Vertical recovery tank for recycling ethyl acetate raffinate

Abstract

The utility model relates to the technical field of ethyl acetate, in particular to a vertical recovery tank for recycling ethyl acetate raffinate, which comprises a tank body, a feed port, a discharge port, a stirring component and a heating component, the tank body is of a three-layer coaxial vertical structure and sequentially comprises a raffinate concentration layer, a distillation layer and a fine filtration layer from bottom to top, annular partition plates are fixedly arranged between every two adjacent layers for sealing connection, first flow guide holes are formed in the annular partition plates, preliminary concentration, azeotropic separation and deep purification are achieved through a three-stage structure of the residual liquid concentration layer, the distillation layer and the refined filtration layer, and the residual liquid concentration layer can remove part of water through stirring and heating; the distillation layer separates azeotropic components at a specific temperature by utilizing the azeotropic characteristic of ethyl acetate, ethanol and water, the refined filtration layer further removes residual impurities through physical adsorption or chemical treatment, and the final purity can break through the 95% bottleneck of traditional single-stage distillation and meet the high-purity requirements of medicine, electronics and the like.

Description

Technical Field

[0001] This utility model relates to the field of ethyl acetate technology, specifically a vertical recovery tank for the recycling of ethyl acetate residue. Background Technology

[0002] As is well known, ethyl acetate, as an important organic solvent, is widely used in the synthesis, extraction and cleaning processes of pharmaceuticals, pesticides, coatings and other industries. The ethyl acetate residue generated during the production process usually contains ethyl acetate, ethanol, water and high-boiling-point impurities. If it is discharged directly, it will not only waste resources, but also pollute the environment.

[0003] Existing equipment is mostly a single-stage separation device, lacking a multi-stage synergistic separation mechanism of coarse filtration, fine filtration, and stratification. Ethyl acetate easily forms binary and ternary azeotropic mixtures with ethanol and water. For example, the boiling point of ethyl acetate-ethanol azeotrope is 71.8℃, and the boiling point of ethyl acetate-water azeotrope is 70.4℃. Traditional single-stage distillation columns cannot break the azeotropic equilibrium, resulting in excessive ethanol and water content in the recovered products, with a purity generally <95%, which cannot meet the reuse requirements of high-end fields such as pharmaceuticals and electronics. Utility Model Content

[0004] Technical problems to be solved

[0005] To overcome the problem that existing vertical recovery tanks for ethyl acetate residue recovery lack multi-stage synergistic separation, this invention provides a vertical recovery tank for ethyl acetate residue recovery that can perform multi-stage synergistic separation.

[0006] Technical solution

[0007] To achieve the above objectives, this utility model provides the following technical solution: a vertical recovery tank for the recycling of ethyl acetate residue, comprising:

[0008] The tank body is a three-layer coaxial vertical structure, consisting of a residual liquid concentration layer, a distillation layer, and a fine filtration layer from bottom to top. Each layer is fixedly connected by an annular partition, and the annular partition has a first flow guide hole.

[0009] A feed inlet is located at the top of the tank.

[0010] A discharge port is located at the bottom of the tank.

[0011] A stirring assembly, the stirring assembly being installed inside the tank; and

[0012] A heating assembly is installed inside the tank.

[0013] Preferably, the stirring assembly includes a stirring shaft that penetrates three layers of the tank body. A spiral scraper blade is fixedly installed at the bottom of the stirring shaft, an inclined blade is fixedly installed in the middle of the stirring shaft, and a guide spiral is fixedly installed at the top of the stirring shaft. A mounting plate is fixedly installed at the top of the tank body, and a motor is fixedly installed on the mounting plate. The output shaft of the motor is connected to the stirring shaft by a key.

[0014] Furthermore, the heating assembly includes a spiral coil and a jacket. The spiral coil is installed on the inner wall of the distillation layer, and a placement hole is provided at the position of the residual liquid concentration layer. The jacket is installed in the placement hole.

[0015] Furthermore, a sintered metal filter element is detachably installed within the fine filtration layer, and the sintered metal filter element is slidably installed with respect to the tank body.

[0016] In a further embodiment, the residual liquid concentration layer has a conical bottom structure, and the spiral scraper blades are adapted to the bottom of the residual liquid concentration layer.

[0017] Based on the aforementioned scheme, a steam hole is fixedly provided on the top of the tank, a conveying pipe is installed on the steam hole, and a vertical condensing tower is fixedly provided at the bottom of the conveying pipe.

