Hydrogen peroxide extraction device

Abstract

The utility model belongs to the technical field of hydrogen peroxide production, and particularly relates to a hydrogen peroxide extraction device which comprises a hydrogen peroxide extraction tower, a raffinate coalescence separator and a purification tower, the raffinate coalescence separator is connected with the top of the hydrogen peroxide extraction tower, and the purification tower is connected with the bottom of the hydrogen peroxide extraction tower; the hydrogen peroxide extraction tower comprises a tower body, an overflow port, a raffinate outlet, a pure water inlet and an oxidation liquid inlet are sequentially formed in the side wall of the tower body from top to bottom, an extract outlet is formed in the bottom of the tower body, a tower plate group is arranged in the tower body, and the tower plate group sequentially comprises a top tower plate, a plurality of composite tower plates and a plurality of common tower plates from top to bottom; the composite tower plate comprises a sieve plate, a coalescence separation layer, a screen mesh and a downcomer, the upper part of the coalescence separation layer is connected with the sieve plate, the lower part of the coalescence separation layer is connected with the screen mesh, one end of the downcomer is connected with the sieve plate, and the other end of the downcomer penetrates through the coalescence separation layer and the screen mesh. The device reduces the back-mixing phenomenon of extract with oil, reduces the water content of raffinate, and improves the separation efficiency of hydrogen peroxide.

Description

Technical Field

[0001] The utility model belongs to the technical field of hydrogen peroxide production, and specifically relates to a hydrogen peroxide extraction device. Background Art

[0002] At present, the commonly used anthraquinone process methods for preparing hydrogen peroxide in China are: 1. fixed bed alkaline process, 2. fixed bed fully acidic process, 3. fluidized bed process; the anthraquinone process has mild reaction, low cost, and is easy for large-scale production. It is currently the main method for producing hydrogen peroxide in industry.

[0003] The main operations of the anthraquinone method include hydrogenation, oxidation, extraction and purification. The principle is to mix heavy aromatic hydrocarbons, trioctyl phosphate, tetrabutyl urea, 2-ethylanthraquinone or tetrahydro-2-ethylanthraquinone, and then catalytically hydrogenate 2-ethylanthraquinone or tetrahydro-2-ethylanthraquinone and oxidize it with air to obtain oxidizing liquid and hydrogen peroxide.

[0004] Extraction is a very important separation step in hydrogen peroxide production; the extraction tower is divided into a concentration section, an equilibrium section, and a raffinate reduction section from bottom to top; and the sieve plate extraction tower is the most widely used, with a simple structure, low energy consumption, and effective extraction. However, there are still many factors that affect its operation, such as flooding point load, minimum load of the extraction tower, and maximum height of the dispersed phase under the plate. The opening rate of the plate tower, the diameter of the hole, and the fluid volume flow rate, the interfacial tension between the two phases, and the density difference between the two phases can directly affect the quality of hydrogen peroxide. The high hydrogen peroxide content in the raffinate restricts the increase in the load of the device and has a high safety risk. The high raffinate returned to the hydrogenation system is prone to cause the decomposition of hydrogen peroxide to produce a flash explosion;

[0005] Therefore, the market is in urgent need of an efficient extraction tray, coalescing and separating fillers to reduce the content of the raffinate; to enable hydrogen peroxide and pure water to fully transfer mass and extract efficiently, and further coalesce and separate to solve these problems. At present, the Ministry of Emergency Management requires the addition of online detection and monitoring measures for the raffinate, and the shutdown of the plant for high raffinate; but it cannot fundamentally solve the safety problem. Utility Model Content

[0006] The utility model aims to solve the problems of high raffinate hydrogen peroxide content and turbid oily extract in the existing hydrogen peroxide extraction tower described in the background technology, and proposes a new hydrogen peroxide extraction tower, which has low raffinate hydrogen peroxide content and high purity of extract.

[0007] The technical solution adopted to achieve the above-mentioned purpose is a hydrogen peroxide extraction device, which includes a hydrogen peroxide extraction tower, a raffinate coalescing separator and a purification tower, wherein the raffinate coalescing separator is connected to the top of the hydrogen peroxide extraction tower, and the purification tower is connected to the bottom of the hydrogen peroxide extraction tower;

[0008] The hydrogen peroxide extraction tower comprises a tower body, the side wall of which is provided with an overflow port, a raffinate outlet, a pure water inlet and an oxidation liquid inlet in order from top to bottom, the bottom of the tower body is provided with an extraction liquid outlet, and a tower plate group is provided inside the tower body, and the tower plate group comprises a top tower plate, a plurality of composite tower plates and a plurality of ordinary tower plates in order from top to bottom;

[0009] The composite tower plate includes a sieve plate, a coalescence separation layer, a screen and a downcomer. The coalescence separation layer is connected to the sieve plate at the top and to the screen at the bottom. One end of the downcomer is connected to the sieve plate, and the other end of the downcomer passes through the coalescence separation layer and the screen.

