A hydrogen peroxide extraction system and method

Abstract

The present application relates to hydrogen peroxide extraction technical field, disclose a kind of hydrogen peroxide extraction system and method.The system includes primary plate column and secondary packing column, the bottom of the primary plate column and the top of the secondary packing column are communicated with each other, the upper portion of the primary plate column has heavy phase feed port, the lower portion of the secondary packing column has light phase feed port;The packing section of the secondary packing column includes several packing trays, each packing tray is stacked by multiple corrugated packing sheets along horizontal direction, and the peak and valley between adjacent two corrugated packing sheets are stacked to form multiple mutually parallel inclined quadrangular prism channels, and the inclination angle α of the inclined quadrangular prism channel is 20°-80°.The method can not only directly extract more than 35wt% hydrogen peroxide aqueous solution, but also can eliminate the explosion risk of high-concentration hydrogen peroxide aqueous solution in contact with anthraquinone working fluid during extraction process.

Description

Technical Field

[0001] This invention relates to the field of hydrogen peroxide extraction technology, and more specifically to a hydrogen peroxide extraction system and method. Background Technology

[0002] Hydrogen peroxide is an important industrial raw material, and its aqueous solution is widely used in chemical oxidation, environmental treatment, disinfection, papermaking, and the food industry. The anthraquinone process is the only mature industrial method for producing hydrogen peroxide, and more than 98% of the world's hydrogen peroxide is obtained using this method.

[0003] Currently, the dominant process for hydrogen peroxide production is the palladium catalyst-anthraquinone hydrogenation process, which consists of a hydrogenation unit, an oxidation unit, an extraction and purification unit, a post-treatment unit, and alkaline evaporation. The anthraquinone process for producing hydrogen peroxide mainly includes three core steps: alkylanthraquinone hydrogenation, hydrogenated alkylanthraquinone oxidation, and hydrogen peroxide extraction. Industrially, a working solution containing 5–10 g / L of hydrogen peroxide is generally obtained through two steps: hydrogenation and oxidation. This solution is then extracted with water to obtain an aqueous hydrogen peroxide solution with a concentration of approximately 27.5 wt.% or 35 wt.%. The extraction and purification unit process is as follows: Utilizing the difference in solubility of hydrogen peroxide in water and the working solution, as well as the density difference between the working solution and water, the working solution containing hydrogen peroxide is extracted with pure water in an extraction tower to obtain an aqueous hydrogen peroxide solution. This aqueous solution is then purified in a purification tower using heavy aromatics to obtain hydrogen peroxide with a concentration of 27.5 wt% or 35 wt%. In some applications, 27.5 wt.% or 35 wt.% hydrogen peroxide aqueous solutions are insufficient, requiring further distillation and concentration to obtain higher concentrations, such as 45 wt.%, 50 wt.%, 60 wt.%, or 70 wt.%. This concentration process employs falling film evaporation, which is energy-intensive.

[0004] Multistage countercurrent extraction of water and anthraquinone working solution is the main method for obtaining hydrogen peroxide aqueous solutions of approximately 27.5 wt.% or 35 wt.%. Industrially, extraction towers are commonly used for this process. Due to the low hydrogen peroxide content in the anthraquinone working solution, this extraction is an extreme ratio process, with oil-to-water volume ratios exceeding 40:1. This system is prone to emulsification under improper operation, making stable operation of the extraction tower a key challenge. In recent years, some novel tower internals and tower types (CN209143698U, CN101279720A) have been developed to continuously improve hydrogen peroxide extraction equipment along this line of thinking. However, overall, the industrial implementation of large-scale tower equipment still faces significant challenges, and the concentration of hydrogen peroxide remains difficult to exceed the 35 wt.% concentration limit through extraction methods. However, with the improvement of the anthraquinone hydrogen peroxide process technology, the hydrogen peroxide content in the working solution generally reaches about 10 g / L, and in some devices, the hydrogen peroxide content in the working solution can reach 14 g / L, which meets the conditions for direct extraction to obtain a hydrogen peroxide aqueous solution of about 50 wt.%. If a high-concentration hydrogen peroxide solution can be obtained by direct extraction, the concentration unit can be eliminated, the process flow can be shortened, energy consumption can be reduced, and the green and low-carbon level of the process can be improved.

[0005] However, the literature (Kirk-Othmer. Hydrogen Peroxide in Encyclopedia of Chemical Technology. 2006, John Wiley & Sons, Inc.) reports that hydrogen peroxide can form a multi-component heterogeneous system with the working fluid during the extraction process, which may lead to an explosion. The literature suggests that the extraction concentration should not exceed 44 wt%. The relevant mechanism has not been publicly reported, which greatly restricts the development of processes for directly extracting high concentrations of hydrogen peroxide.

[0006] According to the principle of extraction, the bottom of the extraction tower has the highest extraction yield. The book "Hydrogen Peroxide Production Technology" (Zhang Guochen, Chemical Industry Press, 2012.1, p. 186) states: "In the first few trays of the extraction tower, almost 70% of the extraction task is completed. Ten trays have already extracted 76.8%–79.8% of the hydrogen peroxide from the oxidation liquid to the aqueous phase. The remaining 35 trays reduce the hydrogen peroxide concentration in the oxidation liquid from 1.52–1.82 g / L to about 0.1 g / L." Therefore, the hydrogen peroxide concentration in the first few trays at the bottom of the extraction tower will be within the explosive range.

[0007] To prevent the entire extraction tower from exploding, there is an urgent need for a hydrogen peroxide extraction system that has explosion suppression and prevention functions while improving extraction efficiency. Summary of the Invention

[0008] The purpose of this invention is to overcome the problems of explosive hydrogen peroxide concentrations in the first few trays at the bottom of existing extraction towers during hydrogen peroxide extraction, as well as the high cost. This invention provides a hydrogen peroxide extraction system and method. This method can not only directly extract an aqueous solution of hydrogen peroxide with a concentration of over 35 wt%, but also eliminates the explosion risk associated with high-concentration hydrogen peroxide solutions contacting the anthraquinone working solution during the extraction process.

[0009] To achieve the above objectives, the present invention provides a hydrogen peroxide extraction system, which includes a primary plate column and a secondary packed column. The bottom of the primary plate column and the top of the secondary packed column are connected to each other. The upper part of the primary plate column has a heavy phase feed inlet, and the lower part of the secondary packed column has a light phase feed inlet.

[0010] The packing section of the secondary packed tower includes several packing discs. Each packing disc is composed of multiple corrugated packing sheets stacked horizontally. The crests and troughs of two adjacent corrugated packing sheets are superimposed to form multiple parallel oblique quadrangular prism channels. The inclination angle α of the oblique quadrangular prism channels is 20° to 80°.

[0011] Preferably, the bottom of the primary plate tower is provided with a first heavy phase outlet and a first light phase inlet, and the top of the secondary packed tower is provided with a first heavy phase inlet and a first light phase outlet. The first heavy phase outlet and the first heavy phase inlet are connected, and the first light phase inlet and the first light phase outlet are connected.

[0012] Preferably, the first-stage plate tower has a second light phase outlet at the top, and the second-stage packed tower has a second heavy phase outlet at the bottom.

[0013] Preferably, the multiple oblique quadrangular prism channels of two adjacent packing discs correspond one-to-one in the vertical direction, and the corresponding oblique quadrangular prism channels intersect each other.

[0014] Preferably, each packing disc is cylindrical, and each packing disc is composed of multiple corrugated packing sheets of different lengths stacked together, with the length of the multiple corrugated packing sheets gradually decreasing from the center along the radial direction of the cylindrical packing disc.

[0015] Preferably, the height of the packing section is 2-6m, more preferably 3-5m; the height of each packing disc is 30-500mm, more preferably 50-200mm.

[0016] Preferably, each corrugated packing sheet has a peak height of 2-6 mm, a peak width d of 3-10 mm, and a thickness of 0.5-3 mm.

[0017] Preferably, the included angle β between the two corrugations of the corrugated packing sheet (23) is 15 to 85°.

[0018] Preferably, the corrugated packing sheet is a plate mesh corrugated packing sheet, wherein the wire diameter of the plate mesh is 0.1 to 4 mm.

[0019] Preferably, the mesh shape of the plate mesh is square, rectangular, or rhomboid, wherein the mesh area is (3-20) x (3-20) mm. 2 .

[0020] Preferably, the primary plate tower is a sieve plate tower with a theoretical number of 10 to 30 plates.

[0021] A second aspect of the present invention provides a hydrogen peroxide extraction method, which is implemented in the system described in the first aspect above. The method includes: introducing water from the heavy phase feed inlet, introducing anthraquinone working solution from the light phase feed inlet, and having the anthraquinone working solution and water in a countercurrent contact in the primary plate column and the secondary packed column.

[0022] Preferably, the anthraquinone working solution and water, after countercurrent contact in the primary plate column, are drawn out from the first heavy phase outlet and then enter the secondary packed column from the first heavy phase inlet to countercurrently contact the anthraquinone working solution; the anthraquinone working solution after countercurrent contact of the anthraquinone working solution and the hydrogen peroxide aqueous solution in the secondary packed column is drawn out from the first light phase outlet and then enters the primary plate column from the first light phase inlet to countercurrently contact the hydrogen peroxide aqueous solution.

[0023] Preferably, the countercurrent contact conditions in the primary plate tower include: a temperature of 50–55°C and a pressure of atmospheric pressure.

