Separation single-tower operation device for producing high-purity dicyclopentadiene

By using a single-tower operation device and a waste heat recovery design for heat exchangers, the problems of high energy consumption and scale formation in the production of high-purity dicyclopentadiene have been solved, achieving high-purity separation and cost reduction.

CN224009053UActive Publication Date: 2026-03-20FUSHUN YIKESI NEW MATERIAL
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2025-04-15
Publication Date
2026-03-20

AI Technical Summary

Technical Problem

Existing technologies for producing high-purity dicyclopentadiene involve high energy consumption, numerous equipment, and high costs. The condenser is prone to scale formation, and waste heat is not effectively utilized, leading to increased production costs.

Method used

A single-tower operation device is adopted to separate dicyclopentadiene by removing light components at the top of the tower, removing heavy components at the bottom of the tower, and extracting it from the side stream. Combined with the heat exchanger to recover the waste heat of the reboiler, a segmented condenser is designed to avoid scale formation.

Benefits of technology

The separation of high-purity dicyclopentadiene was achieved, reducing production costs and energy consumption, decreasing the frequency of scale formation, and improving production efficiency.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model discloses a separation single-tower operation device for producing high-purity dicyclopentadiene, which comprises a rectifying tower, one side of the middle of the rectifying tower is communicated and connected with a heat exchanger, the input end of the heat exchanger is communicated and connected with a first feeding pipe, the bottom of the rectifying tower is communicated and connected with a reboiler, and the reboiler is communicated and connected with the heat exchanger. The output end of the reboiler is communicated and connected to the rectifying tower; according to the dicyclopentadiene refining device disclosed by the utility model, dicyclopentadiene is refined by utilizing a single tower, and impurities in dicyclopentadiene are effectively removed by adopting modes of tower top light component removal, tower kettle heavy component removal and side line extraction, so that the purity of separated dicyclopentadiene can reach more than 98%, and the production cost is effectively reduced compared with a double-tower process; the waste heat of the reboiler is recycled through the heat exchanger, so that the production energy consumption is effectively reduced; and the condenser adopts a sectional cooling design, so that scale substances can be prevented from being separated out due to over-high temperature, the generation of scale is slowed down, and the maintenance frequency and investment are reduced.
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Description

Technical Field

[0001] This utility model relates to the field of chemical technology, and in particular to a single-tower operating device for separating high-purity dicyclopentadiene during production. Background Technology

[0002] In the production of high-purity dicyclopentadiene, existing technologies generally use a dual-tower system to remove light and heavy components from the depolymerized and dimerized dicyclopentadiene in C9. However, this method is not only energy-intensive but also requires numerous pieces of equipment, leading to increased costs. Furthermore, condensers and reboilers are indispensable components in the entire high-purity dicyclopentadiene production process. In existing technologies, industrial water is commonly used as the coolant in condensers. During actual operation, since condensers typically have only one inlet and one outlet, the water temperature gradually increases along the flow direction, resulting in a higher temperature at the outlet. This causes calcium carbonate, originally dissolved in the water, to precipitate due to reduced solubility, forming scale on the heat exchange surface of the condenser. The scale formation severely affects the condenser's condensation efficiency, necessitating increased maintenance frequency and investment to maintain production efficiency, further increasing production costs. Simultaneously, the waste heat generated during the operation of existing reboilers is not effectively recovered and utilized, but is directly released into the environment, resulting in significant waste of thermal energy and exacerbating energy consumption. Utility Model Content

[0003] The purpose of this invention is to provide a single-tower operating device for the separation of high-purity dicyclopentadiene in production, so as to solve the problems mentioned in the background art.

[0004] To solve the above-mentioned technical problems, this utility model provides the following technical solution: a single-tower operating device for separating high-purity dicyclopentadiene, comprising a distillation column, a heat exchanger being conductively connected to one side of the middle section of the distillation column, a first feed pipe being conductively connected to the input end of the heat exchanger, a reboiler being conductively connected to the bottom of the distillation column and being conductively connected to the heat exchanger, the output end of the reboiler being conductively connected to the distillation column, a condenser being conductively connected to the top of the distillation column, a reflux tank being conductively connected to the output end of the condenser, and the output end of the reflux tank being conductively connected to the distillation column.

[0005] Preferably, the reboiler input is connected to a first collection tank, the reflux tank output is connected to a second collection tank, the distillation column output is connected to a third collection tank on the other side of the middle section, and the condenser output is connected to a fourth collection tank.

