Oxidation reaction extraction device and method for producing hydrogen peroxide

Abstract

The invention relates to an oxidation reaction extraction device for producing hydrogen peroxide, the oxidation reaction extraction device comprises an oxidation extraction tower, an oxidation liquid separator, an extraction tower, a coalescer and a dehydrator, the top of the oxidation extraction tower is provided with a hydrogenation liquid inlet for introducing a hydrogenation liquid to be oxidized from the tower top, and the lower part of the oxidation extraction tower is provided with an oxygen-containing gas inlet for introducing an oxygen-containing gas from the tower bottom; a dilute hydrogen peroxide inlet is formed in the middle-lower part of the tower body and positioned above the oxygen-containing gas inlet, and is used for introducing a dilute hydrogen peroxide for extraction from the middle-lower part of the tower body, so that an oxidation extraction process of whole-tower countercurrent oxidation and tower-bottom parallel flow extraction is formed; according to the scheme, high oxidation efficiency, high extraction efficiency and low extraction reverse mixing can be guaranteed at the same time.

Description

Technical Field

[0001] The invention relates to the field of preparing hydrogen peroxide by anthraquinone method, and in particular to an oxidation reaction extraction device and a method for producing hydrogen peroxide. Background Art

[0002] As an important inorganic chemical raw material, hydrogen peroxide is widely used in many fields such as papermaking, textiles, chemicals, environmental protection and electronic component manufacturing. The current industrial method for producing hydrogen peroxide is the anthraquinone method, which uses alkyl anthraquinone dissolved in a mixed organic solvent as a carrier for cyclic hydrogenation and oxidation, and obtains hydrogen peroxide of a certain concentration through a series of processes such as hydrogenation, oxidation, extraction and post-treatment.

[0003] The oxidation towers for producing hydrogen peroxide by the anthraquinone method are mostly two-section or three-section towers, which use hydrogenated liquid and compressed air to contact each other in parallel in the tower and undergo oxidation reaction. This type of oxidation tower has the following problems: (1) Due to the severe backmixing in the oxidation tower, and the low oxygen concentration in the air and the low concentration of hydrogen anthraquinone in the oxidation liquid at the discharge end of the tower, the reaction rate is very slow, and therefore the oxidation yield is generally low. (2) The oxidation tail gas of this type of oxidation tower generally has a high temperature, which poses a safety hazard. (3) Due to the moisture entrained in the air or hydrogenated liquid in the oxidation tower, and the self-decomposition of the hydrogen peroxide obtained by the oxidation reaction, there is oxidation residual liquid at the bottom of the oxidation tower, which needs to be discharged regularly. The operation is cumbersome and there are safety hazards.

[0004] The existing extraction tower needs to have a large number of plates to meet the separation requirements due to the very small density difference between water and oil, and the plate efficiency is extremely low. The residual extract at the oil phase outlet of the extraction tower is high, and vacuum dehydration needs to be set up. If the water separation of the extraction tower is not good, there will be a greater safety risk and increase energy consumption.

[0005] CN106672911A discloses a process in which an oxidizing liquid and an oxygen-containing gas are in parallel contact in an oxidative extraction tower and extracted in countercurrent with an extractant, so that the oxidative extraction tower can both undergo an oxidation reaction and realize the extraction function. Although this method achieves a certain degree of integration in the oxidation and extraction functions, due to severe backmixing, the oxidation efficiency is not high, and the residual extract of the working liquid after extraction is very high, so it cannot be directly returned to the upstream for hydrogenation, and has no obvious advantages.

[0006] CN204265444U discloses a vapor-liquid countercurrent reactor for hydrogen peroxide production, in which the oxidizing liquid and the oxygen-containing gas are in countercurrent contact in the tower. Compared with the cocurrent reaction scheme, the countercurrent contact can effectively improve the mass transfer efficiency of the reactor; however, the scheme only focuses on the oxidation process and does not mention how to further integrate the extraction and purification steps.