[0024] Preferably, the countercurrent contact conditions in the secondary packed tower include: a temperature of 50–55°C and a pressure of atmospheric pressure.

[0025] Preferably, the hydrogen peroxide concentration in the anthraquinone working solution is 6–20 g / L.

[0026] Preferably, the volume ratio of water introduced from the heavy phase inlet to anthraquinone working solution introduced from the light phase inlet is 1:30 to 70.

[0027] Compared with the prior art, the present invention has at least the following advantages:

[0028] (1) The present invention divides the extraction tower into two stages, namely a primary plate tower and a secondary packed tower. At the same time, the high-concentration area with explosion risk is separated from the low-concentration area without explosion risk, and the extraction is carried out in the secondary packed tower and the primary plate tower respectively, thereby reducing the amount of material affected by the explosion and eliminating the explosion risk of high-concentration hydrogen peroxide aqueous solution coming into contact with anthraquinone working solution during the extraction process.

[0029] (2) The structure of the structured packing layer in the secondary packed tower has a cutting and breaking effect on the droplets, reducing the droplet diameter of the anthraquinone working solution and increasing the mass transfer area between the two phases. This enhances the mass transfer process, improves the extraction efficiency, and thus reduces the height of the mass transfer unit, saving equipment investment. Comparative experiments were conducted using a traditional sieve plate extraction device and the present invention, testing the mass transfer efficiency under the same operating conditions. The experimental results show that the extraction efficiency of the extraction equipment and method for producing hydrogen peroxide using the anthraquinone process of the present invention is significantly higher than that of the traditional sieve plate extraction equipment and process.

[0030] (3) Using the system described in this invention, hydrogen peroxide aqueous solution with a content of more than 35 wt% can be directly extracted, and the maximum content can reach 70 wt%, thereby eliminating the hydrogen peroxide concentration unit and reducing investment and energy consumption. Attached Figure Description

[0031] Figure 1 This is a schematic diagram of the hydrogen peroxide extraction system described in this invention;

[0032] Figure 2 This is a schematic diagram of the single corrugated packing sheet described in this invention;

[0033] Figure 3 This is a schematic diagram of the oblique quadrangular prism channel formed by the two corrugated packing sheets described in this invention;

[0034] Figure 4 This is a schematic diagram of the filling angle of the two packing discs.

[0035] Explanation of reference numerals in the attached figures

[0036] 1. Primary plate tower; 2. Secondary packed tower; 11. Heavy phase inlet; 12. First heavy phase outlet; 13. First light phase inlet; 14. Second light phase outlet; 21. Light phase inlet; 22. Packing section; 23. Corrugated packing sheet; 24. Crest; 25. Trough; 26. Inclined quadrangular prism channel; 27. First heavy phase inlet; 28. First light phase outlet; 29. ​​Second heavy phase outlet. Detailed Implementation

[0037] The specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings. It should be understood that the specific embodiments described herein are for illustration and explanation only and are not intended to limit the present invention.

[0038] The endpoints and any values ​​of the ranges disclosed herein are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of the various ranges, the endpoint values ​​of the various ranges and individual point values, and individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed herein.

[0039] The first aspect of this invention provides a hydrogen peroxide extraction system, such as... Figure 1 As shown, the system includes a primary plate tower 1 and a secondary packed tower 2. The bottom of the primary plate tower 1 and the top of the secondary packed tower 2 are connected to each other. The upper part of the primary plate tower 1 has a heavy phase inlet 11, and the lower part of the secondary packed tower 2 has a light phase inlet 21.

[0040] The hydrogen peroxide extraction system described in this invention includes two-stage extraction towers. A low-concentration hydrogen peroxide aqueous solution and a high-concentration hydrogen peroxide aqueous solution are obtained in a first-stage plate tower 1 and a second-stage packed tower 2, respectively. This isolates the low-concentration zone with no explosion risk from the high-concentration zone with an explosion risk, reducing the amount of material affected by an explosion. At the same time, the packing material in the second-stage packed tower 2 is uniquely designed to give the structured packing material in the second-stage packed tower 2 an explosion-suppressing and explosion-proof function, thereby preventing the high-concentration hydrogen peroxide aqueous solution from exploding when it comes into contact with the anthraquinone working solution during the extraction process.

[0041] Specifically, water is introduced from the heavy phase inlet 11 of the primary plate column 1, flows from top to bottom, exits from the bottom of the primary plate column 1, enters the secondary packed column 2 from the top of the secondary packed column 2, and flows from top to bottom in the secondary packed column 2; while the anthraquinone working solution is introduced from the light phase inlet 21 of the secondary packed column 2, moves from bottom to top, exits from the top of the secondary packed column 2, enters from the bottom of the primary plate column 1, and moves from bottom to top in the secondary packed column 2. Thus, the anthraquinone working solution and water come into countercurrent contact in the primary plate column 1 and the secondary packed column 2 to extract hydrogen peroxide.

[0042] The plate column 1 is divided into a raffinate section and an extraction-mass transfer section. The uppermost plate of the plate column is the raffinate section, where the extractant phase is pure water, and the extractable phase is the anthraquinone working solution from the secondary packed column 2. The density difference between the anthraquinone working solution and the aqueous phase in this section is very close, resulting in a low mass transfer driving force and difficulty in mass transfer, requiring a large number of plates for raffinate removal. The lower part of the plate column is the extraction-mass transfer section. In this section, the extractant phase is a low-concentration hydrogen peroxide solution from the raffinate section, and the extractable phase is the anthraquinone working solution from the secondary packed column 2. The density difference between the anthraquinone working solution and the aqueous phase in this section is greater than in the raffinate section, resulting in a greater mass transfer driving force. Extraction separation in this section can increase the hydrogen peroxide concentration of the extractant phase to approximately 30 wt%.

[0043] In this invention, the packing section 22 of the secondary packed tower 2 includes a plurality of packing discs, such as... Figure 2 and Figure 3As shown, each packing disc is formed by stacking multiple corrugated packing sheets 23 horizontally, and the crests 24 and troughs 25 of adjacent corrugated packing sheets 23 are superimposed to form multiple parallel oblique quadrangular prism channels 26, the inclination angle α of the oblique quadrangular prism channels 26 being 20° to 80°. In this document, the inclination angle α refers to an acute angle.

[0044] In the secondary packed tower 2, since there are oblique quadrangular prism channels 26 between adjacent corrugated packing sheets 23, the extractable phase and the extracted phase can be extracted and separated in their respective narrow channels, thereby separating the system into multiple smaller oblique quadrangular prism channels 26; furthermore, the peak height h of the corrugated packing sheet 23 is limited to an appropriate range, and the equivalent diameter of the oblique quadrangular prism channel 26 is smaller than the explosive critical diameter of the system, thereby achieving the effect of explosion prevention and explosion suppression.

[0045] According to the present invention, the secondary packed tower 2 having the aforementioned packing structure is a hydrogen peroxide concentration section. In this region, the extractant phase is low-concentration hydrogen peroxide obtained from the raffinate section and the extraction mass transfer section, and the extracted phase is fresh anthraquinone working solution. In this region, low-concentration hydrogen peroxide is used to extract hydrogen peroxide from the fresh anthraquinone working solution. The density difference between the anthraquinone working solution phase and the aqueous phase in this region is large, resulting in a strong mass transfer driving force. This allows for the production of high-concentration hydrogen peroxide products (above 35 wt%) through enhanced extraction mass transfer. Furthermore, the secondary packed tower 2 of the present invention uses a structured packing with non-interconnected oblique quadrangular prisms, which can prevent the risk of combustion and explosion when hydrogen peroxide (above 44 wt%) is mixed with the anthraquinone working solution, thus providing explosion suppression and prevention functions.

[0046] According to the present invention, such as Figure 3 As shown, multiple corrugated packing sheets 23 are stacked at an angle to form multiple oblique quadrangular prism channels 26. (See diagram) Figure 2 As shown, the horizontal plane where the wave crest 24 is located is at a higher level than the horizontal plane where the wave trough 25 is located.

[0047] In this invention, under preferred conditions, the oblique quadrangular prism channels 26 in the same packing disc are all the same shape, and the channel directions of the oblique quadrangular prism channels 26 formed by two adjacent corrugated packing sheets 23 are parallel to each other.

[0048] In a preferred embodiment, such as Figure 1 As shown, the first-stage plate tower 1 has a first heavy phase outlet 12 and a first light phase inlet 13 at the bottom, and the second-stage packed tower 2 has a first heavy phase inlet 27 and a first light phase outlet 28 at the top. The first heavy phase outlet 12 and the first heavy phase inlet 27 are connected, and the first light phase inlet 13 and the first light phase outlet 28 are connected.

[0049] In this connection, the low-concentration hydrogen peroxide aqueous solution obtained by the countercurrent contact of anthraquinone working solution and water in the first-stage plate column 1 is drawn out from the first heavy phase outlet 12 and then enters the second-stage packed column 2 from the first heavy phase inlet 27 to have countercurrent contact with the anthraquinone working solution. The anthraquinone working solution after the countercurrent contact of the anthraquinone working solution and the hydrogen peroxide aqueous solution in the second-stage packed column 2 is drawn out from the first light phase outlet 28 and then enters the first-stage plate column 1 from the first light phase inlet 13 to have countercurrent contact with the hydrogen peroxide aqueous solution. Using this extraction method, as the extract phase flows downwards in the first-stage plate column 1, the concentration of hydrogen peroxide in the extract phase increases. After entering the second-stage packed column 2, as the extract phase flows downwards in the second-stage packed column 2, the concentration of hydrogen peroxide in the extract phase increases further, with the highest concentration of hydrogen peroxide in the extract phase at the bottom of the second-stage packed column 2.