[0006] Preferably, the condenser includes a shell, a tube bundle, a second feed pipe, a discharge pipe, a baffle plate, a baffle plate, a main drain pipe, a branch drain pipe, a main inlet water pipe, and a branch inlet water pipe. The tube bundle is fixedly connected inside the shell, and multiple baffle plates are connected inside the shell. Multiple baffle plates are provided between two adjacent baffle plates, and the tube bundle is fixedly connected to the baffle plates and the baffle plates.

[0007] Preferably, a drainage branch pipe is provided on one side of the partition, and a water inlet branch pipe is provided on one side of the drainage branch pipe, and the water inlet branch pipe and the drainage branch pipe are connected and fixed to the pipe shell.

[0008] Preferably, a main drain pipe is provided on one side of the pipe shell, and a branch drain pipe is connected and fixed to the main drain pipe. A main inlet pipe is provided on one side of the main drain pipe, and a branch inlet pipe is connected and fixed to the main inlet pipe.

[0009] Preferably, a second feed pipe is connected and fixed at one end of the tube shell, and a discharge pipe is connected and fixed at the other end of the tube shell.

[0010] This invention provides a single-tower operating device for separating high-purity dicyclopentadiene. Its advantages are as follows: This invention utilizes a single-tower purification process for dicyclopentadiene, employing a method of removing light impurities at the top of the tower, removing heavy impurities from the bottom, and using side stream extraction to effectively remove impurities from the dicyclopentadiene. This results in a dicyclopentadiene purity of over 98%, significantly reducing production costs compared to a dual-tower process. Furthermore, the waste heat from the reboiler is recovered and utilized through a heat exchanger, effectively reducing energy consumption. The condenser adopts a segmented cooling design, which avoids scale precipitation due to excessively high temperatures, thus slowing down scale formation and reducing maintenance frequency and investment. Attached Figure Description

[0011] To more clearly illustrate the technical solutions in the embodiments of this utility model or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0012] Figure 1 This is a block diagram of the overall structure of this utility model;

[0013] Figure 2 This is a schematic diagram of the main sectional view of the condenser of this utility model;

[0014] Figure 3 This is a schematic diagram of the three-dimensional cross-sectional structure of the tube shell of this utility model.

[0015] In the diagram: 1. Distillation column; 11. Heat exchanger; 12. First feed pipe; 13. Reboiler; 14. First collection tank; 15. Reflux tank; 16. Second collection tank; 17. Third collection tank; 18. Fourth collection tank; 2. Condenser; 21. Shell and tube; 22. Tube bundle; 23. Second feed pipe; 24. Discharge pipe; 25. Baffle plate; 26. Baffle plate; 27. Main drain pipe; 28. Branch drain pipe; 29. ​​Main water inlet pipe; 210. Branch water inlet pipe. Detailed Implementation

[0016] To make the objectives, technical solutions, and advantages of the embodiments of this utility model clearer, the technical solutions of the embodiments of this utility model will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this utility model, not all embodiments. Based on the embodiments of this utility model, all other embodiments obtained by those skilled in the art without creative effort are within the protection scope of this utility model.