[0007] CN217868137U discloses an oxidation system for producing hydrogen peroxide by anthraquinone method, which also discloses an oxidation scheme of countercurrent contact between the oxidation liquid and the oxygen-containing gas in an oxidation tower. At the same time, the patent also mentions that the obtained oxidation liquid is separated into vapor and liquid and then sent to an extraction tower for extraction. However, the patent does not disclose the specific extraction process used, and does not provide a solution to the serious back-mixing defect in the existing extraction process.

[0008] Therefore, how to organically combine the oxidation process and the extraction process of the anthraquinone method hydrogen peroxide system while ensuring high mass transfer reaction efficiency and low extraction back-mixing rate, so as to efficiently prepare high-purity hydrogen peroxide has become an urgent problem to be solved in the field. Summary of the invention

[0009] In view of the shortcomings of the prior art, the present invention aims to provide an oxidation reaction extraction device and method for producing hydrogen peroxide, which realizes the integration of oxidation reaction and extraction process, has very high oxidation yield and extraction efficiency, and can directly obtain high-concentration hydrogen peroxide without adding a concentrating device.

[0010] Specifically, the present invention provides an oxidation reaction extraction device for producing hydrogen peroxide, comprising an oxidation extraction tower 15, an oxidation liquid separator 16, an extraction tower 17 and a coalescer 19, wherein the oxidation extraction tower 15 adopts countercurrent oxidation and parallel current extraction, and is provided with a hydrogenation liquid inlet 1 at the top for introducing the hydrogenation liquid to be oxidized from the top of the tower, an oxygen-containing gas inlet 2 at the bottom for introducing the oxygen-containing gas from the bottom of the tower, and a hydrogen peroxide rare product inlet 4 at the middle and lower part and located above the oxygen-containing gas inlet 2 for introducing the hydrogen peroxide rare product for extraction from the middle and lower part of the tower body; the oxidation liquid and the hydrogen peroxide rare product flow from top to bottom in the oxidation extraction tower 15, and the oxygen-containing gas flows from bottom to top in the oxidation extraction tower 15, thereby forming an oxidation extraction process of countercurrent oxidation of the whole tower and parallel current extraction at the bottom of the tower. The top of the oxidation extraction tower 15 is provided with a medium-pressure tail gas outlet 3 for discharging the medium-pressure oxidation tail gas.

[0011] The bottom of the oxidation extraction tower 15 is provided with a concentrated oxidizing liquid outlet 5, which is connected to the oxidizing liquid separator 16 through a pipeline; the oxidizing liquid separator 16 is a phase separation device, which is a box-type structure as a whole, and an overflow baffle is provided inside, and a water phase outlet 6 and an oil phase outlet 7 are provided on both sides of the overflow baffle respectively; the water phase outlet 6 is located at the bottom of the oxidizing liquid separator 16, and is used to discharge the concentrated hydrogen peroxide product after oil-water separation; the oil phase outlet 7 is connected to the bottom of the extraction tower 17 through a pipeline, and is used to send the dilute oxidizing liquid after oil-water separation to the extraction tower 17; the top of the oxidizing liquid separator 16 is also provided with an oxidation tail gas outlet.

[0012] Since the hydrogen peroxide has reached the highest concentration in the extractant running to the bottom of the oxidation extraction tower 15, the back mixing of the extraction process has the greatest impact on the extraction efficiency. In the present invention, the concentrated oxidizing liquid outlet 5 is arranged below the oxygen-containing gas inlet 2, which can further eliminate the extraction back mixing phenomenon caused by gas disturbance and ensure the extraction efficiency in the oxidation extraction tower 15.