[0018] Furthermore, based on the aforementioned scheme, the feed inlet is located at the top of the fine filtration layer, and a liquid distributor is fixedly installed inside the feed inlet. The liquid distributor has a straight pipe structure, and a second guide hole is evenly opened at the bottom of the liquid distributor. The discharge outlet is located in the middle of the distillation layer.

[0019] Furthermore, based on the aforementioned scheme, a sight glass is provided between the residual liquid concentration layer, the distillation layer, and the fine filtration layer.

[0020] Beneficial effects

[0021] This vertical recovery tank for ethyl acetate residue recycling uses a three-stage structure consisting of a residue concentration layer, a distillation layer, and a fine filtration layer to achieve preliminary concentration, azeotropic separation, and deep purification, respectively. The residue concentration layer can remove some water through stirring and heating. The distillation layer utilizes the azeotropic properties of ethyl acetate with ethanol and water to separate the azeotropic components at a specific temperature. The fine filtration layer further removes residual impurities through physical adsorption or chemical treatment. The final purity can break through the 95% bottleneck of traditional single-stage distillation, meeting the high purity requirements of pharmaceuticals, electronics, and other industries. Attached Figure Description

[0022] Figure 1 This is a side view of the structure of this utility model;

[0023] Figure 2 This is a schematic diagram of the vertical condensing tower of this utility model;

[0024] Figure 3 This is a schematic diagram of the structure of the sight glass of this utility model;

[0025] Figure 4 This is a schematic diagram of the internal structure of the tank body of this utility model;

[0026] Figure 5 This is a schematic diagram of the structure of the stirring assembly of this utility model;

[0027] Figure 6 This is a schematic diagram of the structure of the annular partition of this utility model;

[0028] Figure 7 This utility model Figure 6 A magnified schematic diagram of the structure at point A in the middle.

[0029] In the diagram: 1. Tank body; 2. Concentration layer; 3. Distillation layer; 4. Fine filtration layer; 5. Annular baffle; 6. First guide hole; 7. Inlet; 8. Outlet; 9. Stirring assembly; 10. Heating assembly; 11. Stirring shaft; 12. Spiral scraper blade; 13. Inclined blade; 14. Guide spiral; 15. Mounting plate; 16. Motor; 17. Spiral coil; 18. Jacket; 19. Placement hole; 20. Sintered metal filter element; 21. Steam hole; 22. Conveying pipe; 23. Vertical condenser; 24. Liquid distributor; 25. Second guide hole; 26. Sight glass. Detailed Implementation

[0030] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0031] See Figures 1-7 A vertical recovery tank for recycling ethyl acetate residue includes a tank body 1, an inlet 7, an outlet 8, a stirring assembly 9, and a heating assembly 10.

[0032] Tank 1 adopts a three-layer coaxial vertical structure, which allows different processing stages in the recycling process to be carried out in an orderly manner in the same equipment. Tank 1 is made of corrosion-resistant stainless steel to adapt to the corrosion of ethyl acetate residue and chemical substances that may be generated during the recycling process, ensuring the service life and safety of tank 1.

[0033] The residual liquid concentration layer 2, located at the bottom of tank 1, is the area for preliminary treatment of ethyl acetate residue. The main function of this layer is to remove some of the solvent or water from the residue through evaporation and other methods, thereby increasing the concentration of ethyl acetate. The middle distillation layer 3 is one of the core parts of the recovery tank. It uses the principle of distillation to further separate and purify the concentrated residue. During the distillation process, by controlling parameters such as temperature and pressure, ethyl acetate is separated from other impurities, achieving preliminary purification of ethyl acetate. The fine filtration layer 4, located at the top of tank 1, is used to finely filter the distilled ethyl acetate. The fine filtration layer 4 can effectively remove small particulate impurities and suspended solids from ethyl acetate, further improving the purity of ethyl acetate. The design of the fine filtration layer 4 enables the recovered ethyl acetate to meet higher quality requirements and is suitable for a wider range of applications.

[0034] The annular baffles 5, which are fixedly installed between each layer, are connected by welding to ensure the airtightness between the layers and prevent the liquids from mixing at different processing stages. The first guide hole 6 on the annular baffle 5 allows the liquid to flow orderly between the layers, while avoiding the adverse effects of excessively fast or slow liquid flow on the recovery process.

