A temperature control comparison device for dispersing blue brominated filter cake

Abstract

This invention provides a temperature control and comparison device for dispensing dispersed blue bromide filter cake, relating to the field of dye manufacturing. It includes a reaction vessel body with a jacket fixedly connected to it. A water inlet pipe is fixedly connected to the bottom of the jacket, and a first, second, and third water outlet pipes are fixedly connected to its side. The first water outlet pipe is positioned at the top of the jacket, forming an upper temperature control zone between the first and second water outlet pipes, a middle temperature control zone between the second and third water outlet pipes, and a lower temperature control zone between the third water outlet pipe and the water inlet pipe. Adjustment mechanisms for regulating liquid flow are provided in each of the upper, middle, and lower temperature control zones. This temperature control and comparison device for dispensing dispersed blue bromide filter cake divides the jacket into upper, middle, and lower temperature control zones along its height. Each zone allows independent adjustment of the circulating liquid flow rate and velocity, achieving temperature difference control between different height zones within the same reaction vessel.

Description

Technical Field

[0001] This invention relates to the field of dye manufacturing technology, specifically to a temperature-controlled comparison device for dispensing dispersed blue bromide filter cake. Background Technology

[0002] Disperse Blue is an important anthraquinone disperse dye, and its production process requires a bromination reaction to obtain a brominated filter cake. Before subsequent dispersion and drying processes, the brominated filter cake typically needs to be neutralized, washed, or recrystallized in a reaction vessel. This process demands extremely strict temperature control: excessively high temperatures can easily lead to side reactions, affecting product purity; excessively low temperatures result in incomplete dissolution of the filter cake, leading to poor treatment results. The optimal reaction temperature may vary between different batches or under different process conditions; therefore, temperature control comparison experiments are often conducted during production to determine the optimal temperature parameters.

[0003] Most existing reactor jackets are integral structures, with cooling water or heat transfer medium entering from the bottom and exiting from the top. This results in uneven temperature distribution within the jacket, making it impossible to simultaneously conduct comparative experiments on different temperature zones within the same reactor. Operators often need to perform multiple sets of experiments in different reactors, which not only consumes a lot of equipment and is inefficient, but also the material differences between the different reactors can affect the accuracy of the comparison results. Summary of the Invention

[0004] To address the shortcomings of existing technologies, this invention provides a temperature control comparison device for dispersing blue bromide filter cake. By dividing the jacket into three independent temperature control zones (upper, middle, and lower), each temperature control zone is equipped with an inflatable annular air bladder to regulate the liquid flow rate. Combined with different water outlet pipes, this device enables independent control and rapid switching between different temperature zones within the same reactor, facilitating temperature control comparison experiments.

[0005] To achieve the above objectives, the present invention provides the following technical solution: a temperature-controlled comparison device for dispersing blue bromide filter cake, comprising a reaction vessel body, wherein a jacket is fixedly connected to the reaction vessel body; a water inlet pipe is fixedly connected to the bottom of the jacket, and a first water outlet pipe, a second water outlet pipe, and a third water outlet pipe are fixedly connected to the side of the jacket; the first water outlet pipe is disposed at the top of the jacket, so that an upper temperature control zone is formed between the first water outlet pipe and the second water outlet pipe, a middle temperature control zone is formed between the second water outlet pipe and the third water outlet pipe, and a lower temperature control zone is formed between the third water outlet pipe and the water inlet pipe; each of the upper, middle, and lower temperature control zones is provided with a regulating mechanism for adjusting the liquid flow rate.

[0006] Furthermore, the adjustment mechanism includes an inflation assembly, a connecting pipe, and an annular airbag; the outer side of the annular airbag is fixedly connected to the inner wall of the jacket, one end of the connecting pipe is fixedly connected to the annular airbag, and the other end is connected to the inflation assembly; the annular airbag is configured to expand inward when inflated, reduce the liquid flow gap, and increase the liquid flow rate in the temperature control zone.