[0050] According to the present invention, the first-stage plate column 1 has a second light phase outlet 14 at the top, and the second-stage packed column 2 has a second heavy phase outlet 29 at the bottom. The hydrogen peroxide in the anthraquinone working solution extracted in the second-stage packed column 2 and the first-stage plate column 1 is greatly reduced and finally exits from the second light phase outlet 14 at the top of the first-stage plate column 1, while the extractant phase, after extracting hydrogen peroxide in the first-stage plate column 1 and the second-stage packed column 2, is exited from the second heavy phase outlet 29 at the bottom of the second-stage packed column 2.

[0051] In this invention, the number of packing discs in the packing section 22 of the secondary packed tower 2 and the number of corrugated packing sheets 23 forming each packing disc are not limited and can be selected according to the actual height and inner diameter of the secondary packed tower 2.

[0052] In one specific embodiment, the multiple oblique quadrangular prism channels 26 of two adjacent packing discs correspond one-to-one in the vertical direction, and the corresponding oblique quadrangular prism channels 26 intersect each other. The one-to-one correspondence of the multiple oblique quadrangular prism channels 26 of two adjacent packing discs in the vertical direction allows the material flow of different channels to be extracted independently along their respective one-to-one corresponding channels throughout the entire packing section 22, avoiding cross-flow of material flow between different channels, which would affect the mass transfer process between material flow and reduce extraction efficiency; while the intersecting arrangement of the one-to-one corresponding oblique quadrangular prism channels 26 allows the liquid in each channel to be deflected during the flow process, which is beneficial to enhance mass transfer.

[0053] According to the present invention, under preferred conditions, each packing disc is cylindrical, and each packing disc is stacked from top to bottom to form a packing segment 22. Further, each packing disc is formed by stacking multiple corrugated packing sheets 23 of different lengths, and the length of the multiple corrugated packing sheets 23 gradually decreases from the center along the radial direction of the cylindrical packing disc. That is, the corrugated packing sheet 23 passing through the center of the cylindrical packing disc has the longest length, and the length of the corrugated packing sheets 23 extending from the center to the arc direction becomes shorter and shorter, thus forming a cylindrical shape.

[0054] In this invention, multiple packing discs are placed in the packing section 22, and the number of packing discs is determined according to the height of the packing section 22 and the height of each packing disc.

[0055] In a preferred embodiment, the height of the packing section 22 can be 2 to 6 m, preferably 3 to 5 m, such as 3 m, 4 m or 5 m; the height of each packing disc is 30 to 500 mm, preferably 50 to 200 mm, such as 50 mm, 80 mm, 100 mm, 120 mm, 150 mm, 180 mm or 200 mm.

[0056] The secondary packed tower 2 of the present invention forms an oblique quadrangular prism channel 26 in the packing tray. The peaks and troughs are designed according to the critical quenching diameter of the explosion system, which can ensure that the size of the oblique quadrangular prism channel 26 is below the critical quenching diameter, thereby achieving the inherent safety of the extraction process of the explosion system.

[0057] In some preferred embodiments, the peak height h of each corrugated packing sheet 23 can be 2 to 6 mm, for example 2 mm, 2.5 mm, 3 mm, 3.5 mm, 4 mm, 4.5 mm, 5 mm, 5.5 mm or 6 mm; the peak width d can be 3 to 10 mm, for example 3 mm, 4 mm, 5 mm, 6 mm, 7 mm, 8 mm, 9 mm or 10 mm; and the thickness can be 0.5 to 3 mm, for example 0.5 mm, 1 mm, 1.5 mm, 2 mm, 2.5 mm or 3 mm.

[0058] In some preferred embodiments, the included angle β between the two corrugations of the corrugated packing sheet 23 is 15-85°, preferably 15°, 30°, 45°, 60°, 75° or 85°.

[0059] According to the present invention, under preferred conditions, the corrugated packing sheet 23 is a plate mesh corrugated packing sheet, wherein the wire diameter of the plate mesh can be 0.1 to 4 mm, for example 0.1 mm, 0.2 mm, 0.4 mm, 0.5 mm, 0.8 mm, 1 mm, 1.5 mm, 2 mm, 2.5 mm, 3 mm, 3.5 mm or 4 mm.

[0060] Furthermore, the mesh shape of the plate mesh is not limited and can be any shape well known in the art. Specifically, the mesh shape of the plate mesh is square, rectangular, or rhomboid. The mesh area is (3–20) x (3–20) mm. 2 .

[0061] In this invention, the primary plate tower 1 is a conventional sieve plate tower, and the plates therein are conventionally used plates. In specific embodiments, the number of plates in the primary plate tower 1 can be adjusted according to actual conditions. Under preferred conditions, the theoretical number of plates is 10-30 layers, for example, 10 layers, 15 layers, 20 layers, 25 layers, or 30 layers.

[0062] The second aspect of the present invention provides a hydrogen peroxide extraction method, which is implemented in the system described in the first aspect above. The method includes: introducing water from the heavy phase feed inlet 11, introducing anthraquinone working solution from the light phase feed inlet 21, and having the anthraquinone working solution and water in countercurrent contact in the primary plate tower 1 and the secondary packed tower 2.

[0063] In the method described in this invention, water, as both the extraction phase and the heavy phase, is introduced from the heavy phase inlet 11 of the primary plate column 1, flows downward in the primary plate column 1, and is then drawn out from the bottom of the primary plate column 1, entering the secondary packed column 2 from the top and flowing downward in the secondary packed column 2. The anthraquinone working solution, as the extractable phase, is introduced from the light phase inlet 21 of the secondary packed column 2, flows upward in the secondary packed column 2, is drawn out from the top of the secondary packed column 2, and enters the primary plate column 1 from the bottom and flows upward in the primary plate column 1. This allows the anthraquinone working solution and water to come into countercurrent contact in the primary plate column 1 and the secondary packed column 2, extracting hydrogen peroxide from the anthraquinone working solution.

[0064] In a preferred embodiment, the anthraquinone working solution and water, after countercurrent contact in the primary plate column 1, are drawn out from the first heavy phase outlet 12 and then enter the secondary packed column 2 from the first heavy phase inlet 27 to have countercurrent contact with the anthraquinone working solution; the anthraquinone working solution after countercurrent contact with the hydrogen peroxide aqueous solution in the secondary packed column 2 is drawn out from the first light phase outlet 28 and then enters the primary plate column 1 from the first light phase inlet 13 to have countercurrent contact with the hydrogen peroxide aqueous solution.

[0065] The low-concentration hydrogen peroxide aqueous solution obtained by countercurrent contact of anthraquinone working solution and water in the first-stage plate column 1 is drawn out from the first heavy phase outlet 12 and then enters the second-stage packed column 2 from the first heavy phase inlet 27 to countercurrently contact with the anthraquinone working solution; the anthraquinone working solution after countercurrent contact of the anthraquinone working solution and the hydrogen peroxide aqueous solution in the second-stage packed column 2 is drawn out from the first light phase outlet 28 and then enters the first-stage plate column 1 from the first light phase inlet 13 to countercurrently contact with the hydrogen peroxide aqueous solution. In this extraction method, as the extractant phase flows downwards in the primary plate column 1, the concentration of hydrogen peroxide in the extractant phase increases. After entering the secondary packed column 2, the concentration of hydrogen peroxide in the extractant phase also increases as it flows downwards in the secondary packed column 2. The hydrogen peroxide concentration in the extractant phase at the bottom of the secondary packed column 2 is the highest. Therefore, the primary plate column 1 yields a low-concentration hydrogen peroxide solution, while the secondary packed column 2 yields a high-concentration hydrogen peroxide solution. This isolates the high-concentration zone with explosion risk from the low-concentration zone without explosion risk, allowing the extraction to proceed separately in the secondary packed column 2 and the primary plate column 1. This reduces the amount of material affected by explosion and eliminates the explosion risk of the high-concentration hydrogen peroxide aqueous solution contacting the anthraquinone working solution during the extraction process.

[0066] According to the present invention, the conditions under which the material is subjected to countercurrent extraction in the primary plate tower 1 and the secondary packed tower 2 have a certain influence on the extraction efficiency of hydrogen peroxide.

[0067] Under preferred conditions, the countercurrent contact conditions in the primary plate tower 1 include: the temperature can be 50-55℃, for example 50℃, 51℃, 52℃, 53℃, 54℃ or 55℃; and the pressure can be atmospheric pressure.

[0068] Under preferred conditions, the countercurrent contact conditions in the secondary packed tower 2 include: a temperature of 50-55°C, for example, 50°C, 51°C, 52°C, 53°C, 54°C, or 55°C; and a pressure of atmospheric pressure.

[0069] In the method described in this invention, specifically, the hydrogen peroxide concentration in the anthraquinone working solution can be 6 to 20 g / L, for example, 6 g / L, 8 g / L, 10 g / L, 12 g / L, 14 g / L, 16 g / L, 18 g / L or 20 g / L.