[0013] The top of the extraction tower 17 is provided with an extractant inlet 9 for inputting a pure water extractant with a stabilizer added thereto into the extraction tower 17; the bottom of the extraction tower 17 is provided with a hydrogen peroxide rare product outlet, the pipeline of which is connected to the hydrogen peroxide rare product inlet 4 at the middle and lower part of the oxidation extraction tower 15, and the pipeline is provided with a hydrogen peroxide rare product pump 18; the top of the extraction tower 17 is provided with a second oxidation tail gas outlet, which is collected together with the aforementioned oxidation tail gas outlet in a low-pressure oxidation tail gas pipe 8; the top side wall of the extraction tower 17 is provided with a raffinate outlet 10, which is connected to a coalescer 19 through a pipeline; the coalescer 19 is built-in with a coalescing filter element, and the filter element material is at least one of a fluorinated polymer or polyphenylene sulfide; the coalescer 19 is provided with a drain port 11 and a working liquid outlet 12, which are respectively used to discharge water and working liquid generated by the raffinate after coalescing treatment.

[0014] It also includes a dehydrator 20, which has a containing cavity, and the containing cavity is connected to the aforementioned working liquid outlet 12 through a pipeline to receive the working liquid discharged from the coalescer 19; at the same time, the outlet end of the low-pressure oxidation tail gas pipe 8 extends into the bottom of the containing cavity and is immersed below the liquid level of the working liquid; the top of the dehydrator 20 is provided with a tail gas outlet 14, and the bottom is provided with a dehydrated working liquid outlet 13. The working liquid that has been dehydrated by the coalescer 19 is in contact with the oxidation tail gas from the low-pressure oxidation tail gas pipe 8 by bubbling in the dehydrator 20, so that the water entrained by the working liquid is further removed by steam stripping.

[0015] The oxidative extraction tower 15 is a plate tower with 8 plates.

[0016] The extraction tower 7 is a plate tower with 15 plates. A polymer grid or a woven mesh is arranged below the plates. The polymer material is at least one of polypropylene and fluorine-containing polymer.

[0017] The present invention also provides an oxidation reaction extraction method for producing hydrogen peroxide, comprising the following steps:

[0018] (1) The hydrogenated liquid is introduced from the top of the oxidation extraction tower 15, and the oxygen-containing gas 2 is introduced from the bottom of the oxidation extraction tower 15. The two are in countercurrent contact in the oxidation extraction tower 15, and an oxidation reaction occurs to continuously generate hydrogen peroxide.

[0019] (2) While step (1) is being carried out, dilute hydrogen peroxide is added to the middle and lower part of the oxidation extraction tower 15, and the dilute hydrogen peroxide gradually extracts the hydrogen peroxide produced by the reaction into the water phase.

[0020] (3) The concentrated oxidizing liquid is introduced into the oxidizing liquid separator 16 at the bottom of the oxidizing extraction tower 15 for water-oil phase separation, and concentrated hydrogen peroxide is extracted at the water phase outlet 6. The dilute oxidizing liquid is introduced into the bottom of the extraction tower 17 at the oil phase outlet 7.

[0021] (4) Pure water with added stabilizer and dilute oxidizing liquid are countercurrently contacted in the extraction tower 17, and dilute hydrogen peroxide product is obtained at the bottom of the extraction tower 17. The dilute hydrogen peroxide product is pressurized through a pipeline and a dilute hydrogen peroxide product pump 18 and sent to the dilute hydrogen peroxide product inlet 4 of the oxidation extraction tower 15; the raffinate is obtained at the top of the extraction tower 17 and sent to the agglomerator 19 for agglomeration and dehydration.

[0022] (5) After the entrained water is separated from the raffinate in the coalescer 19, the raffinate enters the dehydrator 20. At the same time, the oxygen-containing gas entrained in the oxidizing liquid in the oxidizing liquid separator 16 and the extraction tower 17 is transported to the dehydrator 20 through the low-pressure oxidation tail gas pipe 8 for bubbling, thereby taking away the remaining water in the working liquid.

[0023] The tail gas discharged from the dehydrator 20 is subjected to tail gas treatment, and the dehydrated working fluid is returned to the upstream hydrogenation reactor.