[0007] Furthermore, each regulating mechanism contains at least two annular airbags; when the annular airbags are fully inflated, their inner ends are in contact with the outer wall of the reactor body, thereby isolating the liquid flow; under normal conditions, the second and third water outlet pipes are closed, and the liquid flows out from the first water outlet pipe; when the annular airbags in the upper temperature control zone are fully inflated to isolate the temperature control zone, the first and third water outlet pipes are closed, and the liquid flows out from the second water outlet pipe; when the annular airbags in the middle temperature control zone are fully inflated to isolate the temperature control zone, the first and second water outlet pipes are closed, and the liquid flows out from the third water outlet pipe.

[0008] Furthermore, a sealing layer is fixedly connected to the outer side of the annular airbag.

[0009] Furthermore, a vertical rod is provided inside the reactor body, and a first temperature sensor, a second temperature sensor, and a third temperature sensor are fixedly connected to the vertical rod; the first temperature sensor, the second temperature sensor, and the third temperature sensor correspond one-to-one with the upper temperature control zone, the middle temperature control zone, and the lower temperature control zone, respectively.

[0010] Furthermore, a cover is connected to the top of the reactor body, and the top end of the vertical rod is fixedly connected to the cover.

[0011] Furthermore, a motor is fixedly connected to the cover, a stirring shaft is fixedly connected to the output end of the motor, and a stirring paddle is fixedly connected to the stirring shaft.

[0012] Furthermore, the inflation assembly includes three pressure chambers, a pressure sensor, an inflation branch pipe, an inflation main pipe, a first electrically controlled valve, and an air pump; each pressure chamber is fixedly connected to a pressure sensor; one end of each pressure chamber is fixedly connected to the corresponding connecting pipe, and the other end is fixedly connected to the corresponding inflation branch pipe; each inflation branch pipe is fixedly connected to the first electrically controlled valve, and each inflation branch pipe is connected to the inflation main pipe; the inflation main pipe is fixedly connected to the output end of the air pump.

[0013] Furthermore, a second electrically controlled valve is fixedly connected to each of the water inlet pipes and each water outlet pipe.

[0014] Furthermore, the first, second, and third water outlet pipes are all located on the same vertical plane.

[0015] This invention provides a temperature-controlled comparison device for distributing blue bromide filter cake. It has the following beneficial effects: 1. The temperature control comparison device for dispersing blue bromide filter cake divides the jacket into three temperature control zones along the height direction: upper, middle, and lower. The flow rate and velocity of the circulating liquid in each zone can be adjusted independently, thereby achieving temperature difference control in different height zones within the same reactor and facilitating temperature control comparison experiments.

[0016] 2. This temperature control comparison device for dispersing blue bromide filter cake can flexibly select the first, second, or third water outlet as the water outlet by controlling the inflation state of the annular air bladder in different temperature control zones, realizing rapid switching of the circulating liquid path and meeting different temperature control comparison requirements; temperature sensors corresponding to the three temperature control zones are set in the reactor to collect temperature data of each zone in real time, providing accurate basis for temperature control comparison.

[0017] 3. The temperature control comparison device used for dispersing blue bromide filter cake adopts the method of changing the liquid flow cross-sectional area by inflating an annular airbag. Compared with traditional valve regulation, it has a fast response speed and high regulation accuracy. Attached Figure Description

[0018] Figure 1 This is a schematic diagram of the structure of the present invention; Figure 2 This is a cross-sectional view of the structure of the present invention; Figure 3 This is a schematic diagram of the adjustment mechanism structure of the present invention; Figure 4 This is a schematic diagram of the inflation component structure of the present invention.