[0070] According to the present invention, limiting the ratio of extractant to extracted liquid within a suitable range can significantly improve the extraction efficiency of hydrogen peroxide. In a preferred embodiment, the volume ratio of water introduced from the heavy phase inlet 11 to anthraquinone working solution introduced from the light phase inlet 21 can be 1:30-70, for example 1:30, 1:35, 1:40, 1:45, 1:50, 1:55, 1:60, 1:65, or 1:70.

[0071] The present invention will be described in detail below through embodiments, but the scope of protection of the present invention is not limited thereto.

[0072] Example 1

[0073] Example 1 was carried out in the following hydrogen peroxide extraction system, such as... Figure 1-4 As shown:

[0074] The system includes a primary plate tower 1 and a secondary packed tower 2. The primary plate tower 1 is a sieve plate tower with a theoretical number of 10 plates. The opening diameter on the surface of the sieve plate is Ф2.2mm, and the opening rate is 14%.

[0075] The bottom of the primary plate tower 1 and the top of the secondary packed tower 2 are interconnected. The upper part of the primary plate tower 1 has a heavy phase inlet 11, and the lower part of the secondary packed tower 2 has a light phase inlet 21. The bottom of the primary plate tower 1 is provided with a first heavy phase outlet 12 and a first light phase inlet 13. The top of the secondary packed tower 2 is provided with a first heavy phase inlet 27 and a first light phase outlet 28. The first heavy phase outlet 12 and the first heavy phase inlet 27 are connected, and the first light phase inlet 13 and the first light phase outlet 28 are connected. The top of the primary plate tower 1 has a second light phase outlet 14, and the bottom of the secondary packed tower 2 has a second heavy phase outlet 29.

[0076] The packing section 22 of the secondary packed tower 2 includes 20 cylindrical packing discs. Each packing disc is formed by stacking corrugated packing sheets 23 of different lengths horizontally. The lengths of the corrugated packing sheets 23 gradually decrease from the center along the radius of the cylindrical packing disc. The crests 24 and troughs 25 of adjacent corrugated packing sheets 23 overlap to form multiple parallel oblique quadrangular prism channels 26. The inclination angle α of the oblique quadrangular prism channels 26 is 40°. The multiple oblique quadrangular prism channels 26 between adjacent packing discs... The channels 26 are vertically aligned and intersect each other; the height of the packing section 22 is 2m; the height of each packing disc is 100mm; the peak height h of each corrugated packing sheet 23 is 5mm, the peak width d is 6mm, the thickness is 1mm, and the included angle β between the two corrugations of each corrugated packing sheet 23 is 15°; the corrugated packing sheet 23 is a plate mesh corrugated packing sheet, wherein the wire diameter of the plate mesh is 0.4mm, the mesh opening is square, and the mesh area is 5x5mm. 2 .

[0077] Hydrogen peroxide extraction methods include:

[0078] Water is introduced from the heavy phase inlet 11, and anthraquinone working solution is introduced from the light phase inlet 21. The anthraquinone working solution and water are in countercurrent contact in the primary plate column 1 and the secondary packed column 2. The hydrogen peroxide aqueous solution obtained from the countercurrent contact of the anthraquinone working solution and water in the primary plate column 1 is drawn out from the first heavy phase outlet 12, and then enters the secondary packed column 2 from the first heavy phase inlet 27 to have countercurrent contact with the anthraquinone working solution. The anthraquinone working solution after the countercurrent contact of the anthraquinone working solution and the hydrogen peroxide aqueous solution in the secondary packed column 2 is drawn out from the first light phase outlet 28, and then enters the primary plate column 1 from the first light phase inlet 13 to have countercurrent contact with the hydrogen peroxide aqueous solution.

[0079] The countercurrent contact conditions in the primary plate tower 1 include: a temperature of 52°C and a pressure of atmospheric pressure; the countercurrent contact conditions in the secondary packed tower 2 include: a temperature of 52°C and a pressure of atmospheric pressure; a hydrogen peroxide concentration of 10.80 g / L in the anthraquinone working solution; and a water volume of 20 m³ introduced from the heavy phase feed inlet 11. 3 / h, the volume of anthraquinone working solution introduced from the light phase inlet 21 is 1300m³. 3 / h, the volume ratio of water to anthraquinone working solution is 1:65.

[0080] After extraction, the hydrogen peroxide concentration obtained from the second heavy phase outlet 29 at the bottom of the secondary packed tower 2 is 52.6 wt%, and the residual hydrogen peroxide content in the raffinate drawn from the second light phase outlet 14 at the top of the primary plate tower 1 is 0.10 g / L.

[0081] Example 2

[0082] Example 2 was carried out in the following hydrogen peroxide extraction system, such as... Figure 1-3 As shown:

[0083] The system includes a primary plate tower 1 and a secondary packed tower 2. The primary plate tower 1 is a sieve plate tower with a theoretical number of 12 plates. The opening diameter of the sieve plate surface is Ф2.2mm, and the opening rate is 14%.

[0084] The bottom of the primary plate tower 1 and the top of the secondary packed tower 2 are interconnected. The upper part of the primary plate tower 1 has a heavy phase inlet 11, and the lower part of the secondary packed tower 2 has a light phase inlet 21. The bottom of the primary plate tower 1 is provided with a first heavy phase outlet 12 and a first light phase inlet 13. The top of the secondary packed tower 2 is provided with a first heavy phase inlet 27 and a first light phase outlet 28. The first heavy phase outlet 12 and the first heavy phase inlet 27 are connected, and the first light phase inlet 13 and the first light phase outlet 28 are connected. The top of the primary plate tower 1 has a second light phase outlet 14, and the bottom of the secondary packed tower 2 has a second heavy phase outlet 29.

[0085] The packing section 22 of the secondary packed tower 2 includes 24 cylindrical packing discs. Each packing disc is formed by stacking corrugated packing sheets 23 of different lengths horizontally. The lengths of the corrugated packing sheets 23 gradually decrease from the center along the radius of the cylindrical packing disc. The crests 24 and troughs 25 of adjacent corrugated packing sheets 23 overlap to form multiple parallel oblique quadrangular prism channels 26. The inclination angle α of the oblique quadrangular prism channels 26 is 40°. The multiple oblique quadrangular prism channels between adjacent packing discs... 26 correspond one-to-one in the vertical direction, and the corresponding oblique quadrangular prism channels 26 intersect each other; the height of the packing section 22 is 2.4m; the height of each packing disc is 100mm; the peak height h of each corrugated packing sheet 23 is 5mm, the peak width d is 6mm, the thickness is 1mm, and the included angle β between the two corrugations of each corrugated packing sheet 23 is 15°; the corrugated packing sheet 23 is a plate mesh corrugated packing sheet, wherein the wire diameter of the plate mesh is 0.4mm, the mesh opening is square, and the mesh area is 5x5mm. 2 .

[0086] Hydrogen peroxide extraction methods include:

[0087] Water is introduced from the heavy phase inlet 11, and anthraquinone working solution is introduced from the light phase inlet 21. The anthraquinone working solution and water are in countercurrent contact in the primary plate column 1 and the secondary packed column 2. The hydrogen peroxide aqueous solution obtained from the countercurrent contact of the anthraquinone working solution and water in the primary plate column 1 is drawn out from the first heavy phase outlet 12, and then enters the secondary packed column 2 from the first heavy phase inlet 27 to have countercurrent contact with the anthraquinone working solution. The anthraquinone working solution after the countercurrent contact of the anthraquinone working solution and the hydrogen peroxide aqueous solution in the secondary packed column 2 is drawn out from the first light phase outlet 28, and then enters the primary plate column 1 from the first light phase inlet 13 to have countercurrent contact with the hydrogen peroxide aqueous solution.

[0088] The countercurrent contact conditions in the primary plate tower 1 include: a temperature of 53°C and a pressure of atmospheric pressure; the countercurrent contact conditions in the secondary packed tower 2 include: a temperature of 53°C and a pressure of atmospheric pressure; a hydrogen peroxide concentration of 10.80 g / L in the anthraquinone working solution; and a water volume of 20 m³ introduced from the heavy phase feed inlet 11. 3 The volume of anthraquinone working solution introduced from the light phase inlet 21 is 600 m³ / h. 3 / h, the volume ratio of water to anthraquinone working solution is 1:30.

[0089] After extraction, the hydrogen peroxide concentration obtained from the second heavy phase outlet 29 at the bottom of the secondary packed tower 2 is 44.2 wt%, and the residual hydrogen peroxide content in the raffinate drawn from the second light phase outlet 14 at the top of the primary plate tower 1 is 0.10 g / L.

[0090] Example 3

[0091] Example 3 was carried out in the following hydrogen peroxide extraction system, such as... Figure 1-3 As shown:

[0092] The system includes a primary plate tower 1 and a secondary packed tower 2. The primary plate tower 1 is a sieve plate tower with a theoretical number of 16 plates. The opening diameter on the surface of the sieve plate is Ф2.2mm, and the opening rate is 14%.

[0093] The bottom of the primary plate tower 1 and the top of the secondary packed tower 2 are interconnected. The upper part of the primary plate tower 1 has a heavy phase inlet 11, and the lower part of the secondary packed tower 2 has a light phase inlet 21. The bottom of the primary plate tower 1 is provided with a first heavy phase outlet 12 and a first light phase inlet 13. The top of the secondary packed tower 2 is provided with a first heavy phase inlet 27 and a first light phase outlet 28. The first heavy phase outlet 12 and the first heavy phase inlet 27 are connected, and the first light phase inlet 13 and the first light phase outlet 28 are connected. The top of the primary plate tower 1 has a second light phase outlet 14, and the bottom of the secondary packed tower 2 has a second heavy phase outlet 29.

