A continuous flow apparatus for dye synthesis reactions
By combining a precooler, a tubular reactor group, and a circulating reactor, along with a refrigerant transfer port and a Y-shaped confluence structure, the problems of uneven mixing and inaccurate temperature control in the dye synthesis reaction were solved, achieving efficient continuous production and high product yield.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- HANGZHOU ANTHRACITE TECH CO LTD
- Filing Date
- 2025-08-05
- Publication Date
- 2026-07-24
Smart Images
Figure CN224541701U_ABST
Abstract
Description
Technical Field
[0001] This utility model belongs to the technical field of dye synthesis equipment, and more specifically, relates to a continuous flow device for dye synthesis reaction. Background Technology
[0002] Dye synthesis typically involves diazotization-coupling reactions, a process characterized by intense exothermic activity, rapid reaction rates, and numerous side reactions. Current methods primarily employ batch reactors that rely on mechanical stirring. The presence of concentration gradients in the reaction solution can easily lead to localized pH or temperature imbalances, increasing byproducts. Furthermore, the concentrated exothermic reaction results in low refrigerant heat exchange efficiency, impacting product yield. Some methods utilize semi-continuous flow devices, improving mixing efficiency through pipeline transport and partially achieving continuous operation. However, straight-tube reactors suffer from insufficient turbulence, leading to easy stratification of the reaction solution. Uneven refrigerant coverage in long pipelines results in a rapid temperature rise in the later stages of the reaction. Therefore, a continuous flow device for dye synthesis reactions that provides uniform mixing, improved product yield, and precise cooling is needed. Utility Model Content
[0003] The technical problem to be solved by this utility model is to provide a continuous flow device for dye synthesis reaction, which can meet the requirements of uniform mixing, improved product yield and precise cooling in the continuous flow device for dye synthesis reaction.
[0004] This utility model discloses a continuous flow device for dye synthesis reaction, comprising a precooler, a tubular reactor group, a circulating reactor, a circulating regulating pump, a diverting regulating pump, a diazo liquid input tank, and a reaction liquid storage tank. The inlet of the precooler is connected to the reaction liquid storage tank, and the outlet is connected to the inlet of the circulating regulating pump via a conveying pipeline. The diazo liquid input tank is connected to the inlet of the circulating regulating pump via a conveying pipeline. The outlet of the circulating regulating pump is connected to the inlet of the tubular reactor group via a conveying pipeline. A three-way valve is connected to the outlet of the tubular reactor group, and the other two ends of the three-way valve are respectively connected to the inlet of the circulating regulating pump and the inlet of the diverting regulating pump. The outlet of the diverting regulating pump is connected to the inlet of the circulating reactor via a conveying pipeline. The outlet of the circulating reactor can discharge qualified materials via a conveying pipeline. The closed-loop reaction of the tubular reactor group and the reaction diverted to the circulating reactor improve the uniformity of the reaction mixing and ensure complete reaction.
[0005] As a further improvement of this utility model, the tube reactor group consists of a first tube reactor and a second tube reactor connected in series through a U-shaped connecting pipe to form a closed loop. The outlet of the circulation regulating pump is connected to the bottom inlet of the first tube reactor, and the bottom outlet of the second tube reactor is returned to the circulation inlet of the circulation regulating pump through a conveying pipeline.
[0006] As a further improvement of this utility model, two circulating reactors are provided, and the two circulating reactors are connected in series.
[0007] As a further improvement of this utility model, the reaction liquid storage tank stores a reaction liquid composed of water, esterification liquid and additives, and the diazo liquid input tank stores diazo liquid. The reaction liquid and diazo liquid are mixed into a mixture by a circulation regulating pump. The mixing ratio of reaction liquid to diazo liquid in the mixture is 700:1. The ratio of the mixture is controlled by the output rate of the reaction liquid storage tank and the diazo liquid input tank.