[0010] In the above technical scheme, the oxidizing liquid enters from the bottom of the hydrogen peroxide extraction tower and is dispersed into fine liquid droplets by the sieve plate group, and the pure water enters from the top of the hydrogen peroxide extraction tower to countercurrently contact with the oxidizing liquid, and the concentration of hydrogen peroxide in the pure water is continuously increased, and finally discharged from the extraction liquid outlet into the purification tower for further extraction and separation to obtain hydrogen peroxide; the top raffinate is discharged through the raffinate outlet into the raffinate coalescing separator for flash dehydration, wherein, in the countercurrent extraction process, the raffinate oil phase components mainly include dispersed oil, dissolved oil and emulsified oil, and the difficulty of oil removal lies in the removal of dissolved oil and emulsified oil. The utility model cuts the emulsified oil by the sieve at the bottom of the composite tower plate to achieve physical demulsification.

[0011] Furthermore, the screen is a mesh-shaped polytetrafluoroethylene wire mesh.

[0012] Furthermore, polytetrafluoroethylene filler is filled between the top tower plate and the uppermost composite tower plate.

[0013] In the above technical solution, the middle of the top tray sieve plate is provided with uniform sieve holes, and the lower sieve plate adopts stepped holes, which, combined with polytetrafluoroethylene fillers, can increase the throughput of the equipment. This makes the operation flexible and the volumetric efficiency of the equipment high. In addition, the dispersed oil is more easily dispersed into smaller droplets when flowing through the demulsification section and the clarification section, which makes the mass transfer specific surface area large and the extraction and separation efficiency high, solving the problem of large top interfacial tension and water in the raffinate.

[0014] Furthermore, a first packing layer is provided between the raffinate outlet and the pure water inlet.

[0015] Furthermore, the first packing layer is filled with stainless steel corrugated packing with polytetrafluoroethylene sprayed on the surface.

[0016] In the above technical solution, the use of this filler can improve the strength of the filler, which is not easy to corrode, clog and deform. The polytetrafluoroethylene coating has oleophilic and hydrophobic properties, thereby increasing the ability of the raffinate to pass through the first filler layer, and can reduce the flow pressure drop ratio of the corrugated screen tube by 30%, thereby increasing the service life and oil permeability of the device, and further improving the agglomeration and separation effect.

[0017] Furthermore, the hydrogen peroxide extraction tower is provided with 7-10 layers of composite tower plates, preferably 7 layers of composite tower plates.

[0018] In the above technical solution, the 7-layer composite tower plate can achieve the purpose of physical demulsification and reduce the entrainment problem.

[0019] Furthermore, the pore size of the sieve plate is 3.4±0.1 mm.

[0020] In the above technical solution, the aperture of the sieve plate is increased, and the principle of like dissolves like is used to promote the separation of oil components in water.

[0021] Furthermore, the hydrogen peroxide extraction tower is provided with 7 to 41 layers of ordinary tower plates.

[0022] Furthermore, the distance between the coalescence separation layer and the sieve plate of the adjacent upper composite tower plate is 400-500 mm.

[0023] In the above technical scheme, the spacing combined with the composite tower plate creates a forced separation layer between two adjacent sieve plates, thereby increasing the extraction efficiency of each sieve plate by more than 30%, so that there is both a mass transfer section and a pinellia separation section between two adjacent sieve plates, thereby improving the extraction efficiency of the extraction tower.

[0024] Furthermore, the purification tower is provided with several sections of second packing layers, and the second packing layers are filled with stainless steel corrugated packing with polytetrafluoroethylene sprayed on the surface, preferably 3 sections of second packing layers.

[0025] In the above technical solution, the fillers are distributed in a certain proportion, and the extract and the continuous phase heavy aromatics are further extracted and separated to obtain qualified hydrogen peroxide.

[0026] The advantages of the utility model are:

[0027] 1. The utility model solves the problem of water in the raffinate by filling polytetrafluoroethylene filler between the top tray and the top composite tray to reduce the droplet size of the dispersed phase and lower the top interfacial tension.

[0028] 2. The utility model provides a first packing layer between the raffinate outlet and the pure water inlet, and the first packing layer can increase the passing rate of the raffinate, further improving the coalescence separation efficiency and the service life of the device.