[0017] Please see the appendix Figure 1 -Appendix Figure 3This utility model provides an embodiment of a single-tower operating device for the separation of high-purity dicyclopentadiene, comprising a distillation column 1, a heat exchanger 11 connected to one side of the middle section of the distillation column 1, a first feed pipe 12 connected to the input end of the heat exchanger 11, a reboiler 13 connected to the bottom of the distillation column 1 and connected to the heat exchanger 11, and an output end of the reboiler 13 connected to the distillation column 1, a condenser 2 connected to the top of the distillation column 1, a reflux tank 15 connected to the output end of the condenser 2 and connected to the output end of the reflux tank 15, and the distillation column 1 is used to distill the dimerized dicyclopentadiene. The device utilizes temperature and pressure control at different locations. The distillation column 1 is constructed by applying force to the light components, causing them to rise to the top and the heavy components to settle to the bottom, thus separating dicyclopentadiene from impurities. A high-purity dicyclopentadiene product is collected via a side stream. The condenser 2 cools and liquefies the gaseous light components. The heat exchanger 11 uses the heat from the reboiler 13 to preheat the material entering the distillation column 1. The first feed pipe 12 delivers the dimerized dicyclopentadiene material to the distillation column 1. The reboiler 13 heats the material in the bottom of the distillation column 1, providing heat for the distillation process, causing the material to vaporize and rise, maintaining gas-liquid balance and mass and heat transfer within the column. The reflux tank 15 stores the material liquefied by the condenser 2. The input of the reboiler 13 is connected to the first collection tank 14, and the output of the reflux tank 15... The first collection tank 14 is used to collect heavy components drawn from the bottom of the distillation column 1; the second collection tank 16 is used to collect part of the material output from the reflux tank 15; the third collection tank 17 is used to collect high-purity dicyclopentadiene product drawn from the side stream of the distillation column 1; and the fourth collection tank 18 is used to collect incompletely condensed light vapor components. The condenser 2 includes a shell 21, a tube bundle 22, a second feed pipe 23, a discharge pipe 24, a baffle 25, a baffle plate 26, a main drain pipe 27, a branch drain pipe 28, a main water inlet pipe 29, and a branch water inlet pipe 2000. 10. A tube bundle 22 is fixedly connected inside the tube shell 21. Multiple baffles 25 are connected inside the tube shell 21. Multiple baffles 26 are arranged between two adjacent baffles 25. The tube bundle 22 is fixedly connected to the baffles 25 and the baffles 26. The tube shell 21 is used to contain cooling water. The tube bundle 22 is used to transport gaseous light components. The baffles 25 are used to divide the inside of the tube shell 21 into multiple sections. The baffles 26 are used to guide the flow of cooling water. A drain branch pipe 28 is arranged on one side of the baffle 25. A water inlet branch pipe 210 is arranged on one side of the drain branch pipe 28. The water inlet branch pipe 210 and the drain branch pipe 28 are fixedly connected to the tube shell 21. The drain branch pipe 28 is used to drain cooling water. The water inlet branch pipe 210 is used to inlet cooling water.A main drain pipe 27 is provided on one side of the casing 21, and a branch drain pipe 28 is connected and fixed to the main drain pipe 27. A main inlet pipe 29 is provided on one side of the main drain pipe 27, and a branch inlet pipe 210 is connected and fixed to the main inlet pipe 29. The main drain pipe 27 is the common drain end of the branch drain pipe 28, and the main inlet pipe 29 is the common inlet end of the branch inlet pipe 210. A second feed pipe 23 is connected and fixed to one end of the casing 21, and a discharge pipe 24 is connected and fixed to the other end of the casing 21. The second feed pipe 23 is used for the input of gaseous light components, and the discharge pipe 24 is used for the output of liquid components.

[0018] Working principle: When using this invention, the dimerized dicyclopentadiene enters the heat exchanger 11 through the first feed pipe 12. The heat exchanger 11 uses the residual heat of the reboiler 13 to preheat the material. The preheated material enters the middle of the distillation column 1. After entering the distillation column 1, the material undergoes separation within the column. The top temperature is controlled at 89±3℃, the top pressure is -90±5KPa, the bottom temperature is 100±5℃, and the bottom pressure is -88±5KPa. Under these temperature and pressure conditions, light components such as cyclopentadiene and methylcyclopentadiene rise to the top of the column, and the recombining components... Substances such as methylcyclopentadiene dimer settle to the bottom of the column. The reboiler 13 heats the material in the bottom of the column, providing heat for the distillation process, causing the material to continuously vaporize and rise, maintaining the gas-liquid balance and mass and heat transfer processes within the distillation column 1. The rising light vapor components from the top of the column enter the condenser 2, which cools and liquefies them. The liquefied material enters the reflux tank 15. A portion of the material returns to the top of the distillation column 1 as reflux liquid, maintaining stable distillation operations within the column 1. The reflux temperature is controlled at 45±3℃. The other portion of the material enters the second recovery tank through the outlet of the reflux tank 15. The material is collected in collecting tank 16. After distillation separation, the heavy components are collected from the bottom of the column and enter the first collecting tank 14. The dicyclopentadiene product is collected from the side stream and enters the third collecting tank 17. Some material from the output of condenser 2 also enters the fourth collecting tank 18. This material is part of the incompletely condensed gaseous substance from the light components collected from the top of the column. The dicyclopentadiene product collected from the third collecting tank 17 has a purity of over 98%. In condenser 2, baffles 25 divide the shell 21 into multiple sections. Each section is equipped with baffles 26 to guide the flow of cooling water. The cooling water flows through the main inlet pipe 2. 9 enters the inlet branch pipe 210, and after heat exchange, flows from the drain branch pipe 28 into the drain main pipe 27. The gaseous light components enter the tube bundle 22 through the second feed pipe 23. After heat exchange, the generated liquid components are discharged through the discharge pipe 24. By designing the number and spacing of baffles 25 and the number of baffles 26 in each section, the temperature of the cooling water discharged from the drain branch pipe 28 can be close to and lower than the precipitation temperature of scale, thereby slowing down the condensation of scale inside the condenser 2. The specific operating control parameters of the distillation column 1 are shown in Table 1, and the composition of the refined dicyclopentadiene is shown in Table 2.