[0094] The packing section 22 of the secondary packed tower 2 includes 32 cylindrical packing discs. Each packing disc is formed by stacking corrugated packing sheets 23 of different lengths horizontally. The lengths of the corrugated packing sheets 23 gradually decrease from the center along the radius of the cylindrical packing disc. The crests 24 and troughs 25 of adjacent corrugated packing sheets 23 overlap to form multiple parallel oblique quadrangular prism channels 26. The inclination angle α of the oblique quadrangular prism channels 26 is 40°. The multiple oblique quadrangular prism channels between adjacent packing discs... 26 correspond one-to-one in the vertical direction, and the corresponding oblique quadrangular prism channels 26 intersect each other; the height of the packing section 22 is 3.2m; the height of each packing disc is 100mm; the peak height h of each corrugated packing sheet 23 is 5mm, the peak width d is 6mm, the thickness is 1mm, and the included angle β between the two corrugations of each corrugated packing sheet 23 is 15°; the corrugated packing sheet 23 is a plate mesh corrugated packing sheet, wherein the wire diameter of the plate mesh is 0.4mm, the mesh opening is square, and the mesh area is 5x5mm. 2 .

[0095] Hydrogen peroxide extraction methods include:

[0096] Water is introduced from the heavy phase inlet 11, and anthraquinone working solution is introduced from the light phase inlet 21. The anthraquinone working solution and water are in countercurrent contact in the primary plate column 1 and the secondary packed column 2. The hydrogen peroxide aqueous solution obtained from the countercurrent contact of the anthraquinone working solution and water in the primary plate column 1 is drawn out from the first heavy phase outlet 12, and then enters the secondary packed column 2 from the first heavy phase inlet 27 to have countercurrent contact with the anthraquinone working solution. The anthraquinone working solution after the countercurrent contact of the anthraquinone working solution and the hydrogen peroxide aqueous solution in the secondary packed column 2 is drawn out from the first light phase outlet 28, and then enters the primary plate column 1 from the first light phase inlet 13 to have countercurrent contact with the hydrogen peroxide aqueous solution.

[0097] The countercurrent contact conditions in the primary plate tower 1 include: a temperature of 54°C and a pressure of atmospheric pressure; the countercurrent contact conditions in the secondary packed tower 2 include: a temperature of 54°C and a pressure of atmospheric pressure; a hydrogen peroxide concentration of 10.80 g / L in the anthraquinone working solution; and a water volume of 20 m³ introduced from the heavy phase feed inlet 11. 3 / h, the volume of anthraquinone working solution introduced from the light phase inlet 21 is 800m³. 3 / h, the volume ratio of water to anthraquinone working solution is 1:40.

[0098] After extraction, the hydrogen peroxide concentration obtained from the second heavy phase outlet 29 at the bottom of the secondary packed tower 2 is 46.3 wt%, and the residual hydrogen peroxide content in the raffinate drawn from the second light phase outlet 14 at the top of the primary plate tower 1 is 0.08 g / L.

[0099] Example 4

[0100] Example 4 was carried out in the following hydrogen peroxide extraction system, such as... Figure 1-3 As shown:

[0101] The system includes a primary plate tower 1 and a secondary packed tower 2. The primary plate tower 1 is a sieve plate tower with a theoretical number of 18 plates. The opening diameter on the surface of the sieve plate is Ф2.2mm, and the opening rate is 14%.

[0102] The bottom of the primary plate tower 1 and the top of the secondary packed tower 2 are interconnected. The upper part of the primary plate tower 1 has a heavy phase inlet 11, and the lower part of the secondary packed tower 2 has a light phase inlet 21. The bottom of the primary plate tower 1 is provided with a first heavy phase outlet 12 and a first light phase inlet 13. The top of the secondary packed tower 2 is provided with a first heavy phase inlet 27 and a first light phase outlet 28. The first heavy phase outlet 12 and the first heavy phase inlet 27 are connected, and the first light phase inlet 13 and the first light phase outlet 28 are connected. The top of the primary plate tower 1 has a second light phase outlet 14, and the bottom of the secondary packed tower 2 has a second heavy phase outlet 29.

[0103] The packing section 22 of the secondary packed tower 2 includes 36 cylindrical packing discs. Each packing disc is formed by stacking corrugated packing sheets 23 of different lengths horizontally. The lengths of the corrugated packing sheets 23 gradually decrease from the center along the radius of the cylindrical packing disc. The crests 24 and troughs 25 of adjacent corrugated packing sheets 23 overlap to form multiple parallel oblique quadrangular prism channels 26. The inclination angle α of the oblique quadrangular prism channels 26 is 40°. The multiple oblique quadrangular prism channels between adjacent packing discs... 26 correspond one-to-one in the vertical direction, and the corresponding oblique quadrangular prism channels 26 intersect each other; the height of the packing section 22 is 3.6m; the height of each packing disc is 100mm; the peak height h of each corrugated packing sheet 23 is 5mm, the peak width d is 6mm, the thickness is 1mm, and the included angle β between the two corrugations of each corrugated packing sheet 23 is 35°; the corrugated packing sheet 23 is a plate mesh corrugated packing sheet, wherein the wire diameter of the plate mesh is 0.4mm, the mesh opening is square, and the mesh area is 5x5mm. 2 .

[0104] Hydrogen peroxide extraction methods include:

[0105] Water is introduced from the heavy phase inlet 11, and anthraquinone working solution is introduced from the light phase inlet 21. The anthraquinone working solution and water are in countercurrent contact in the primary plate column 1 and the secondary packed column 2. The hydrogen peroxide aqueous solution obtained from the countercurrent contact of the anthraquinone working solution and water in the primary plate column 1 is drawn out from the first heavy phase outlet 12, and then enters the secondary packed column 2 from the first heavy phase inlet 27 to have countercurrent contact with the anthraquinone working solution. The anthraquinone working solution after the countercurrent contact of the anthraquinone working solution and the hydrogen peroxide aqueous solution in the secondary packed column 2 is drawn out from the first light phase outlet 28, and then enters the primary plate column 1 from the first light phase inlet 13 to have countercurrent contact with the hydrogen peroxide aqueous solution.

[0106] The countercurrent contact conditions in the primary plate tower 1 include: a temperature of 55°C and a pressure of atmospheric pressure; the countercurrent contact conditions in the secondary packed tower 2 include: a temperature of 55°C and a pressure of atmospheric pressure; a hydrogen peroxide concentration of 10.80 g / L in the anthraquinone working solution; and a water volume of 20 m³ introduced from the heavy phase feed inlet 11. 3 / h, the volume of anthraquinone working solution introduced from the light phase inlet 21 is 1000m³. 3 / h, the volume ratio of water to anthraquinone working solution is 1:50.

[0107] After extraction, the hydrogen peroxide concentration obtained from the second heavy phase outlet 29 at the bottom of the secondary packed tower 2 is 48.7 wt%, and the residual hydrogen peroxide content in the raffinate drawn from the second light phase outlet 14 at the top of the primary plate tower 1 is 0.08 g / L.

[0108] Example 5

[0109] Example 5 was carried out in the following hydrogen peroxide extraction system, such as... Figure 1-3 As shown:

[0110] The system includes a primary plate tower 1 and a secondary packed tower 2. The primary plate tower 1 is a sieve plate tower with a theoretical number of 20 plates. The opening diameter on the surface of the sieve plate is Ф2.2mm, and the opening ratio is 14%.

[0111] The bottom of the primary plate tower 1 and the top of the secondary packed tower 2 are interconnected. The upper part of the primary plate tower 1 has a heavy phase inlet 11, and the lower part of the secondary packed tower 2 has a light phase inlet 21. The bottom of the primary plate tower 1 is provided with a first heavy phase outlet 12 and a first light phase inlet 13. The top of the secondary packed tower 2 is provided with a first heavy phase inlet 27 and a first light phase outlet 28. The first heavy phase outlet 12 and the first heavy phase inlet 27 are connected, and the first light phase inlet 13 and the first light phase outlet 28 are connected. The top of the primary plate tower 1 has a second light phase outlet 14, and the bottom of the secondary packed tower 2 has a second heavy phase outlet 29.

[0112] The packing section 22 of the secondary packed tower 2 includes 40 cylindrical packing discs. Each packing disc is formed by stacking corrugated packing sheets 23 of different lengths horizontally. The lengths of the corrugated packing sheets 23 gradually decrease from the center along the radius of the cylindrical packing disc. The crests 24 and troughs 25 of adjacent corrugated packing sheets 23 overlap to form multiple parallel oblique quadrangular prism channels 26. The inclination angle α of the oblique quadrangular prism channels 26 is 40°. The multiple oblique quadrangular prism channels 26 between adjacent packing discs... The channels 26 are vertically aligned and intersect each other; the height of the packing section 22 is 4m; the height of each packing disc is 100mm; the peak height h of each corrugated packing sheet 23 is 5mm, the peak width d is 6mm, the thickness is 1mm, and the included angle β between the two corrugations of each corrugated packing sheet 23 is 45°; the corrugated packing sheet 23 is a plate mesh corrugated packing sheet, wherein the wire diameter of the plate mesh is 0.4mm, the mesh opening is square, and the mesh area is 5x5mm. 2 .