[0029] 3. The utility model realizes physical demulsification of emulsified oil by filling the screen.

[0030] 4. The utility model realizes the separation of oil components in water by increasing the aperture of the sieve plate.

[0031] 5. The utility model further reduces the content of organic carbon, free acid and non-volatile matter through the composite tower plate. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] In order to more clearly illustrate the embodiments of the utility model or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings in the following description are only embodiments of the utility model. For ordinary technicians in this field, other drawings can be obtained based on the provided drawings without paying creative work.

[0033] Figure 1 It is a flow chart of the utility model;

[0034] Figure 2 This is a schematic diagram of the structure of the hydrogen peroxide extraction tower of the utility model;

[0035] Figure 3 It is a structural schematic diagram of the composite tower plate of the utility model.

[0036] Illustrations: 1. Hydrogen peroxide extraction tower, 2. Raffinate coalescing separator, 3. Purification tower, 4. Tower body, 5. Overflow port, 6. Raffinate outlet, 7. Pure water inlet, 8. Oxidation liquid inlet, 9. Extraction liquid outlet, 10. Top tower plate, 11. Composite tower plate, 12. Ordinary tower plate, 13. Sieve plate, 14. Coalescing separation layer, 15. Screen, 16. Downcomer, 17. First packing layer. DETAILED DESCRIPTION

[0037] In order to enable those skilled in the art to better understand the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only embodiments of a part of the present invention rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work belong to the protection scope of the present invention.

[0038] In the description of the present invention, it should be understood that the terms "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation on the present invention.

[0039] like Figure 1As shown, a hydrogen peroxide extraction device comprises a hydrogen peroxide extraction tower 1, a raffinate coalescing separator 2 and a purification tower 3, wherein the raffinate coalescing separator 2 is connected to the top of the hydrogen peroxide extraction tower 1, and the purification tower 3 is connected to the bottom of the hydrogen peroxide extraction tower 1;

[0040] In this embodiment, a heat exchanger is further provided on the pipeline connecting the purification tower 3 and the hydrogen peroxide extraction tower 1. Another pipeline connected to the hydrogen peroxide extraction tower 1 is further provided at the bottom of the heat exchanger, and a phosphoric acid adding pipeline is provided on the pipeline.

[0041] like Figure 2 As shown, the hydrogen peroxide extraction tower 1 includes a tower body 4, and the side wall of the tower body 4 is provided with an overflow port 5, a raffinate outlet 6, a pure water inlet 7 and an oxidation liquid inlet 8 from top to bottom, an extract outlet 9 is provided at the bottom of the tower body 4, and a vent is provided at the top of the tower body 4. A tower plate group is arranged inside the tower body 4, and the tower plate group includes a top tower plate 10, 7 layers of composite tower plates 11 and 41 layers of ordinary tower plates 12 from top to bottom.

[0042] The top side wall of the tower body 4 is also provided with nitrogen replenishment, liquid level gauge ports and interface gauge ports.

[0043] like Figure 3 As shown, the composite tower plate 11 includes a sieve plate 13, a coalescing separation layer 14, a screen 15 and a downcomer 16. The coalescing separation layer 14 is connected to the sieve plate 13 at the top and to the screen 15 at the bottom. One end of the downcomer 16 is connected to the sieve plate 13, and the other end of the downcomer 16 passes through the coalescing separation layer 14 and the screen 15.

[0044] In this embodiment, the screen 15 is a mesh-shaped polytetrafluoroethylene mesh, and the mesh distribution is preferably irregular for physical demulsification.

[0045] In this embodiment, polytetrafluoroethylene filler is filled between the top tray 10 and the uppermost composite tray 11 .

[0046] In this embodiment, a first packing layer 17 is provided between the raffinate outlet 6 and the pure water inlet 7 , and the first packing layer 17 is filled with a stainless steel corrugated packing with a surface sprayed with polytetrafluoroethylene.

[0047] In this embodiment, the pore size of the sieve plate 13 is 3.4±0.1 mm, which is larger than that of conventionally selected sieve plates and is used to separate oil components in water.

[0048] In this embodiment, the distance between the coalescence separation layer 14 and the sieve plate 13 of the adjacent upper composite tray 11 is 400-500 mm, preferably 450 mm.

[0049] In this embodiment, three sections of second packing layers are provided in the purification tower 3, and the second packing layers are filled with stainless steel corrugated packing with polytetrafluoroethylene sprayed on the surface.