[0008] As a further improvement of this utility model, the feed inlet of the circulating regulating pump adopts a Y-type confluence structure to fully mix the reaction liquid and diazo liquid, ensuring consistent delivery endpoints and reducing the error in the ratio of reaction liquid to diazo liquid. The diameter of the delivery pipeline between the precooler and the circulating regulating pump is equal to the diameter of the feed inlet of the circulating regulating pump. The ratio of the diameter of the delivery pipeline between the precooler and the circulating regulating pump to the diameter of the delivery pipeline between the diazo liquid input tank and the circulating regulating pump is 12.5:1. This is used to assist in the precise ratio of reaction liquid to diazo liquid, reduce the rate difference between the input liquid in the reaction liquid storage tank and the diazo liquid input tank, improve the mixing degree of the mixture, and thus improve the preparation efficiency of the dye slurry.
[0009] As a further improvement of this utility model, a spiral guide groove is provided on the inner wall of the U-shaped connecting pipe to prevent solid particles from depositing.
[0010] As a further improvement of this utility model, the ratio of the circulating flow rate of the reaction liquid in the tubular reactor group to the discharge flow rate pumped out by the diversion regulating pump is 1:0.02, ensuring that the mixture can fully react in the tubular reactor group; the impeller diameter ratio of the circulating regulating pump to the diversion regulating pump is 5:1, reducing the speed difference between the circulating regulating pump and the diversion regulating pump, and reducing the driving energy consumption to meet the ratio of circulating flow rate to discharge flow rate.
[0011] As a further improvement of this utility model, it also includes two sets of refrigerant transfer ports. One set of refrigerant transfer ports is opened on the precooler to cool the reaction liquid, and the other set is opened on the tube reactor group to remove the heat generated by the reaction. The temperature of the two sets of refrigerant transfer ports is controlled in separate zones to achieve precise cooling of different components of the device. The refrigerant temperature on the precooler and the refrigerant temperature on the tube reactor group are not greater than -15℃.
[0012] As a further improvement of this invention, the temperature of the reaction liquid is 5°C when it is transported after being cooled in the precooler, so as to improve the reaction efficiency.
[0013] As a further improvement of this utility model, the proportion of esterification liquid in the reaction solution is 0.12%, the proportion of auxiliary agent is 0.003%, and the balance is water.
[0014] Compared with the prior art, the beneficial effects of this utility model are as follows: through the coordinated operation of the precooler, the tubular reactor group and the circulating reactor, the continuous production of dye synthesis reaction is realized, and the combination of closed-loop circulation and diversion regulation is used to improve the uniformity of reaction mixing. Two circulating reactors are connected in series to lengthen the flow path and reaction time of the mixture, ensuring a complete reaction. A refrigerant inlet is provided to pre-cool the reaction solution and remove heat generated during the reaction. Temperature control is implemented in two separate refrigerant inlets for precise cooling of different components. The inlet of the circulating regulating pump uses a Y-shaped confluence structure to thoroughly mix the reaction solution and diazo solution, ensuring consistent delivery endpoints and reducing errors in the ratio of reaction solution to diazo solution. The diameter ratio of the delivery pipeline between the precooler and the circulating regulating pump to that between the diazo solution input tank and the circulating regulating pump is 12.5:1, assisting in precise mixing of the reaction solution and diazo solution, reducing the rate difference between the input liquid in the reaction solution storage tank and the diazo solution input tank, improving the mixing degree of the mixture, and thus increasing the preparation efficiency of the dye slurry. A spiral guide groove is formed on the inner wall of the U-shaped connecting pipe to prevent solid particle deposition. Attached Figure Description
[0015] Figure 1 This is a schematic diagram of the structure of this utility model; Figure 2 For the present utility model Figure 1 Enlarged view of region A in the middle; Figure 3 This is a schematic diagram of the structure of the tubular reactor group of this utility model; Figure 4 For the present utility model Figure 3 Enlarged cross-sectional view of region B in the middle.