[0019] Table 1 Refining Operation Control Parameters

[0020] Control Project parameter unit Tower top temperature 89±3 ℃ Tower top pressure -90±5 kPa Feed rate 2500 kg / h Lateral extraction volume 2000 kg / h Top liquid discharge rate 48.07 kg / h Top gas discharge rate 301.93 kg / h Pipe yield 150.0 kg / h Return traffic 2275 kg / h Reflux temperature 45±3 ℃ Tower temperature 100±5 ℃ Side line temperature 92±3 ℃ Tower pressure -88±5 kPa

[0021] Table 2. Composition of purified dicyclopentadiene

[0022] Components content(%) Dicyclopentadiene 98.78 cyclopentadiene 0.03 Between methylcyclopentadiene and bicyclic 0.66 Between dicyclopentadiene and methylcyclopentadiene dimers 0.09 methylcyclopentadiene dimer 0.39 After methylcyclopentadiene dimer 0.02 Trimer -

[0023] In the description of this utility model, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "joining" should be interpreted broadly. For example, they can refer to a connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this utility model based on the specific circumstances.

[0024] The device embodiments described above are merely illustrative. The units described as separate components may or may not be physically separate. The components shown as units may or may not be physical units; that is, they may be located in one place or distributed across multiple network units. Some or all of the modules can be selected to achieve the purpose of this embodiment according to actual needs. Those skilled in the art can understand and implement this without any creative effort.

[0025] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of this utility model, and not to limit it. Although this utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of this utility model.

Claims

1. A single-tower operating apparatus for the separation of high-purity dicyclopentadiene, comprising a distillation column (1), characterized in that: A heat exchanger (11) is connected to one side of the middle section of the distillation column (1). The input end of the heat exchanger (11) is connected to the first feed pipe (12). A reboiler (13) is connected to the bottom of the distillation column (1) and is connected to the heat exchanger (11). The output end of the reboiler (13) is connected to the distillation column (1). A condenser (2) is connected to the top of the distillation column (1). The output end of the condenser (2) is connected to the reflux tank (15) and is connected to the output end of the reflux tank (15).

2. The single-tower operating device for separating high-purity dicyclopentadiene according to claim 1, characterized in that: The reboiler (13) is connected to the first collection tank (14) at the input end, the reflux tank (15) is connected to the second collection tank (16) at the output end, the distillation column (1) is connected to the third collection tank (17) on the other side of the middle section, and the condenser (2) is connected to the fourth collection tank (18) at the output end.

3. A single-tower operating device for separating high-purity dicyclopentadiene according to claim 2, characterized in that: The condenser (2) includes a shell (21), a tube bundle (22), a second feed pipe (23), a discharge pipe (24), a baffle (25), a baffle (26), a main drain pipe (27), a branch drain pipe (28), a main inlet pipe (29), and a branch inlet pipe (210). The tube bundle (22) is fixedly connected inside the shell (21). Multiple baffles (25) are connected inside the shell (21). Multiple baffles (26) are provided between two adjacent baffles (25), and the tube bundle (22) is fixedly connected to the baffles (25) and the baffles (26).

4. A single-tower operating device for separating high-purity dicyclopentadiene according to claim 3, characterized in that: A drainage branch pipe (28) is provided on one side of the partition (25), and an inlet branch pipe (210) is provided on one side of the drainage branch pipe (28). The inlet branch pipe (210) and the drainage branch pipe (28) are connected and fixed on the pipe shell (21).

5. A single-tower operating device for separating high-purity dicyclopentadiene according to claim 4, characterized in that: A main drain pipe (27) is provided on one side of the casing (21), and a branch drain pipe (28) is connected and fixed to the main drain pipe (27). A main inlet pipe (29) is provided on one side of the main drain pipe (27), and a branch inlet pipe (210) is connected and fixed to the main inlet pipe (29).

6. A single-tower operating device for separating high-purity dicyclopentadiene according to claim 5, characterized in that: One end of the tube shell (21) is connected to and fixed with a second feed pipe (23), and the other end of the tube shell (21) is connected to and fixed with a discharge pipe (24).