[0113] Hydrogen peroxide extraction methods include:

[0114] Water is introduced from the heavy phase inlet 11, and anthraquinone working solution is introduced from the light phase inlet 21. The anthraquinone working solution and water are in countercurrent contact in the primary plate column 1 and the secondary packed column 2. The hydrogen peroxide aqueous solution obtained from the countercurrent contact of the anthraquinone working solution and water in the primary plate column 1 is drawn out from the first heavy phase outlet 12, and then enters the secondary packed column 2 from the first heavy phase inlet 27 to have countercurrent contact with the anthraquinone working solution. The anthraquinone working solution after the countercurrent contact of the anthraquinone working solution and the hydrogen peroxide aqueous solution in the secondary packed column 2 is drawn out from the first light phase outlet 28, and then enters the primary plate column 1 from the first light phase inlet 13 to have countercurrent contact with the hydrogen peroxide aqueous solution.

[0115] The countercurrent contact conditions in the primary plate tower 1 include: a temperature of 50°C and a pressure of atmospheric pressure; the countercurrent contact conditions in the secondary packed tower 2 include: a temperature of 50°C and a pressure of atmospheric pressure; a hydrogen peroxide concentration of 10.80 g / L in the anthraquinone working solution; and a water volume of 20 m³ introduced from the heavy phase feed inlet 11. 3 / h, the volume of anthraquinone working solution introduced from the light phase inlet 21 is 1300m³. 3 / h, the volume ratio of water to anthraquinone working solution is 1:65.

[0116] After extraction, the hydrogen peroxide concentration obtained from the second heavy phase outlet 29 at the bottom of the secondary packed tower 2 is 53.6 wt%, and the residual hydrogen peroxide content in the raffinate drawn from the second light phase outlet 14 at the top of the primary plate tower 1 is 0.07 g / L.

[0117] Example 6

[0118] Example 6 was carried out in the following hydrogen peroxide extraction system, such as... Figure 1-3 As shown:

[0119] The system includes a primary plate tower 1 and a secondary packed tower 2. The primary plate tower 1 is a sieve plate tower with a theoretical number of 22 plates. The opening diameter on the surface of the sieve plate is Ф2.2mm, and the opening rate is 14%.

[0120] The bottom of the primary plate tower 1 and the top of the secondary packed tower 2 are interconnected. The upper part of the primary plate tower 1 has a heavy phase inlet 11, and the lower part of the secondary packed tower 2 has a light phase inlet 21. The bottom of the primary plate tower 1 is provided with a first heavy phase outlet 12 and a first light phase inlet 13. The top of the secondary packed tower 2 is provided with a first heavy phase inlet 27 and a first light phase outlet 28. The first heavy phase outlet 12 and the first heavy phase inlet 27 are connected, and the first light phase inlet 13 and the first light phase outlet 28 are connected. The top of the primary plate tower 1 has a second light phase outlet 14, and the bottom of the secondary packed tower 2 has a second heavy phase outlet 29.

[0121] The packing section 22 of the secondary packed tower 2 includes 44 cylindrical packing discs. Each packing disc is formed by stacking corrugated packing sheets 23 of different lengths horizontally. The lengths of the corrugated packing sheets 23 gradually decrease from the center along the radius of the cylindrical packing disc. The crests 24 and troughs 25 of adjacent corrugated packing sheets 23 overlap to form multiple parallel oblique quadrangular prism channels 26. The inclination angle α of the oblique quadrangular prism channels 26 is 40°. The multiple oblique quadrangular prism channels between adjacent packing discs... 26 correspond one-to-one in the vertical direction, and the corresponding oblique quadrangular prism channels 26 intersect each other; the height of the packing section 22 is 4.4m; the height of each packing disc is 100mm; the peak height h of each corrugated packing sheet 23 is 5mm, the peak width d is 6mm, the thickness is 1mm, and the included angle β between the two corrugations of each corrugated packing sheet 23 is 45°; the corrugated packing sheet 23 is a plate mesh corrugated packing sheet, wherein the wire diameter of the plate mesh is 0.4mm, the mesh opening is square, and the mesh area is 5x5mm. 2 .

[0122] Hydrogen peroxide extraction methods include:

[0123] Water is introduced from the heavy phase inlet 11, and anthraquinone working solution is introduced from the light phase inlet 21. The anthraquinone working solution and water are in countercurrent contact in the primary plate column 1 and the secondary packed column 2. The hydrogen peroxide aqueous solution obtained from the countercurrent contact of the anthraquinone working solution and water in the primary plate column 1 is drawn out from the first heavy phase outlet 12, and then enters the secondary packed column 2 from the first heavy phase inlet 27 to have countercurrent contact with the anthraquinone working solution. The anthraquinone working solution after the countercurrent contact of the anthraquinone working solution and the hydrogen peroxide aqueous solution in the secondary packed column 2 is drawn out from the first light phase outlet 28, and then enters the primary plate column 1 from the first light phase inlet 13 to have countercurrent contact with the hydrogen peroxide aqueous solution.

[0124] The countercurrent contact conditions in the primary plate tower 1 include: a temperature of 51°C and a pressure of atmospheric pressure; the countercurrent contact conditions in the secondary packed tower 2 include: a temperature of 51°C and a pressure of atmospheric pressure; a hydrogen peroxide concentration of 10.80 g / L in the anthraquinone working solution; and a water volume of 20 m³ introduced from the heavy phase feed inlet 11. 3 / h, the volume of anthraquinone working solution introduced from the light phase inlet 21 is 1400m³. 3 / h, the volume ratio of water to anthraquinone working solution is 1:70.

[0125] After extraction, the hydrogen peroxide concentration obtained from the second heavy phase outlet 29 at the bottom of the secondary packed tower 2 is 55.2 wt%, and the residual hydrogen peroxide content in the raffinate drawn from the second light phase outlet 14 at the top of the primary plate tower 1 is 0.07 g / L.

[0126] Example 7

[0127] Example 7 was carried out in the following hydrogen peroxide extraction system, such as... Figure 1-3 As shown:

[0128] The system includes a primary plate tower 1 and a secondary packed tower 2. The primary plate tower 1 is a sieve plate tower with a theoretical number of 24 plates. The opening diameter on the surface of the sieve plate is Ф2.2mm, and the opening rate is 14%.

[0129] The bottom of the primary plate tower 1 and the top of the secondary packed tower 2 are interconnected. The upper part of the primary plate tower 1 has a heavy phase inlet 11, and the lower part of the secondary packed tower 2 has a light phase inlet 21. The bottom of the primary plate tower 1 is provided with a first heavy phase outlet 12 and a first light phase inlet 13. The top of the secondary packed tower 2 is provided with a first heavy phase inlet 27 and a first light phase outlet 28. The first heavy phase outlet 12 and the first heavy phase inlet 27 are connected, and the first light phase inlet 13 and the first light phase outlet 28 are connected. The top of the primary plate tower 1 has a second light phase outlet 14, and the bottom of the secondary packed tower 2 has a second heavy phase outlet 29.

[0130] The packing section 22 of the secondary packed tower 2 includes 48 cylindrical packing discs. Each packing disc is formed by stacking corrugated packing sheets 23 of different lengths horizontally. The lengths of the corrugated packing sheets 23 gradually decrease from the center along the radius of the cylindrical packing disc. The crests 24 and troughs 25 of adjacent corrugated packing sheets 23 overlap to form multiple parallel oblique quadrangular prism channels 26. The inclination angle α of the oblique quadrangular prism channels 26 is 40°. The multiple oblique quadrangular prism channels between adjacent packing discs... 26 correspond one-to-one in the vertical direction, and the corresponding oblique quadrangular prism channels 26 intersect each other; the height of the packing section 22 is 4.8m; the height of each packing disc is 100mm; the peak height h of each corrugated packing sheet 23 is 5mm, the peak width d is 6mm, the thickness is 1mm, and the included angle β between the two corrugations of each corrugated packing sheet 23 is 75°; the corrugated packing sheet 23 is a plate mesh corrugated packing sheet, wherein the wire diameter of the plate mesh is 0.4mm, the mesh opening is square, and the mesh area is 5x5mm. 2 .

[0131] Hydrogen peroxide extraction methods include:

[0132] Water is introduced from the heavy phase inlet 11, and anthraquinone working solution is introduced from the light phase inlet 21. The anthraquinone working solution and water are in countercurrent contact in the primary plate column 1 and the secondary packed column 2. The hydrogen peroxide aqueous solution obtained from the countercurrent contact of the anthraquinone working solution and water in the primary plate column 1 is drawn out from the first heavy phase outlet 12, and then enters the secondary packed column 2 from the first heavy phase inlet 27 to have countercurrent contact with the anthraquinone working solution. The anthraquinone working solution after the countercurrent contact of the anthraquinone working solution and the hydrogen peroxide aqueous solution in the secondary packed column 2 is drawn out from the first light phase outlet 28, and then enters the primary plate column 1 from the first light phase inlet 13 to have countercurrent contact with the hydrogen peroxide aqueous solution.