[0016] Explanation of the labels in the diagram: Precooler 1; Tube reactor group 2; First tube reactor 21; Second tube reactor 22; U-shaped connecting pipe 23; Circulating reactor 3; Circulating regulating pump 4; Flow regulating pump 5; Diazo liquid input tank 6; Refrigerant transfer port 7; Reaction liquid storage tank 8; First delivery pipeline L1; Second delivery pipeline L2; Third delivery pipeline L3; Fourth delivery pipeline L4; Fifth delivery pipeline L5. Detailed Implementation
[0017] Specific Implementation Example 1: Please refer to Figures 1-4This utility model relates to a continuous flow device for dye synthesis reaction, including a precooler 1, a tubular reactor group 2, a circulating reactor 3, a circulating regulating pump 4, a split regulating pump 5, a diazo liquid input tank 6, and a reaction liquid storage tank 8. For ease of description, the connecting pipelines between the various structures are sequentially represented by the first conveying pipeline L1 to the fifth conveying pipeline L5 according to the process sequence. The inlet of the precooler 1 is connected to the reaction liquid storage tank 8, and the outlet is connected to the inlet of the circulating regulating pump 4 through the first conveying pipeline L1. The reaction liquid storage tank 8 stores the reaction liquid composed of water, esterification liquid, and auxiliaries. The diazo liquid input tank 6 is connected to the reaction liquid storage tank 8 through the second conveying pipeline L2. The inlet of the circulating regulating pump 4 is connected to the diazo liquid input tank 6, which stores diazo liquid. The reaction liquid and diazo liquid are mixed into a mixture after passing through the circulating regulating pump 4. The outlet of the circulating regulating pump 4 is connected to the inlet of the tubular reactor group 2 through the third conveying pipeline L3. The outlet of the tubular reactor group 2 is connected to a three-way valve. One end of the other two ends of the three-way valve is connected to the inlet of the circulating regulating pump 4 through the fourth conveying pipeline L4, and the other end is connected to the inlet of the diversion regulating pump 5. The outlet of the diversion regulating pump 5 is connected to the bottom inlet of the circulating reactor 3 through the fifth conveying pipeline L5. The top product outlet of the circulating reactor 3 discharges qualified materials through the conveying pipeline.
[0018] In a further embodiment, such as Figure 1 As shown, there are two circulating reactors 3 connected in series, which lengthens the flow path and reaction time of the mixture to ensure a complete reaction.
[0019] In a further embodiment, such as Figures 3-4 As shown, the tubular reactor group 2 consists of a first tubular reactor 21 and a second tubular reactor 22 connected in series via a U-shaped connecting pipe 23 to form a closed loop. The outlet of the circulation regulating pump 4 is connected to the bottom inlet of the first tubular reactor 21 via a third conveying pipe L3, and the bottom outlet of the second tubular reactor 22 is returned to the circulation inlet of the circulation regulating pump 4 via a fourth conveying pipe L4. The inner wall of the U-shaped connecting pipe 23 is provided with a spiral guide groove to prevent solid particles from depositing.
[0020] In a further embodiment, such as Figure 1 As shown, in the tubular reactor group 2, the reaction liquid and diazonium liquid form a mixture and react, wherein the ratio of the reaction liquid to the diazonium liquid is 700:1.
[0021] In a further embodiment, such as Figure 2 As shown, the inlet of the circulating regulating pump 4 adopts a Y-type confluence structure to fully mix the reaction liquid and the diazo liquid, ensuring consistent delivery endpoints and reducing the error in the ratio of reaction liquid to diazo liquid. The diameter D1 of the first delivery pipeline L1 is equal to the diameter d of the inlet of the circulating regulating pump 4, and the ratio of the diameter D1 of the first delivery pipeline L1 to the diameter D2 of the second delivery pipeline L2 is D1:D2=12.5:1, which is used to assist in the accurate ratio of diazo liquid.
[0022] In a further embodiment, such as Figure 1 As shown, the ratio of the circulating flow rate of the reaction liquid in the tubular reactor group 2 to the discharge flow rate pumped out by the diversion regulating pump 5 is 1:0.02.
[0023] In a further embodiment, such as Figure 1 As shown, it also includes two sets of refrigerant transfer ports 7. One set of refrigerant transfer ports 7 is opened on the precooler 1 to precool the reaction liquid, and the other set is opened on the tube reactor group 2 to remove the heat generated by the reaction. The temperature of the two sets of refrigerant transfer ports 7 is controlled in separate zones to achieve precise cooling of different components of the device. The refrigerant temperature on the precooler 1 and the refrigerant temperature on the tube reactor group 2 are not greater than -15℃.
[0024] In a further embodiment, such as Figure 1 As shown, the reaction solution is cooled to 5°C in the precooler 1 and then transferred to the inlet of the circulation regulating pump 4 to improve the reaction efficiency.