[0024] In the oxidation extraction process of the present invention, the hydrogenated liquid, the oxygen-containing gas and the hydrogen peroxide product simultaneously enter the oxidation extraction tower 15. The hydrogenated liquid and the hydrogen peroxide product are contacted in the middle and lower part of the oxidation extraction tower 15 and then extracted in parallel. At the same time, the hydrogenated liquid and the oxygen-containing gas are countercurrently contacted in the entire oxidation extraction tower 15 (referring to the vapor-liquid contact mode of the tower section below the oxygen-containing gas inlet 2), and the oxidation reaction and extraction process are carried out.

[0025] The hydrogenation efficiency of the hydrogenated liquid fed to the oxidation extraction tower 15 (referring to the hydrogen peroxide content per unit volume of the hydrogenated liquid after oxidation) is 6-20 g / L, the oxygen concentration of the oxygen-containing gas is 20-100 vt%, and the concentration of the rare hydrogen peroxide is 26-36 wt%.

[0026] The oxidation yield of the oxidation extraction tower 15 is 96-98%. The operating pressure of the oxidation extraction tower 15 is 0.2-1.0 MPaG, and the operating temperature is 45-58°C.

[0027] The residence time of the water-oil phase separation in the oxidation liquid separator 16 is 2 to 15 minutes, the concentration of hydrogen peroxide in the water phase discharge is 33 to 43 wt%, and the content of hydrogen peroxide in the oil phase discharge is 6 to 10 g / L.

[0028] The oxidation liquid separator 16 and the extraction tower 7 are gas-connected, and the operating pressure is 0.03-0.25 MPaG.

[0029] The dehydrator 20 uses the low-pressure oxidation tail gas discharged from the oxidation liquid separator 16 and the extraction tower 7 to strip the residual water in the working liquid. The flow ratio of the tail gas entering the dehydrator 20 to the working liquid is 1:20 to 1:5 (v / v%), and the water content of the dehydrated working liquid leaving the dehydrator 20 is 300 to 3000 ppm. The operating pressure of the dehydrator 20 is 0.005 to 0.1 MPaG, and the operating temperature is 45 to 55°C.

[0030] The working fluid is a mixed solution of alkyl anthraquinone, heavy aromatic hydrocarbons and a polar solvent. The alkyl anthraquinone is at least one of 2-ethyl anthraquinone, 2-butyl anthraquinone and 2-pentyl anthraquinone. The polar solvent is at least one of trioctyl phosphate, 2-methylcyclohexyl acetate, tetrabutyl urea and diisobutyl carbinol.

[0031] Compared with the prior art, the present invention has at least the following beneficial effects:

[0032] The present invention adopts whole-tower countercurrent oxidation plus front-stage countercurrent extraction and rear-stage parallel-current extraction operations, wherein the whole-tower countercurrent oxidation can greatly improve the mass transfer driving force and the oxidation efficiency compared with the traditional parallel-current oxidation process, thereby reducing the number of plates required for the oxidation tower; the front-stage countercurrent extraction operation can make the extractant and the material flow to be extracted fully turbulently contact, and with the help of the high mass transfer driving force of the countercurrent extraction, it is ensured that the front-stage extraction process has a high extraction efficiency. Although the countercurrent extraction will inevitably produce more obvious back-mixing, the concentration of hydrogen peroxide in the extractant is still low during the front-stage extraction process, and there is no need to discharge the material (meaning that there is no need to output the extracted product), so the negative impact of the back-mixing is limited; in the rear stage of the extraction, since there is a need to discharge the material and the concentration of hydrogen peroxide in the extractant is already very high at this time, a smaller degree of back-mixing is required. It will also have a great impact on the concentration of hydrogen peroxide in the discharge; based on this, the present invention creatively adopts a combined oxidation extraction process of whole tower countercurrent oxidation plus front-stage countercurrent extraction plus rear-stage parallel extraction, while ensuring high oxidation efficiency, high extraction efficiency and low extraction back-mixing effect; the introduction of hydrogen peroxide rare product in the oxidation tower can quickly transfer the hydrogen peroxide generated by the reaction from the oil phase to the water phase, which is conducive to promoting the oxidation reaction; on the other hand, it can also greatly reduce the load of the downstream extraction tower, thus allowing the use of a smaller extraction tower; after the hydrogenated liquid is countercurrently oxidized and extracted in parallel, it is separated into water and oil phases by the oxidation liquid separator, and high-concentration hydrogen peroxide can be directly produced without the need for an additional concentration device, which reduces energy consumption and reduces the safety risk of heating and decomposing high-concentration hydrogen peroxide during concentration. The present invention adopts pressurized extraction, which has higher separation efficiency, and the tail gas released by reduced pressure is used as the stripping feed gas of the dehydrator, which can take out the moisture in the working liquid, reduces energy consumption, and makes the production process safer. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 Schematic diagram of the oxidation reaction extraction process for producing hydrogen peroxide.