[0035] The inlet 7 is located at the top of the tank 1 to facilitate the transfer of ethyl acetate residue into the tank 1, and the outlet 8 is located at the bottom of the tank 1 to discharge the recycled ethyl acetate.

[0036] The stirring assembly 9 is installed inside the tank 1. Its main function is to promote the mixing and mass transfer of the liquid during the residual liquid treatment process. The heating assembly 10 is installed inside the tank 1. In the residual liquid concentration layer 2, the heating assembly 10 provides heat to evaporate the solvent or water in the residual liquid, thereby concentrating the residual liquid. In the distillation layer 3, the heating assembly 10 controls the distillation temperature to separate ethyl acetate from other impurities.

[0037] First, refer to Figure 5 In this embodiment, the stirring assembly 9 includes a stirring shaft 11 that runs through the three-layer tank 1. The stirring shaft 11 is made of high-strength and corrosion-resistant stainless steel. Its length is precisely customized according to the height of the tank 1 to ensure that it can cover the residual liquid concentration layer 2, the distillation layer 3 and the fine filtration layer 4. The diameter of the stirring shaft 11 can withstand the torque generated by the stirring blades and the resistance of the liquid, while avoiding the deformation of the shaft from affecting the stirring effect.

[0038] A spiral scraper blade 12 is fixedly installed at the bottom of the stirring shaft 11. The spiral scraper blade 12 is adapted to the conical bottom structure of the residual liquid concentration layer 2. The spiral scraper blade 12 is made of wear-resistant stainless steel. In the residual liquid concentration layer 2, since crystals or impurities may form on the tank wall during the evaporation and concentration process, the spiral scraper blade 12 can move spirally along the conical bottom wall of the residual liquid concentration layer 2 as the stirring shaft 11 rotates, scraping off the substances attached to the wall and remixing them into the liquid, preventing scaling on the wall from affecting the concentration effect, and also ensuring the full mixing and uniform evaporation of the residual liquid.

[0039] An inclined blade 13 is fixedly installed in the middle of the stirring shaft 11, located in the distillation layer 3. The inclined blade 13 is made of stainless steel plate. When the inclined blade 13 rotates, it can drive the liquid in the distillation layer 3 to circulate, increase the contact area between gas and liquid, and enhance the mass transfer and heat transfer effect in the distillation process. Through the stirring action of the inclined blade 13, the liquid distribution on the distillation tray or packing is more uniform, improving the distillation efficiency and promoting the separation of ethyl acetate from other impurities.

[0040] A flow guide spiral 14 is fixedly installed on the top of the stirring shaft 11 and is located in the fine filter layer 4. The flow guide spiral 14 is made of stainless steel. In the fine filter layer 4, the flow guide spiral 14 rotates with the stirring shaft 11 and can guide the liquid to flow along a specific path, so that the liquid is more evenly distributed when passing through the filter medium, thereby improving the filtration effect. The flow guide spiral 14 can also prevent the liquid from forming local eddies or dead corners in the fine filter layer 4, ensuring that the liquid in the fine filter layer 4 can be fully filtered, thereby improving the purity of the recovered ethyl acetate.

[0041] A mounting plate 15 is fixedly installed on the top of the tank body 1. The mounting plate 15 is made of high-strength metal plate and is connected to the top of the tank body 1 by welding. A motor 16 fixedly installed on the mounting plate 15 provides power to the stirring shaft 11.

[0042] Then, refer to Figure 4 and Figure 6In this embodiment, the heating assembly 10 includes a spiral coil 17 and a jacket 18. The spiral coil 17 is installed on the inner wall of the distillation layer 3 and is made of a high-temperature resistant and corrosion-resistant metal material, such as stainless steel. Its spiral shape fits tightly against the inner wall of the distillation layer 3, increasing the contact area with the liquid in the distillation layer 3. A heating medium, such as steam or hot liquid, can be introduced into the spiral coil 17 to provide heat to the liquid in the distillation layer 3 through heat conduction, so that the liquid reaches the temperature required for distillation and promotes the separation of ethyl acetate from other impurities. A placement hole 19 is provided at the position of the residual liquid concentration layer 2, and the jacket 18 is installed in the placement hole 19. The jacket 18 is also made of a corrosion-resistant metal material, forming a heating space around the residual liquid concentration layer 2. A heating medium can also be introduced into the jacket 18 to heat the liquid in the residual liquid concentration layer 2, accelerate the evaporation of solvent or water in the liquid, and achieve the concentration of residual liquid. The design of the jacket 18 makes the heating more concentrated and efficient, and can better control the temperature of the residual liquid concentration layer 2.