[0133] The countercurrent contact conditions in the primary plate tower 1 include: a temperature of 53°C and a pressure of atmospheric pressure; the countercurrent contact conditions in the secondary packed tower 2 include: a temperature of 53°C and a pressure of atmospheric pressure; a hydrogen peroxide concentration of 10.80 g / L in the anthraquinone working solution; and a water volume of 20 m³ introduced from the heavy phase feed inlet 11. 3 / h, the volume of anthraquinone working solution introduced from the light phase inlet 21 is 1300m³. 3 / h, the volume ratio of water to anthraquinone working solution is 1:65.

[0134] After extraction, the hydrogen peroxide concentration obtained from the second heavy phase outlet 29 at the bottom of the secondary packed tower 2 is 54.2 wt%, and the residual hydrogen peroxide content in the raffinate drawn from the second light phase outlet 14 at the top of the primary plate tower 1 is 0.07 g / L.

[0135] Example 8

[0136] Example 8 was carried out in the following hydrogen peroxide extraction system, such as... Figure 1-3 As shown:

[0137] The system includes a primary plate tower 1 and a secondary packed tower 2. The primary plate tower 1 is a sieve plate tower with a theoretical number of 26 plates. The opening diameter on the surface of the sieve plate is Ф2.2mm, and the opening rate is 14%.

[0138] The bottom of the primary plate tower 1 and the top of the secondary packed tower 2 are interconnected. The upper part of the primary plate tower 1 has a heavy phase inlet 11, and the lower part of the secondary packed tower 2 has a light phase inlet 21. The bottom of the primary plate tower 1 is provided with a first heavy phase outlet 12 and a first light phase inlet 13. The top of the secondary packed tower 2 is provided with a first heavy phase inlet 27 and a first light phase outlet 28. The first heavy phase outlet 12 and the first heavy phase inlet 27 are connected, and the first light phase inlet 13 and the first light phase outlet 28 are connected. The top of the primary plate tower 1 has a second light phase outlet 14, and the bottom of the secondary packed tower 2 has a second heavy phase outlet 29.

[0139] The packing section 22 of the secondary packed tower 2 includes 52 cylindrical packing discs. Each packing disc is formed by stacking corrugated packing sheets 23 of different lengths horizontally. The lengths of the corrugated packing sheets 23 gradually decrease from the center along the radius of the cylindrical packing disc. The crests 24 and troughs 25 of adjacent corrugated packing sheets 23 overlap to form multiple parallel oblique quadrangular prism channels 26. The inclination angle α of the oblique quadrangular prism channels 26 is 40°. The multiple oblique quadrangular prisms of adjacent packing discs... The channels 26 correspond one-to-one in the vertical direction, and the corresponding oblique quadrangular prism channels 26 intersect each other; the height of the packing section 22 is 5.2m; the height of each packing disc is 100mm; the peak height h of each corrugated packing sheet 23 is 5mm, the peak width d is 6mm, the thickness is 1mm, and the included angle β between the two corrugations of each corrugated packing sheet 31 is 75°; the corrugated packing sheet 23 is a plate mesh corrugated packing sheet, wherein the wire diameter of the plate mesh is 0.4mm, the mesh opening is square, and the mesh area is 5x5mm. 2 .

[0140] Hydrogen peroxide extraction methods include:

[0141] Water is introduced from the heavy phase inlet 11, and anthraquinone working solution is introduced from the light phase inlet 21. The anthraquinone working solution and water are in countercurrent contact in the primary plate column 1 and the secondary packed column 2. The hydrogen peroxide aqueous solution obtained from the countercurrent contact of the anthraquinone working solution and water in the primary plate column 1 is drawn out from the first heavy phase outlet 12, and then enters the secondary packed column 2 from the first heavy phase inlet 27 to have countercurrent contact with the anthraquinone working solution. The anthraquinone working solution after the countercurrent contact of the anthraquinone working solution and the hydrogen peroxide aqueous solution in the secondary packed column 2 is drawn out from the first light phase outlet 28, and then enters the primary plate column 1 from the first light phase inlet 13 to have countercurrent contact with the hydrogen peroxide aqueous solution.

[0142] The countercurrent contact conditions in the primary plate tower 1 include: a temperature of 53°C and a pressure of atmospheric pressure; the countercurrent contact conditions in the secondary packed tower 2 include: a temperature of 53°C and a pressure of atmospheric pressure; a hydrogen peroxide concentration of 10.80 g / L in the anthraquinone working solution; and a water volume of 20 m³ introduced from the heavy phase feed inlet 11. 3 / h, the volume of anthraquinone working solution introduced from the light phase inlet 21 is 1400m³. 3 / h, the volume ratio of water to anthraquinone working solution is 1:70.

[0143] After extraction, the hydrogen peroxide concentration obtained from the second heavy phase outlet 29 at the bottom of the secondary packed tower 2 is 58.3 wt%, and the residual hydrogen peroxide content in the raffinate drawn from the second light phase outlet 14 at the top of the primary plate tower 1 is 0.05 g / L.

[0144] Example 9

[0145] Example 9 was carried out in the following hydrogen peroxide extraction system, such as... Figure 1-3 As shown:

[0146] The system includes a primary plate tower 1 and a secondary packed tower 2. The primary plate tower 1 is a sieve plate tower with a theoretical number of 28 plates. The opening diameter on the surface of the sieve plate is Ф2.2mm, and the opening ratio is 14%.

[0147] The bottom of the primary plate tower 1 and the top of the secondary packed tower 2 are interconnected. The upper part of the primary plate tower 1 has a heavy phase inlet 11, and the lower part of the secondary packed tower 2 has a light phase inlet 21. The bottom of the primary plate tower 1 is provided with a first heavy phase outlet 12 and a first light phase inlet 13. The top of the secondary packed tower 2 is provided with a first heavy phase inlet 27 and a first light phase outlet 28. The first heavy phase outlet 12 and the first heavy phase inlet 27 are connected, and the first light phase inlet 13 and the first light phase outlet 28 are connected. The top of the primary plate tower 1 has a second light phase outlet 14, and the bottom of the secondary packed tower 2 has a second heavy phase outlet 29.

[0148] The packing section 22 of the secondary packed tower 2 includes 56 cylindrical packing discs. Each packing disc is formed by stacking corrugated packing sheets 23 of different lengths horizontally. The lengths of the corrugated packing sheets 23 gradually decrease from the center along the radius of the cylindrical packing disc. The crests 24 and troughs 25 of adjacent corrugated packing sheets 23 overlap to form multiple parallel oblique quadrangular prism channels 26. The inclination angle α of the oblique quadrangular prism channels 26 is 40°. The multiple oblique quadrangular prism channels between adjacent packing discs... 26 correspond one-to-one in the vertical direction, and the corresponding oblique quadrangular prism channels 26 intersect each other; the height of the packing section 22 is 5.6m; the height of each packing disc is 100mm; the peak height h of each corrugated packing sheet 23 is 5mm, the peak width d is 6mm, the thickness is 1mm, and the included angle β between the two corrugations of each corrugated packing sheet 23 is 85°; the corrugated packing sheet 23 is a plate mesh corrugated packing sheet, wherein the wire diameter of the plate mesh is 0.4mm, the mesh opening is square, and the mesh area is 5x5mm. 2 .

[0149] Hydrogen peroxide extraction methods include:

[0150] Water is introduced from the heavy phase inlet 11, and anthraquinone working solution is introduced from the light phase inlet 21. The anthraquinone working solution and water are in countercurrent contact in the primary plate column 1 and the secondary packed column 2. The hydrogen peroxide aqueous solution obtained from the countercurrent contact of the anthraquinone working solution and water in the primary plate column 1 is drawn out from the first heavy phase outlet 12, and then enters the secondary packed column 2 from the first heavy phase inlet 27 to have countercurrent contact with the anthraquinone working solution. The anthraquinone working solution after the countercurrent contact of the anthraquinone working solution and the hydrogen peroxide aqueous solution in the secondary packed column 2 is drawn out from the first light phase outlet 28, and then enters the primary plate column 1 from the first light phase inlet 13 to have countercurrent contact with the hydrogen peroxide aqueous solution.

[0151] The countercurrent contact conditions in the primary plate tower 1 include: a temperature of 54°C and a pressure of atmospheric pressure; the countercurrent contact conditions in the secondary packed tower 2 include: a temperature of 54°C and a pressure of atmospheric pressure; a hydrogen peroxide concentration of 10.80 g / L in the anthraquinone working solution; and a water volume of 20 m³ introduced from the heavy phase feed inlet 11. 3 / h, the volume of anthraquinone working solution introduced from the light phase inlet 21 is 1400m³. 3 / h, the volume ratio of water to anthraquinone working solution is 1:70.

[0152] After extraction, the hydrogen peroxide concentration obtained from the second heavy phase outlet 29 at the bottom of the secondary packed tower 2 is 59.4 wt%, and the residual hydrogen peroxide content in the raffinate drawn from the second light phase outlet 14 at the top of the primary plate tower 1 is 0.05 g / L.

[0153] Example 10

[0154] Example 10 was carried out in the following hydrogen peroxide extraction system, such as... Figure 1-3 As shown:

[0155] The system includes a primary plate tower 1 and a secondary packed tower 2. The primary plate tower 1 is a sieve plate tower with a theoretical number of 30 plates. The opening diameter on the surface of the sieve plate is Ф2.2mm, and the opening ratio is 14%.