[0034] In the figure: 1. hydrogenation liquid inlet, 2. oxygen-containing gas inlet, 3. medium-pressure oxidation tail gas, 4. hydrogen peroxide dilute product inlet, 5. concentrated oxidation liquid outlet, 6. water phase outlet, 7. oil phase outlet, 8. low-pressure oxidation tail gas pipe, 9. extractant inlet with pure water plus stabilizer, 10. raffinate outlet, 11. coalescer drainage, 12. dehydrated raffinate, 13. stripping raffinate outlet, 14. tail gas outlet, 15. oxidation extraction tower, 16. oxidation liquid separator, 17. extraction tower, 18. hydrogen peroxide dilute product pump, 19. coalescer, 20. dehydrator. Specific implementation plan

[0035] The technical solution of the present invention is described below with specific embodiments, but the protection scope of the present invention is not limited thereto.

[0036] Example 1

[0037] Relying on the oxidation reaction extraction device as described above, the oxidation extraction tower 15 has a diameter of 600mm, a height of 10m, and a number of plates of 8; the oxidation liquid separator 16 has a diameter of 600mm and a length of 3m; the extraction tower 7 has a diameter of 600mm, a height of 12m, and a number of plates of 15; the coalescer 19 has a diameter of 600mm and a length of 3m; the dehydrator 20 has a diameter of 800mm and a height of 2m. The hydrogenation liquid flow rate is 5m 3 / h, hydrogenation efficiency is 6.5g / L, oxygen-containing gas is 140Nm 3 / h. The operating pressure of the oxidation extraction tower is 0.3MPaG, and the operating temperature is 45-55°C. The results show that the oxidation yield of the oxidation extraction tower 15 is 97.2%, the concentrated hydrogen peroxide product output by the oxidation liquid separator 16 is 33wt%, and the water content of the working liquid output by the dehydrator 20 is 2300ppm.

[0038] Example 2

[0039] Relying on the oxidation reaction extraction device as described above, the oxidation extraction tower 15 has a diameter of 600mm, a height of 10m, and a number of plates of 8; the oxidation liquid separator has a diameter of 600mm and a length of 3m; the extraction tower has a diameter of 600mm, a height of 12m, and a number of plates of 15; the coalescer has a diameter of 600mm and a length of 3m; the dehydrator has a diameter of 800mm and a height of 2m. The hydrogenation liquid flow rate is 5m 3 / h, hydrogenation efficiency is 8g / L, oxygen-containing gas is 173Nm 3 / h. The operating pressure of the oxidation extraction tower is 0.3MPaG, and the operating temperature is 45-55°C. The results show that the oxidation yield of the oxidation extraction tower 15 is about 96%, the concentrated hydrogen peroxide output by the oxidation liquid separator 16 is 37wt%, and the water content of the working liquid output by the dehydrator 20 is 2150ppm.