[0019] In the diagram: 1. Reactor body; 2. Cover; 3. Motor; 4. Stirring shaft; 5. Stirring paddle; 6. Jacket; 7. Water inlet pipe; 8. Connecting pipe; 9. First water outlet pipe; 10. Second water outlet pipe; 11. Third water outlet pipe; 12. Annular airbag; 13. Vertical rod; 14. First temperature sensor; 15. Second temperature sensor; 16. Third temperature sensor; 17. Pressure chamber; 18. Pressure sensor; 19. Inflation branch pipe; 20. First electrically controlled valve; 21. Inflation main pipe; 22. Air pump. Detailed Implementation

[0020] This invention provides a temperature control comparison device for dispensing dispersed blue bromide filter cake, such as... Figures 1 to 4 As shown, it includes a reaction vessel body 1, a jacket 6, an adjustment mechanism, a temperature detection component, a stirring component, and an aeration component.

[0021] The reactor body 1 is a vertical cylindrical stainless steel container with a nominal volume of 500L and a design pressure of 0.6MPa, used to hold dispersed blue bromide filter cake and treatment liquid. The top of the reactor body 1 is connected to a cover 2 via a flange. A motor 3 (in this embodiment, the power is 5.5kW and the speed is adjustable from 0-100rpm) is fixedly installed on the cover 2. The output end of the motor 3 is connected downward to a stirring shaft 4, and two layers of stirring paddles 5 are fixed on the stirring shaft 4 to stir the materials and make them mix evenly.

[0022] The jacket 6 is a cylindrical shell made of carbon steel, welded to the outer wall of the reactor body 1. A 50mm thick annular cavity is formed between the jacket 6 and the reactor body 1 for introducing circulating fluid (hot water or cooling water) to achieve temperature control. The jacket 6 is designed to withstand a pressure of 0.4MPa, and the working medium is softened water or heat transfer oil.

[0023] A water inlet pipe 7 is fixedly connected to the bottom center of the jacket 6 for introducing circulating fluid. A first water outlet pipe 9, a second water outlet pipe 10, and a third water outlet pipe 11 are fixedly connected sequentially along the vertical direction on the side of the jacket 6. All three water outlet pipes are on the same vertical plane, which facilitates pipeline connection and operation.

[0024] Due to the different locations of the water outlet pipes, three independent temperature control zones are naturally formed inside jacket 6: The area between the first water outlet pipe 9 and the second water outlet pipe 10 is the upper temperature control zone; The area between the second water outlet pipe 10 and the third water outlet pipe 11 is the medium temperature control zone; The area between the third outlet pipe 11 and the inlet pipe 7 is the lower temperature control zone.

[0025] Each temperature control zone is equipped with an adjustment mechanism to independently adjust the flow cross-sectional area and flow rate of the circulating fluid within that zone.

[0026] The core component of the regulating mechanism is the annular airbag 12. The annular airbag 12 is made of high-temperature resistant (-20℃~150℃), oil-resistant, and aging-resistant nitrile rubber or fluororubber, with a wall thickness of 2mm. After inflation, its inner diameter can expand to 310mm (fitting the outer diameter of the reactor vessel). The outer side of the annular airbag 12 is fixedly connected to the inner wall of the jacket 6 via adhesive bonding or a pressure plate, while the inner side can be freely inflated. Two annular airbags 12 are installed in each temperature control zone, with a vertical spacing of 100mm, forming a double sealing barrier. A 1.5mm thick polytetrafluoroethylene sealing layer is also fixed to the outer side of the annular airbag 12 to ensure airtightness between it and the inner wall of the jacket after inflation.

[0027] The quantitative principle of flow rate regulation by the annular airbag 12: When compressed air is introduced into the annular air bladder 12, the air bladder expands inward, which is equivalent to increasing the outer radius of the reactor body. According to the fluid continuity equation, with the total flow rate in the inlet pipe remaining constant, the flow velocity in this region will increase within the head range of the circulating pump, and the heat transfer coefficient will increase accordingly. Therefore, by controlling the inflation pressure of the annular air bladder 12, the flow velocity of the circulating liquid in this temperature control zone can be precisely adjusted, thereby changing the convective heat transfer coefficient and achieving independent control of the heat transfer intensity in the temperature control zone.