[0156] The bottom of the primary plate tower 1 and the top of the secondary packed tower 2 are interconnected. The upper part of the primary plate tower 1 has a heavy phase inlet 11, and the lower part of the secondary packed tower 2 has a light phase inlet 21. The bottom of the primary plate tower 1 is provided with a first heavy phase outlet 12 and a first light phase inlet 13. The top of the secondary packed tower 2 is provided with a first heavy phase inlet 27 and a first light phase outlet 28. The first heavy phase outlet 12 and the first heavy phase inlet 27 are connected, and the first light phase inlet 13 and the first light phase outlet 28 are connected. The top of the primary plate tower 1 has a second light phase outlet 14, and the bottom of the secondary packed tower 2 has a second heavy phase outlet 29.

[0157] The packing section 22 of the secondary packed tower 2 includes 60 cylindrical packing discs. Each packing disc is formed by stacking corrugated packing sheets 23 of different lengths horizontally. The lengths of the corrugated packing sheets 23 gradually decrease from the center along the radius of the cylindrical packing disc. The crests 24 and troughs 25 of adjacent corrugated packing sheets 23 overlap to form multiple parallel oblique quadrangular prism channels 26. The inclination angle α of the oblique quadrangular prism channels 26 is 40°. The multiple oblique quadrangular prism channels 26 between adjacent packing discs... The channels 26 are vertically aligned and intersect each other; the height of the packing section 22 is 6m; the height of each packing disc is 100mm; the peak height h of each corrugated packing sheet 23 is 5mm, the peak width d is 6mm, the thickness is 1mm, and the included angle β between the two corrugations of each corrugated packing sheet 23 is 85°; the corrugated packing sheet 23 is a plate mesh corrugated packing sheet, wherein the wire diameter of the plate mesh is 0.4mm, the mesh opening is square, and the mesh area is 5x5mm. 2 .

[0158] Hydrogen peroxide extraction methods include:

[0159] Water is introduced from the heavy phase inlet 11, and anthraquinone working solution is introduced from the light phase inlet 21. The anthraquinone working solution and water are in countercurrent contact in the primary plate column 1 and the secondary packed column 2. The hydrogen peroxide aqueous solution obtained from the countercurrent contact of the anthraquinone working solution and water in the primary plate column 1 is drawn out from the first heavy phase outlet 12, and then enters the secondary packed column 2 from the first heavy phase inlet 27 to have countercurrent contact with the anthraquinone working solution. The anthraquinone working solution after the countercurrent contact of the anthraquinone working solution and the hydrogen peroxide aqueous solution in the secondary packed column 2 is drawn out from the first light phase outlet 28, and then enters the primary plate column 1 from the first light phase inlet 13 to have countercurrent contact with the hydrogen peroxide aqueous solution.

[0160] The countercurrent contact conditions in the primary plate tower 1 include: a temperature of 51°C and a pressure of atmospheric pressure; the countercurrent contact conditions in the secondary packed tower 2 include: a temperature of 51°C and a pressure of atmospheric pressure; a hydrogen peroxide concentration of 10.80 g / L in the anthraquinone working solution; and a water volume of 20 m³ introduced from the heavy phase feed inlet 11. 3 / h, the volume of anthraquinone working solution introduced from the light phase inlet 21 is 1400m³. 3 / h, the volume ratio of water to anthraquinone working solution is 1:70.

[0161] After extraction, the hydrogen peroxide concentration obtained from the second heavy phase outlet 29 at the bottom of the secondary packed tower 2 is 60.4 wt%, and the residual hydrogen peroxide content in the raffinate drawn from the second light phase outlet 14 at the top of the primary plate tower 1 is 0.05 g / L.

[0162] Comparative Example

[0163] Extraction was performed using a conventional plate column with 60 plates, a height of 35 meters, a temperature of 51°C, and atmospheric pressure. The volume of water introduced from the top of the column was 20 m³. 3 / h, the volume of anthraquinone working solution introduced from the bottom of the column is 880m³. 3 / h, the volume ratio of water to anthraquinone working solution is 1:44, and the hydrogen peroxide concentration in the anthraquinone working solution is 10.80 g / L.

[0164] After extraction, the concentration of hydrogen peroxide obtained from the bottom of the column was 35.4 wt%, and the residual hydrogen peroxide content in the raffinate drawn from the bottom of the column was 0.11 g / L.

[0165] As can be seen from the examples and comparative examples, the hydrogen peroxide concentration obtained by extracting hydrogen peroxide from the anthraquinone working solution using the system and method described in this invention is greater than 44%, and the extraction efficiency is high. At the same time, it eliminates the risk of explosion when high-concentration hydrogen peroxide aqueous solution comes into contact with the anthraquinone working solution during the extraction process.

[0166] The preferred embodiments of the present invention have been described in detail above; however, the present invention is not limited thereto. Within the scope of the inventive concept, various simple modifications can be made to the technical solutions of the present invention, including combinations of various technical features in any other suitable manner. These simple modifications and combinations should also be considered as the content disclosed in the present invention and are all within the protection scope of the present invention.

Claims

1. A hydrogen peroxide extraction system, characterized in that, The system includes a primary plate tower (1) and a secondary packed tower (2). The bottom of the primary plate tower (1) and the top of the secondary packed tower (2) are connected to each other. The upper part of the primary plate tower (1) has a heavy phase feed inlet (11), and the lower part of the secondary packed tower (2) has a light phase feed inlet (21). The packing section (22) of the secondary packed tower (2) includes several packing discs. Each packing disc is formed by multiple corrugated packing sheets (23) stacked in the horizontal direction. The crests (24) and troughs (25) of two adjacent corrugated packing sheets (23) are superimposed to form multiple parallel oblique quadrangular prism channels (26). The inclination angle α of the oblique quadrangular prism channels (26) is 20°~80°. Multiple oblique quadrangular prism channels (26) of two adjacent packing discs correspond one-to-one in the vertical direction, and the corresponding oblique quadrangular prism channels (26) intersect each other.

2. The system according to claim 1, characterized in that, The first-stage plate tower (1) is provided with a first heavy phase outlet (12) and a first light phase inlet (13) at the bottom of the tower, and the second-stage packed tower (2) is provided with a first heavy phase inlet (27) and a first light phase outlet (28) at the top of the tower. The first heavy phase outlet (12) and the first heavy phase inlet (27) are connected, and the first light phase inlet (13) and the first light phase outlet (28) are connected.

3. The system according to claim 2, characterized in that, The first-stage plate tower (1) has a second light phase outlet (14) at the top, and the second-stage packed tower (2) has a second heavy phase outlet (29) at the bottom.

4. The system according to claim 1, characterized in that, Each packing disc is cylindrical and is composed of multiple corrugated packing sheets (23) of different lengths stacked together. The length of the multiple corrugated packing sheets (23) gradually decreases from the center along the radius of the cylindrical packing disc.

5. The system according to claim 1, characterized in that, The height of the packing section (22) is 2~6m; the height of each packing disc is 30~500mm.

6. The system according to claim 5, characterized in that, The height of the packing section (22) is 3~5m.

7. The system according to claim 5, characterized in that, The height of each packing disc is 50~200mm.

8. The system according to claim 1, characterized in that, Each corrugated packing sheet (23) has a peak height h of 2~6mm, a peak width d of 3~10mm, and a thickness of 0.5~3mm.

9. The system according to claim 1, characterized in that, The included angle β between the two corrugations of the corrugated packing sheet (23) is 15-85°.

10. The system according to claim 1, characterized in that, The corrugated packing sheet (23) is a plate mesh corrugated packing sheet, wherein the wire diameter of the plate mesh is 0.1~4mm.

11. The system according to claim 10, characterized in that, The mesh shape of the plate mesh is square, rectangular, or rhomboid, and the mesh area is (3~20) x (3~20) mm. 2 .

12. The system according to claim 1, characterized in that, The first-stage plate tower (1) is a sieve plate tower with a theoretical number of 10 to 30 plates.

13. A method for hydrogen peroxide extraction, characterized in that, The method is implemented in the system of any one of claims 1-12, and the method includes: introducing water from the heavy phase feed inlet (11), introducing anthraquinone working liquid from the light phase feed inlet (21), and having the anthraquinone working liquid and water in countercurrent contact in the primary plate tower (1) and the secondary packed tower (2).

14. The method according to claim 13, characterized in that, The hydrogen peroxide aqueous solution obtained by the countercurrent contact of anthraquinone working solution and water in the first-stage plate tower (1) is drawn out from the first heavy phase outlet (12) and then enters the second-stage packed tower (2) from the first heavy phase inlet (27) to have countercurrent contact with the anthraquinone working solution; The anthraquinone working solution, after being countercurrently contacted with the hydrogen peroxide aqueous solution in the secondary packed tower (2), is drawn out from the first light phase outlet (28) and then enters the primary plate tower (1) from the first light phase inlet (13) to countercurrently contact with the hydrogen peroxide aqueous solution.

15. The method according to claim 13 or 14, characterized in that, The countercurrent contact conditions in the first-stage plate tower (1) include: a temperature of 50~55℃ and a pressure of atmospheric pressure.

16. The method according to claim 13, characterized in that, The countercurrent contact conditions in the secondary packed tower (2) include: a temperature of 50~55℃ and a pressure of atmospheric pressure.

17. The method according to claim 13, characterized in that, The hydrogen peroxide concentration in the anthraquinone working solution is 6~20 g / L.

18. The method according to claim 13, characterized in that, The volume ratio of water introduced from the heavy phase inlet (11) to anthraquinone working solution introduced from the light phase inlet (21) is 1:30~70.

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