[0040] Example 3

[0041] Relying on the oxidation reaction extraction device as described above, the oxidation extraction tower 15 has a diameter of 600mm, a height of 10m, and a number of plates of 8; the oxidation liquid separator has a diameter of 600mm and a length of 3m; the extraction tower has a diameter of 600mm, a height of 12m, and a number of plates of 15; the coalescer has a diameter of 600mm and a length of 3m; the dehydrator has a diameter of 800mm and a height of 2m. The hydrogenation liquid flow rate is 5m 3 / h, hydrogenation efficiency is 12g / L, oxygen-containing gas is 260Nm 3 / h. The operating pressure of the oxidation extraction tower is 0.3MPaG, and the operating temperature is 45-55°C. The results show that the oxidation yield of the oxidation extraction tower is about 98%, the concentrated hydrogen peroxide product from the oxidation liquid separator is 43wt%, and the water content of the working liquid from the dehydrator 20 is 2000ppm.

[0042] Comparative Example 1

[0043] The oxidation extraction process uses conventional oxidation towers and extraction towers. The oxidation tower consists of two sections, the diameter of the two oxidation towers is 600mm, the height is 5m, and the number of plates of the two towers is 4; the diameter of the extraction tower is 600mm, the height is 12m, and the number of plates is 15; the hydrogenated liquid enters from the bottom of the upper tower and flows upward with the air from the lower tower, and the gas and liquid are separated at the top, the gas is treated for exhaust gas, and the liquid overflows to the bottom of the lower tower and flows upward with the air at the bottom of the lower tower. Similarly, the gas and liquid are separated at the top of the lower tower, and the gas goes to the bottom of the upper tower. The liquid is discharged as the oxidation liquid, and after being buffered in the oxidation liquid storage tank, it enters the bottom of the extraction tower and contacts with the pure water coming down from the top in countercurrent. The crude hydrogen peroxide is obtained at the bottom of the extraction tower, and the top raffinate enters the agglomerator for separation and dehydration. The hydrogenated liquid flow rate is 5m 3 / h, hydrogenation efficiency is 8g / L, oxygen-containing gas is 190Nm 3 / h. The operating pressure of the oxidation tower is 0.25MPaG, and the operating temperature is 45-55℃. The operating pressure of the extraction tower is normal pressure, and the operating temperature is 50℃. The results show that the oxidation yield of the oxidation tower is about 90%, the crude hydrogen peroxide product from the extraction tower is 23wt%, and the water content of the working liquid from the coalescer is 5000ppm.

[0044] Comparative Example 2

[0045] The countercurrent contact oxidation tower disclosed in CN217868137U as the background technology scheme is adopted and a conventional countercurrent extraction tower is additionally configured for extracting the concentrated oxidation liquid discharged from the oxidation tower. Among them, the oxidation tower has a diameter of 600mm, a height of 10m, and a number of plates of 8; the oxidation liquid separator has a diameter of 300mm and a height of 2m; the extraction tower has a diameter of 600mm, a height of 12m, and a number of plates of 15; the hydrogenation liquid flow rate is 5m 3 / h, hydrogenation efficiency is 6.5g / L, oxygen-containing gas is 140Nm 3 / h. The operating pressure of the oxidation tower is 0.3MPaG, and the operating temperature is 45-55°C. The results show that the oxidation yield of the oxidation tower is 94%, and the output hydrogen peroxide concentration is 29wt%.

[0046] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any way. Any simple modification, change and equivalent transformation made to the above embodiment based on the technical essence of the present invention still falls within the protection scope of the technical solution of the present invention.