[0050] The working principle of the hydrogen peroxide extraction tower 1 of the utility model is as follows: the oxidizing liquid enters the hydrogen peroxide extraction tower 1 from the bottom of the tower and is dispersed into fine liquid droplets under the action of the tower plate group, the pure water enters the tower from the top of the tower, and contacts with the oxidizing liquid in a countercurrent and rapid manner, the water is interconnected through the through holes in the sieve plate 13 and the downcomer, and the concentration of hydrogen peroxide is continuously increased from the top of the tower to the bottom of the tower, and after reaching the concentration, it enters the purification tower through the extract outlet pipe for further extraction and separation by similar compatibility, the raffinate enters the raffinate coalescing separator 2 from the top of the tower, and the extract enters the purification tower 3 from the bottom of the tower.

[0051] In the utility model, the emulsified oil is physically demulsified by the screen 15, and the water and oil are separated by increasing the aperture of the screen plate 13. By arranging the composite tower plate 11, the extraction efficiency of the screen plate 13 is increased by more than 30%, so that there are both a mass transfer section on the plate and a separation section under the plate between two adjacent screen plates, so that the efficiency of the screen plate 13 of the entire hydrogen peroxide extraction tower 1 is increased by more than 1 / 3. By filling the space between the top tower plate 10 and the top composite tower plate 11 with polytetrafluoroethylene filler, the problem of large top interfacial tension and the problem of water in the raffinate are solved. By arranging the first filler layer 17, the oil permeability is increased, and the coalescence separation efficiency is further improved.

[0052] Finally, it should be noted that this embodiment is only used to illustrate the present invention and does not limit the scope of the present invention. In addition, it should be understood that after reading the content of the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms also fall within the scope defined by the claims attached to this application.

Claims

1. A hydrogen peroxide extraction device, characterized in that: The hydrogen peroxide extraction device comprises a hydrogen peroxide extraction tower (1), a raffinate coalescing separator (2) and a purification tower (3), wherein the raffinate coalescing separator (2) is connected to the top of the hydrogen peroxide extraction tower (1), and the purification tower (3) is connected to the bottom of the hydrogen peroxide extraction tower (1); The hydrogen peroxide extraction tower (1) comprises a tower body (4), the side wall of the tower body (4) is provided with an overflow port (5), a raffinate outlet (6), a pure water inlet (7) and an oxidation liquid inlet (8) in order from top to bottom, the bottom of the tower body (4) is provided with an extraction liquid outlet (9), and a tower plate group is arranged inside the tower body (4), and the tower plate group comprises, in order from top to bottom, a top tower plate (10), a plurality of composite tower plates (11) and a plurality of ordinary tower plates (12); The composite tower plate (11) comprises a sieve plate (13), a coalescence separation layer (14), a screen (15) and a downcomer (16); the coalescence separation layer (14) is connected to the sieve plate (13) at the top, and is connected to the screen (15) at the bottom; one end of the downcomer (16) is connected to the sieve plate (13), and the other end of the downcomer (16) passes through the coalescence separation layer (14) and the screen (15).

2. The hydrogen peroxide extraction device according to claim 1, characterized in that: The screen (15) is a mesh-shaped polytetrafluoroethylene wire mesh.

3. The hydrogen peroxide extraction device according to claim 1, characterized in that: A polytetrafluoroethylene filler is filled between the top tower plate (10) and the uppermost composite tower plate (11).

4. The hydrogen peroxide extraction device according to claim 1, characterized in that: A first packing layer (17) is provided between the raffinate outlet (6) and the pure water inlet (7).

5. The hydrogen peroxide extraction device according to claim 4, characterized in that: The first packing layer (17) is filled with stainless steel corrugated packing with a surface sprayed with polytetrafluoroethylene.

6. The hydrogen peroxide extraction device according to claim 1, characterized in that: The hydrogen peroxide extraction tower (1) is provided with 7 to 10 layers of composite tower plates (11).

7. The hydrogen peroxide extraction device according to claim 1, characterized in that: The pore size of the sieve plate (13) is 3.4±0.1 mm.

8. The hydrogen peroxide extraction device according to claim 1, characterized in that: The hydrogen peroxide extraction tower (1) is provided with 7 to 41 layers of common tower plates (12).

9. The hydrogen peroxide extraction device according to claim 1, characterized in that: The distance between the coalescence separation layer (14) and the sieve plate (13) of the adjacent upper composite tower plate (11) is 400-500 mm.

10. The hydrogen peroxide extraction device according to claim 1, characterized in that: The purification tower (3) is provided with a plurality of second packing layers, and the second packing layers are filled with stainless steel corrugated packing with a surface sprayed with polytetrafluoroethylene.

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