[0043] Secondly, see Figure 6 In this embodiment, a sintered metal filter element 20 is detachably installed in the fine filtration layer 4. The sintered metal filter element 20 is slidably installed with the tank body 1. The sintered metal filter element 20 is made of sintered metal powder and has high strength and good filtration performance. It can effectively remove small particulate impurities, suspended solids and other substances from ethyl acetate. The detachable design of the sintered metal filter element 20 facilitates regular replacement and cleaning to ensure the fine filtration effect. The sliding arrangement of the filter element with the tank body 1 makes the installation and removal of the filter element more convenient and quick. Operators can easily take the filter element out of the tank body 1 or install it in.

[0044] See again Figure 2 In this embodiment, a steam hole 21 is fixedly provided on the top of the tank 1, and a conveying pipe 22 is installed on the steam hole 21. A vertical condenser tower 23 is fixedly provided at the bottom of the conveying pipe 22. The steam generated during the distillation process enters the conveying pipe 22 through the steam hole 21 and is then conveyed to the vertical condenser tower 23. The vertical condenser tower 23 is equipped with components such as condenser tubes. Through the action of the cooling medium, the steam is cooled and condensed into liquid, realizing the recovery and treatment of steam. This structure ensures that the steam generated during the distillation process can be effectively treated, avoiding the direct discharge of steam into the environment and causing pollution, while also improving the recovery rate of ethyl acetate.

[0045] In addition, see Figure 4 and Figure 7In this embodiment, the feed inlet 7 is located at the top of the fine filter layer 4. A liquid distributor 24 is fixedly installed inside the feed inlet 7. The liquid distributor 24 has a straight pipe structure and a second guide hole 25 is evenly opened at the bottom. The function of the liquid distributor 24 is to evenly distribute the ethyl acetate residue entering the tank 1 in the fine filter layer 4, so as to avoid the residue from accumulating in a certain area and affecting the subsequent processing. The straight pipe structure of the liquid distributor 24 and the design of the evenly distributed second guide hole 25 enable the residue to flow smoothly into the fine filter layer 4 and form a relatively uniform liquid distribution in the fine filter layer 4, thereby improving the fine filtration effect. The discharge port 8 is located in the middle of the distillation layer 3. The ethyl acetate that has been distilled and preliminarily purified is discharged from the discharge port 8. The position of the discharge port 8 in the middle of the distillation layer 3 is designed to ensure that the discharged ethyl acetate has a high purity, while avoiding the discharge of incompletely distilled liquid or impurities from the discharge port 8.

[0046] Finally, see Figure 3 In this embodiment, a sight glass 26 is provided between the residual liquid concentration layer 2, the distillation layer 3 and the fine filtration layer 4. The sight glass 26 is made of a transparent material that is resistant to high temperature and corrosion, such as tempered glass or quartz glass. The sight glass 26 allows the operator to directly observe the state, color, liquid level and other conditions of the liquid in each layer, so as to adjust the parameters in the recovery process in a timely manner, such as temperature and stirring speed, to ensure the smooth progress of the recovery process.

[0047] Working principle:

[0048] This vertical recovery tank for ethyl acetate residue recycling first introduces the ethyl acetate residue into the tank body 1 through the inlet 7, located at the top of the fine filter layer 4. After entering the inlet 7, the residue is evenly dispersed into the fine filter layer 4 through the second guide holes 25 evenly distributed at the bottom of the distributor 24. In the fine filter layer 4, the guide spiral 14 rotates with the stirring shaft 11, guiding the liquid to flow evenly and ensuring it passes fully through the sintered metal filter element 20. The sintered metal filter element 20 performs fine filtration on the residue, removing small particulate impurities and suspended solids, thus initially improving the purity of ethyl acetate. The filtered liquid flows into the distillation layer 3 through the first guide hole 6 on the annular partition 5. The spiral coil 17 of the heating assembly 10 is activated, introducing a heating medium into the spiral coil 17 to provide heat to the liquid in the distillation layer 3. The inclined blades 13 in the middle of the stirring shaft 11 rotate, driving the liquid to circulate and enhancing the mass and heat transfer effect, allowing the liquid to reach the temperature required for distillation. Utilizing the azeotropic properties of ethyl acetate with ethanol and water, the liquid is further distilled. The azeotropic components are separated at a constant temperature to achieve preliminary purification of ethyl acetate. The steam generated during the distillation process enters the vertical condenser 23 through the steam hole 21 at the top of the tank 1 and the conveying pipe 22. The steam is cooled and condensed into liquid for recovery in the condenser. Part of the pre-purified ethyl acetate is discharged from the outlet 8 in the middle of the distillation layer 3, and the other part flows into the residual liquid concentration layer 2 through the first guide hole 6 on the annular baffle 5. The jacket 18 of the heating component 10 heats the liquid in the residual liquid concentration layer 2. At the same time, the spiral scraper blades 12 at the bottom of the stirring shaft 11 rotate with the stirring shaft 11 and move spirally along the conical bottom wall to scrape off the material attached to the wall, promote uniform evaporation of the liquid, remove some water, and concentrate the residual liquid. The concentrated residual liquid can flow back to the distillation layer 3 through the first guide hole 6 on the annular baffle 5 for further distillation, or be discharged from the outlet 8 at the bottom of the tank 1. During the entire recovery process, the operator observes the state, color, liquid level and other conditions of the liquid in each layer through the sight glass 26.

[0049] Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the present invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A vertical recovery tank for ethyl acetate raffinate recycling, characterized by, The utility model relates to a three -layer coaxial vertical structure of tank body (1) is from bottom to top residual liquid concentration layer (2), distillation layer (3) and fine filter layer (4) in proper order, fixedly arranged with annular baffle (5) sealed connection between each layer, the first flow guide hole (6) is opened in annular baffle (5) on, Feed inlet (7) is opened in the top of tank body (1), Discharge outlet (8) is opened in the bottom of tank body (1), Stirring assembly (9) is installed in tank body (1), Heating assembly (10) is installed in tank body (1). The stirring assembly (9) includes a stirring shaft (11), which penetrates the three-layer tank body (1), the bottom of the stirring shaft (11) is fixedly provided with a spiral wall scraping blade (12), the middle part of the stirring shaft (11) is fixedly provided with an inclined paddle (13), the top of the stirring shaft (11) is fixedly provided with a flow guide spiral (14), the top of the tank body (1) is fixedly provided with a mounting plate (15), the mounting plate (15) is fixedly provided with a motor (16), and the output shaft of the motor (16) is connected with the stirring shaft (11) through a key.

2. The vertical recovery tank for recycling of ethyl acetate residual liquid according to claim 1, characterized by, The heating assembly (10) includes a spiral coil (17) and a jacket (18), the spiral coil (17) is installed on the inner wall of the distillation layer (3), a placement hole (19) is opened at the position of the residual liquid concentration layer (2), and the jacket (18) is installed in the placement hole (19).

3. The vertical recovery tank for recycling of ethyl acetate residual liquid according to claim 1, characterized by, A sintered metal filter core (20) is detachably arranged in the fine filter layer (4), and the sintered metal filter core (20) is slidably arranged with the tank body (1).

4. The vertical recovery tank for recycling of ethyl acetate residual liquid according to claim 1, characterized by, The residual liquid concentration layer (2) is a conical bottom structure, and the spiral wall scraping blade (12) is adapted to the bottom of the residual liquid concentration layer (2).

5. The vertical recovery tank for recycling of ethyl acetate residual liquid according to claim 2, characterized by, A steam hole (21) is fixedly arranged at the top of the tank body (1), a delivery pipe (22) is installed on the steam hole (21), and a vertical condensation tower (23) is fixedly arranged at the bottom of the delivery pipe (22).

6. The vertical recovery tank for recycling of ethyl acetate raffinate according to claim 1, characterized in that, The feed inlet (7) is located at the top of the fine filter layer (4), a liquid distributor (24) is fixedly arranged in the feed inlet (7), the liquid distributor (24) is a straight pipe structure, second flow guide holes (25) are uniformly opened at the bottom of the liquid distributor (24), and the discharge outlet (8) is located in the middle of the distillation layer (3).

7. The vertical recovery tank for recycling of ethyl acetate raffinate according to claim 1, characterized in that, A sight glass (26) is opened between the residual liquid concentration layer (2), the distillation layer (3) and the fine filter layer (4).

8. The vertical recovery tank for recycling of ethyl acetate raffinate according to claim 1, characterized in that, ​

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