Claims

1. An oxidation reaction extraction device for producing hydrogen peroxide, comprising an oxidation extraction tower (15), an oxidation liquid separator (16), an extraction tower (17) and a coalescer (19), characterized in that: The oxidation extraction tower (15) is used to perform countercurrent oxidation and parallel current extraction processes. The top of the oxidation extraction tower (1) is provided with a hydrogenation liquid inlet (1) for introducing the hydrogenation liquid to be oxidized from the top of the tower, the bottom is provided with an oxygen-containing gas inlet (2) for introducing the oxygen-containing gas from the bottom of the tower, and the middle and lower part and above the oxygen-containing gas inlet (2) is provided with a hydrogen peroxide rare product inlet (4) for introducing the hydrogen peroxide rare product for extraction from the middle and lower part of the tower body; the oxidation liquid and the hydrogen peroxide rare product flow from top to bottom in the oxidation extraction tower (15), and the oxygen-containing gas flows from bottom to top in the oxidation extraction tower (15), thereby forming an oxidation extraction process in which the whole tower is countercurrently oxidized and the bottom of the tower is parallelly extracted; the top of the oxidation extraction tower (15) is provided with a medium-pressure tail gas outlet (3); the bottom of the oxidation extraction tower (15) is provided with a concentrated oxidation liquid outlet (5), and the The oxidizing liquid separator (16) is connected to the oxidizing liquid separator (16) through a pipeline; an overflow baffle is provided inside the oxidizing liquid separator (16), and a water phase outlet (6) and an oil phase outlet (7) are provided on both sides of the overflow baffle; the water phase outlet (6) is located at the bottom of the oxidizing liquid separator (16) and is used to discharge the concentrated hydrogen peroxide product after oil-water separation; the oil phase outlet (7) is connected to the bottom of the extraction tower (17) through a pipeline, and the top of the oxidizing liquid separator (16) is also provided with an oxidation tail gas outlet; the top of the extraction tower (17) is provided with an extractant inlet (9) for inputting a pure water extractant added with a stabilizer into the extraction tower (17); the bottom of the extraction tower (17) is provided with a hydrogen peroxide dilute product outlet, and its pipeline is connected to the hydrogen peroxide dilute product inlet (4) at the middle and lower part of the oxidizing extraction tower (15).

2. The oxidation reaction extraction device for producing hydrogen peroxide as claimed in claim 1, characterized in that: A hydrogen peroxide rare product pump (18) is provided on a pipeline connecting the hydrogen peroxide rare product outlet of the extraction tower (17) and the hydrogen peroxide rare product inlet (4) of the oxidation extraction tower (15).

3. The oxidation reaction extraction device for producing hydrogen peroxide as claimed in claim 2, characterized in that: The top of the extraction tower (17) is provided with a second oxidation tail gas outlet, which is collected together with the oxidation tail gas outlet at the top of the extraction tower (17) in a low-pressure oxidation tail gas pipe (8); the top side wall of the extraction tower (17) is provided with a raffinate outlet (10), which is connected to a coalescer (19) through a pipeline; the coalescer (19) is provided with a drain outlet (11) and a working liquid outlet (12), which are used to discharge water and working liquid generated by the raffinate after coalescence treatment, respectively.

4. The oxidation reaction extraction device for producing hydrogen peroxide as claimed in claim 3, characterized in that: It also includes a dehydrator (20), which has a accommodating cavity, and the accommodating cavity is connected to the working fluid outlet (12) of the coalescer (19) through a pipeline; the outlet end of the low-pressure oxidation tail gas pipe (8) extends into the bottom of the accommodating cavity and is immersed below the liquid level of the working fluid; the top of the dehydrator (20) is provided with a tail gas outlet (14), and the bottom is provided with a dehydrated working fluid outlet (13).

5. The oxidation reaction extraction device for producing hydrogen peroxide as claimed in claim 4, characterized in that: The oxidative extraction tower (15) is a plate tower; the extraction tower (7) is also a plate tower, and a polymer material grid or a woven mesh is arranged under the tower plate, and the polymer material is at least one of polypropylene or a fluorine-containing polymer.