[0028] When the annular airbag 12 is fully inflated (pressure 0.4 MPa, expands to fit against the outer wall of the reactor, and the gap is reduced to 0), the liquid flow in the temperature control zone is completely cut off, and the circulating liquid cannot pass through this zone and can only bypass from other zones.

[0029] The inflation assembly is used to independently inflate the annular airbags 12 in each temperature control zone and monitor the pressure. Its structure is as follows: Figure 4 As shown. The inflation assembly includes three pressure chambers 17, a pressure sensor 18, an inflation branch pipe 19, a first electrically controlled valve 20 (in this embodiment, it is a two-position three-way solenoid valve with a response time ≤0.5s), an inflation main pipe 21, and an air pump 22.

[0030] Each pressure chamber 17 corresponds to a temperature control zone. One end of the pressure chamber 17 is connected to the annular airbag 12 via a connecting pipe 8, and the other end is connected to the main inflation pipe 21 via an inflation branch pipe 19. Each inflation branch pipe 19 is equipped with a first electrically controlled valve 20, used to independently control the inflation and deflation of each temperature control zone. The main inflation pipe 21 is connected to the output end of the air pump 22. The pressure sensor 18 provides real-time feedback of the pressure of each airbag to the control system (PLC or microcontroller).

[0031] The controller automatically completes the switching through the following steps: Turn off the air pump 22; switch all electrically controlled valves 20 outside the target isolation zone to the venting position, and close them after 2 seconds; switch the electrically controlled valve 20 of the target isolation zone to the inflation position, start the air pump 22, read the value of the air pressure sensor 18 in real time, and close the electrically controlled valve 20 and stop the air pump when the pressure reaches the set threshold (such as 0.4MPa); at the same time, control the switching of the electric valve on the water outlet pipe.

[0032] To accurately monitor the temperature of materials at different heights within the reactor, a vertical rod 13 (a stainless steel pipe in this embodiment) is vertically installed inside the reactor body 1. The top of the rod 13 is fixedly connected to the cover 2 via threads. A first temperature sensor 14, a second temperature sensor 15, and a third temperature sensor 16 (PT100 platinum resistance thermometers in this embodiment, with an accuracy of ±0.1℃ and a measuring range of 0~150℃) are sequentially fixedly installed on the rod 13 from top to bottom. The installation heights of the three temperature sensors correspond one-to-one with the middle positions of the upper, middle, and lower temperature control zones of the jacket. The temperature sensor signals are connected to the control system for real-time display and recording.

[0033] Second electrically controlled valves are installed on the inlet pipe 7, the first outlet pipe 9, the second outlet pipe 10, and the third outlet pipe 11.

[0034] Working principle: The core working principle of this device is: by controlling the inflation degree of the annular airbag 12 in different temperature control zones, the flow path of the circulating liquid and the flow rate of each zone are changed, thereby forming a controllable temperature gradient along the height direction in the reactor, which facilitates the temperature control comparison experiment of dispersing blue bromide filter cake.

[0035] Normal working mode The control system keeps the second electrically controlled valve of the first outlet pipe 9 open, while the second electrically controlled valves of the second and third outlet pipes are closed. The annular air bladders 12 in all temperature control zones are not inflated (the air bladders are in a contracted state). The circulation pump is started, and the heating medium (or cooling medium) enters the bottom of the jacket from the inlet pipe 7, flowing sequentially through the lower, middle, and upper temperature control zones, finally exiting from the first outlet pipe 9 and returning to the circulation tank. At this time, the entire jacket cross-sectional area is at its maximum, the flow velocity is low, the heat exchange is gentle, and the overall temperature inside the vessel is uniform. Data measured by the three temperature sensors are used to monitor the base temperature.

[0036] Upper temperature-controlled isolation mode When a comparative experiment is required to conduct a test on the upper temperature control zone where there is no direct heat exchange effect, the control system performs the following operations: closes the second electrically controlled valves on the first water outlet pipe 9 and the third water outlet pipe 11, and only opens the second water outlet pipe 10.

