state of continuous flow, and the heated mixed solution 2 will continuously The mixed liquid 1 is heated, and the discharged mixed liquid 1 will enter the pre-storage tank 2. When the mixed liquid 2 in the distillation tank 1 is stirred and heated, the steam heating is turned off, and the speed of the stirring rack 5 is reduced. At this time, the distillation tank 1 enters the cooling stage. At this time, as the mixed liquid 1 at room temperature continues to flow into the stirring rack 5, the temperature of the mixed liquid 2 in the distillation tank 1 can be taken away, and because the stirring rack 5 is in a rotating state, 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 long stirring rack 5, and the stirring rack 5 is in a continuously rotating state, the mixed liquid 1 is cooled at the same time. The crude product and solvent injected into the stirring rack 5 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 5, when the mixed liquid 2 stops, the mixed liquid 1 is just discharged into the pre-storage tank 2, and then the mixed and heated mixed liquid 1 is injected into another distillation tank 1, and heating and rotation are started. At the same time, the third batch of mixed liquid is injected into the stirring rack 5 of the distillation tank 1, and the first distillation tank 1 is discharging the finished product at this time, waiting for the next injection of the mixed liquid. Through this arrangement , effectively combining the heating, fusion and heating evaporation processes of the mixed liquid, successfully shortening the time consumed by the process flow, and at the same time, half of the heating process utilizes the excess heat that could only be dissipated outward, achieving the effect of energy recovery and utilization; both the distillation tank 1 and the pre-storage tank 2 are provided with temperature measurement modules to ensure accurate temperature control, and the inner wall of the pre-storage tank 2 is provided with an electric heating module, which is regulated by the electric heating control box 10 to ensure that the temperature of the mixed liquid can be maintained in the pre-storage tank 2, to prevent the problem of premature precipitation of the finished product caused by the temperature being too low; The multiple split tubes 17 evenly divide the mixed liquid, and at the same time increase the contact area of ​​the stirring frame 5, thereby improving the heat exchange effect; the mixed liquid is introduced into the split tubes 17 in the following manner: the mixed liquid is connected to two of the split tubes 17, and the mixed liquid is injected into the split tubes from top to bottom, and then the mixed liquid moves from the bottom multiple split tubes 17 from bottom to top, and finally discharged from the drain pipe 12, thereby ensuring that the stirring frame 5 is filled with the mixed liquid; the stirring frame 5 is driven to rotate stably by the reduction motor 14; 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; 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; 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; 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; 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. 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; 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; The heat transfer sheet 24 is used to increase the contact surface between the mixed liquid and the raw material tube 11, further increasing the heat exchange effect, and the spiral arrangement allows the mixed liquid to move in a spiral manner inside the raw material tube 11, thereby improving the mixing effect of the two raw materials in the mixed liquid.

[0032] The above shows and describes the basic principles, main features and advantages of the present invention. It should be understood by those skilled in the art that the present invention is not limited to the above embodiments. The above embodiments and descriptions are only for explaining the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, which fall within the scope of the present invention. The scope of protection of the present invention is defined by the attached claims and their equivalents.

Claims

1. A full-process precipitation and 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; 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. A full-process precipitation and crystallization device for bromine-based substances according to claim 1, characterized in that: 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. A full-process precipitation and crystallization device for bromine-based 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 full-process precipitation and crystallization device for bromine-based substances according to claim 3, characterized in that: 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 discharge 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.

5. A full-process precipitation and crystallization device for bromine-based substances according to claim 4, characterized in that: 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 clamped with a clamping ring 1 and a clamping ring 2. The clamping ring 1 is connected to the mixing ring 1 through two connecting pipes, and the clamping ring 2 is also connected to the mixing ring 2 through two connecting pipes. The bottom of the connecting shaft is provided with a connecting groove 2 connected to the clamping ring 2, and the bottom of the connecting shaft is also provided with a connecting groove 1 connected to the clamping ring 1.

6. A full-process precipitation and crystallization device for bromine-based substances according to claim 5, 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.

7. A full-process precipitation and crystallization device for bromine-based substances according to claim 6, 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.

8. A full-process precipitation and crystallization device for bromine-based substances according to claim 7, characterized in that: 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.

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