6. An oxidation reaction extraction method for producing hydrogen peroxide, which is carried out by using the oxidation reaction extraction device according to any one of claims 1 to 5, characterized in that: The steps include: (1) introducing the hydrogenated liquid from the top of the oxidation extraction tower (15), and introducing the oxygen-containing gas (2) from the bottom of the oxidation extraction tower (15), the two are in countercurrent contact in the oxidation extraction tower (15), and an oxidation reaction occurs to continuously generate hydrogen peroxide; (2) While step (1) is being carried out, dilute hydrogen peroxide is added to the middle and lower part of the oxidation extraction tower (15), and the dilute hydrogen peroxide gradually extracts the hydrogen peroxide produced by the reaction into the water phase; (3) introducing the concentrated oxidizing liquid into the oxidizing liquid separator (16) at the bottom of the oxidizing extraction tower (15) for water-oil phase separation, extracting the concentrated hydrogen peroxide product at the water phase outlet (6), and introducing the dilute oxidizing liquid into the bottom of the extraction tower (17) at the oil phase outlet (7); (4) Pure water with added stabilizer and dilute oxidizing liquid are countercurrently contacted in an extraction tower (17), and a dilute hydrogen peroxide product is obtained at the bottom of the extraction tower (17). The dilute hydrogen peroxide product is pressurized through a pipeline and a dilute hydrogen peroxide product pump (18) and then sent to the dilute hydrogen peroxide product inlet (4) of the oxidation extraction tower (15); a raffinate is obtained at the top of the extraction tower (17), and the raffinate is sent to a coalescer (19) for coalescence and dehydration; (5) The raffinate is separated from the entrained water in the coalescer (19) and enters the dehydrator (20). At the same time, the tail gas discharged from the oxidation liquid separator (16) and the extraction tower (17) is transported to the dehydrator (20) through the low-pressure oxidation tail gas pipe (8) for bubbling to take away the remaining water in the working liquid; the tail gas discharged from the dehydrator (20) is treated with tail gas, and the dehydrated working liquid is returned to the upstream hydrogenation reactor.

7. The oxidation reaction extraction method for producing hydrogen peroxide as claimed in claim 6, characterized in that: The hydrogenation efficiency of the feed hydrogenated liquid of the oxidative extraction tower (15) is 6 to 20 g / L, and the oxygen concentration of the oxygen-containing gas is 20 to 100 vt%.

8. The oxidation reaction extraction method for producing hydrogen peroxide as claimed in claim 7, characterized in that: The oxidation yield of the oxidation extraction tower (15) is 96-98%; the operating pressure is 0.2-1.0 MPaG, and the operating temperature is 45-58°C; the residence time of the water-oil phase separation in the oxidation liquid separator (16) is 2-15 minutes, the concentration of hydrogen peroxide in the water phase discharge is 33-43wt%, and the hydrogen peroxide content in the oil phase discharge is 6-10g / L.

9. The oxidation reaction extraction method for producing hydrogen peroxide as claimed in claim 8, characterized in that: The oxidation liquid separator (16) and the extraction tower (7) are gas-connected, and the operating pressure is 0.03-0.25 MPaG; the flow ratio of the tail gas to the working liquid entering the dehydrator 20 is 1:20-1:5 (v / v%), and the water content in the dehydrated working liquid leaving the dehydrator (20) is 300-3000 ppm; the operating pressure of the dehydrator (20) is 0.005-0.1 MPaG, and the operating temperature is 45-55°C.

10. The oxidation reaction extraction method for producing hydrogen peroxide as claimed in claim 9, characterized in that: The working fluid is a mixture of alkyl anthraquinone, heavy aromatic hydrocarbons and polar solvents; the alkyl anthraquinone is at least one of 2-ethyl anthraquinone, 2-butyl anthraquinone and 2-pentyl anthraquinone; the polar solvent is at least one of trioctyl phosphate, 2-methylcyclohexyl acetate, tetrabutyl urea and diisobutyl carbinol.

Images