[0037] Start the air pump 22 and open the first electrically controlled valve 20 corresponding to the upper temperature control zone to inflate the two annular air bladders 12 in the upper temperature control zone to a pressure of 0.4 MPa. The air bladders expand until they fit tightly against the outer wall of the reactor, completely isolating the liquid flow channel in the upper temperature control zone.

[0038] After entering through the inlet pipe 7, the circulating liquid can only flow through the lower and middle temperature control zones, and then flows out through the second outlet pipe 10. No circulating liquid flows through the upper temperature control zone; heat transfer relies solely on heat conduction from the reactor wall and natural convection from the materials inside the reactor.

[0039] At this point, the temperature detected by the first temperature sensor 14 will gradually deviate from the set value, while the second and third temperature sensors are still controlled by the circulating fluid. By recording the curves of the difference between the three temperature sensors over time, the rate of temperature change in the upper temperature control zone under the condition of losing forced heat exchange can be quantitatively evaluated, simulating the overheating phenomenon caused by local circulation blockage or bubble accumulation in actual production, thereby optimizing operating parameters.

[0040] Temperature-controlled isolation mode Similarly, when the annular airbag 12 in the middle temperature control zone is fully inflated and isolated, the control system closes the first and second water outlet pipes and opens the third water outlet pipe 11. The circulating fluid only flows through the lower temperature control zone and then flows out from the third water outlet pipe 11. No circulating fluid flows through the middle and upper temperature control zones. At this time, the second temperature sensor 15 (middle temperature control zone) and the first temperature sensor 14 (upper temperature control zone) will show different temperature rise rates, which can be used to analyze the impact of the middle section heat exchange failure.

[0041] Fine-tuned temperature control mode with partial inflation flow rate adjustment When it is not necessary to completely isolate a temperature control zone, but only to reduce the heat transfer intensity of that zone, the annular gasbag 12 can be partially inflated (e.g., at an inflation pressure of 0.2 MPa). At this time, the gasbag expands until the gap between it and the outer wall of the reactor vessel decreases, the cross-sectional area decreases, the flow velocity increases, and the convective heat transfer coefficient improves, thus enhancing heat transfer in that zone (if a heating medium is introduced, the temperature rises faster; if a cooling medium is introduced, the temperature drops faster). The inflation pressure can be adjusted via PID control, allowing continuous adjustment of the heat transfer capacity of each temperature control zone to achieve precise gradient temperature control.

[0042] Dispersed Blue Brominated Filter Cake Feeding Experimental Procedure A measured amount of the treatment solution is added to the reactor, stirring is started, and the circulating solution temperature is set.

[0043] A fixed amount of bromine filter cake was added, and the temperature was uniformly increased to the set temperature under normal conditions. The time taken for the three temperature sensors to reach steady state was recorded.

[0044] Switch to the upper temperature control zone isolation mode and continue running for 30 minutes, recording the temperature difference changes in the upper, middle, and lower temperature zones.

[0045] Deflate the airbag in the upper temperature control zone to restore normal operation, then switch to the middle temperature control zone isolation mode and repeat the experiment.

[0046] By comparing the temperature curves and filter cake dissolution effects under different modes, the optimal temperature control strategy was determined.

[0047] The above are merely specific embodiments of the present invention, but the scope of protection of the present invention is not limited thereto. The scope of protection of the present invention should be determined by the scope of the claims.