[0025] In a further embodiment, such as Figure 1 As shown, the esterification solution accounts for 0.12% of the reaction solution, the auxiliary agent accounts for 0.003%, and the remainder is water.
[0026] The reaction solution, composed of water, esterification liquid, and additives, is fed from the reaction solution storage tank 8 into the precooler 1. The refrigerant cools the precooler 1 through the refrigerant transfer port 7. After being cooled in the precooler 1, the reaction solution is transferred to the inlet of the circulation regulating pump 4 through the first transfer pipeline L1. At the same time, the diazo liquid is transferred from the diazo liquid input tank 6 to the inlet of the circulation regulating pump 4 through the second transfer pipeline L2. The mixture of the two is circulated back and forth in the tube reactor group 2 under the drive of the circulation regulating pump 4 and reacts. Meanwhile, the refrigerant cools the tube reactor group 2 through the refrigerant transfer port 7. After the reaction stabilizes, the split regulating pump 5 pumps out part of the mixture from the tube reactor group 2 and transfers it to the two circulating reactors 3 through the fifth transfer pipeline L5 to continue the reaction until the reaction is complete and qualified dye slurry is produced. The qualified dye slurry is discharged from the product outlet at the top of the circulating reactor 3.
Claims
1. A continuous flow apparatus for dye synthesis reaction, characterized in that: The reactor includes a precooler (1), a tubular reactor group (2), a circulating reactor (3), a circulating regulating pump (4), a diverting regulating pump (5), a diazonium liquid input tank (6), and a reaction liquid storage tank (8). The inlet of the precooler (1) is connected to the reaction liquid storage tank (8), and the outlet is connected to the inlet of the circulating regulating pump (4) through a conveying pipeline. The diazonium liquid input tank (6) is connected to the inlet of the circulating regulating pump (4) through a conveying pipeline. The outlet of the circulating regulating pump (4) is connected to the inlet of the tubular reactor group (2) through a conveying pipeline. The outlet of the tubular reactor group (2) is connected to a three-way valve. The other two ends of the three-way valve are connected to the inlet of the circulating regulating pump (4) and the inlet of the diverting regulating pump (5), respectively. The outlet of the diverting regulating pump (5) is connected to the inlet of the circulating reactor (3) through a conveying pipeline. The outlet of the circulating reactor (3) can discharge qualified materials through a conveying pipeline.
2. The continuous flow apparatus for dye synthesis reaction according to claim 1, characterized in that: The tubular reactor group (2) consists of a first tubular reactor (21) and a second tubular reactor (22) connected in series via a U-shaped connecting pipe (23) to form a closed loop. The outlet of the circulation regulating pump (4) is connected to the bottom inlet of the first tubular reactor (21), and the bottom outlet of the second tubular reactor (22) returns to the inlet of the circulation regulating pump (4).
3. The continuous flow apparatus for dye synthesis reaction according to claim 1, characterized in that: There are two circulating reactors (3), and the two circulating reactors (3) are connected in series.
4. The continuous flow apparatus for dye synthesis reaction according to claim 1, characterized in that: The feed inlet of the circulating regulating pump (4) adopts a Y-type confluence structure, wherein the diameter of the conveying pipeline between the precooler (1) and the circulating regulating pump (4) is equal to the diameter of the feed inlet of the circulating regulating pump (4), and the ratio of the diameter of the conveying pipeline between the precooler (1) and the circulating regulating pump (4) to the diameter of the conveying pipeline between the diazonium liquid input tank (6) and the circulating regulating pump (4) is 12.5:
1.
5. The continuous flow apparatus for dye synthesis reaction according to claim 1, characterized in that: The impeller diameter ratio of the circulating regulating pump (4) to the diversion regulating pump (5) is 5:
1.
6. The continuous flow apparatus for dye synthesis reaction according to claim 1, characterized in that: It also includes two sets of refrigerant transfer ports (7), one set of refrigerant transfer ports (7) is located on the precooler (1), and the other set is located on the tubular reactor group (2).
7. The continuous flow apparatus for dye synthesis reaction according to claim 1, characterized in that: The inner wall of the U-shaped connecting pipe (23) is provided with a spiral guide groove.