Claims

1. A temperature-controlled comparison device for dispersing blue bromide filter cake, comprising a reaction vessel (1), characterized in that: A jacket (6) is fixedly connected to the reactor body (1); a water inlet pipe (7) is fixedly connected to the bottom of the jacket (6), and a first water outlet pipe (9), a second water outlet pipe (10) and a third water outlet pipe (11) are fixedly connected to the side; the first water outlet pipe (9) is located at the top of the jacket (6), so that an upper temperature control zone is formed between the first water outlet pipe (9) and the second water outlet pipe (10), a middle temperature control zone is formed between the second water outlet pipe (10) and the third water outlet pipe (11), and a lower temperature control zone is formed between the third water outlet pipe (11) and the water inlet pipe (7); an adjustment mechanism for adjusting the liquid flow rate is provided in the upper temperature control zone, the middle temperature control zone and the lower temperature control zone.

2. The temperature control comparison device according to claim 1, characterized in that: The adjustment mechanism includes an inflation assembly, a connecting pipe (8), and an annular airbag (12). The outer side of the annular airbag (12) is fixedly connected to the inner wall of the jacket (6), one end of the connecting pipe (8) is fixedly connected to the annular airbag (12), and the other end is connected to the inflation assembly; the annular airbag (12) is configured to expand inward when inflated, reduce the liquid flow gap, and increase the liquid flow rate in the temperature control zone.

3. The temperature control comparison device according to claim 2, characterized in that: The number of the annular airbags (12) in each regulating mechanism is at least two; when the annular airbags (12) are fully inflated, their inner ends are in contact with the outer wall of the reactor body (1), thereby cutting off the flow of liquid; Under normal conditions, the second water outlet pipe (10) and the third water outlet pipe (11) are closed, and the liquid flows out from the first water outlet pipe (9). When the annular airbag (12) of the upper temperature control zone is fully inflated to isolate the temperature control zone, the first water outlet pipe (9) and the third water outlet pipe (11) are closed, and the liquid flows out from the second water outlet pipe (10). When the annular airbag (12) of the middle temperature control zone is fully inflated to isolate the temperature control zone, the first water outlet pipe (9) and the second water outlet pipe (10) are closed, and the liquid flows out from the third water outlet pipe (11).

4. The temperature control comparison device according to claim 3, characterized in that: A sealing layer is fixedly connected to the outside of the annular airbag (12).

5. The temperature control comparison device according to claim 1, characterized in that: The reactor body (1) is provided with a vertical rod (13), and a first temperature sensor (14), a second temperature sensor (15) and a third temperature sensor (16) are fixedly connected to the vertical rod (13). The first temperature sensor (14), the second temperature sensor (15), and the third temperature sensor (16) correspond one-to-one with the upper temperature control zone, the middle temperature control zone, and the lower temperature control zone, respectively.

6. The temperature control comparison device according to claim 5, characterized in that: The top of the reactor body (1) is connected to a cover (2), and the top of the vertical rod (13) is fixedly connected to the cover (2).

7. The temperature control comparison device according to claim 6, characterized in that: A motor (3) is fixedly connected to the cover (2), and a stirring shaft (4) is fixedly connected to the output end of the motor (3). A stirring paddle (5) is fixedly connected to the stirring shaft (4).

8. The temperature control comparison device according to claim 2, characterized in that: The inflation assembly includes three pressure chambers (17), a pressure sensor (18), an inflation branch pipe (19), an inflation main pipe (21), a first electrically controlled valve (20), and an air pump (22). Each of the pressure chambers (17) is fixedly connected to a pressure sensor (18); one end of each pressure chamber (17) is fixedly connected to the corresponding connecting pipe (8), and the other end is fixedly connected to the corresponding inflation branch pipe (19); each inflation branch pipe (19) is fixedly connected to a first electrically controlled valve (20), and each inflation branch pipe (19) is connected to the inflation main pipe (21); the inflation main pipe (21) is fixedly connected to the output end of the air pump (22).

9. The temperature control comparison device according to claim 1, characterized in that: A second electrically controlled valve is fixedly connected to each of the water inlet pipe (7) and each water outlet pipe.

10. The temperature control comparison device according to claim 1, characterized in that: The first water outlet pipe (9), the second water outlet pipe (10), and the third water outlet pipe (11) are all located on the same vertical plane.

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