A hydrogen peroxide staged extraction column and method

Abstract

The present application relates to hydrogen peroxide extraction technical field, disclose a kind of hydrogen peroxide subsection extraction tower and method.The hydrogen peroxide subsection extraction tower includes tower body, the tower body is sequentially provided with plate column section and filler column section from top to bottom, the upper portion of the plate column section has water phase entrance, the lower portion of the filler column section has anthraquinone working fluid entrance;The filler column section includes several filler trays, each filler tray is stacked by multiple corrugated filler pieces along horizontal direction, and the wave crest and wave trough between adjacent two corrugated filler pieces 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 not only can 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, specifically to a hydrogen peroxide fractional extraction tower 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 tower that has explosion suppression and explosion 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 staged hydrogen peroxide extraction tower and method. This staged hydrogen peroxide extraction tower and 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 aqueous solution contacting the anthraquinone working solution during the extraction process.

[0009] To achieve the above objectives, the present invention provides a hydrogen peroxide segmented extraction tower, which includes a tower body, wherein a plate tower section and a packed tower section are arranged sequentially from top to bottom. The upper part of the plate tower section has an aqueous phase inlet, and the lower part of the packed tower section has an anthraquinone working solution inlet.

[0010] The packed tower section includes several packing discs, each of which 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 hydrogen peroxide fractional extraction tower has a working liquid outlet at the top and an aqueous phase outlet at the bottom.

[0012] Preferably, in the packed tower section, 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.

[0013] 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.

[0014] Preferably, the height of the packing layer in the packed tower section is 2 to 6 m, and more preferably 3 to 5 m.

[0015] Preferably, the height of each packing disc is 30–500 mm, more preferably 50–200 mm.

[0016] Preferably, the peak height h of each corrugated packing sheet is 2 to 12 mm, the peak width d is 3 to 30 mm, and the thickness is 0.5 mm to 3 mm.

[0017] Preferably, the included angle β between the two corrugations of the corrugated packing sheet 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 plate tower section is a sieve plate tower with a theoretical number of 10 to 40 plates.

[0021] A second aspect of the present invention provides a hydrogen peroxide extraction method, which is carried out in the hydrogen peroxide segmented extraction tower described in the first aspect above. The method includes: introducing water from the aqueous phase inlet, introducing anthraquinone working solution from the anthraquinone working solution inlet, and having the anthraquinone working solution and water in countercurrent contact in the plate tower section and the packed tower section.

[0022] Preferably, the countercurrent contact conditions in the plate tower section include: a temperature of 50–55°C and a pressure of atmospheric pressure.

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

[0024] Preferably, the hydrogen peroxide concentration in the anthraquinone working solution is 6–20 g / L.

[0025] Preferably, the volume ratio of water introduced from the aqueous phase inlet to anthraquinone working solution introduced from the anthraquinone working solution inlet is 1:30 to 70.

[0026] Compared with the prior art, the present invention has at least the following advantages:

[0027] (1) The present invention divides the extraction tower into two sections, namely a plate tower section and a packed tower section. The high concentration area with explosion risk is carried out in the packed tower section, and the low concentration area without explosion risk is carried out in the plate tower section, thereby isolating the high concentration area with explosion risk from the low concentration area without explosion risk, reducing the amount of material affected by explosion, and eliminating the explosion risk of high concentration hydrogen peroxide aqueous solution coming into contact with anthraquinone working solution during the extraction process.

[0028] (2) The structure of the structured packing layer in the packed tower section has a cutting and breaking effect on the droplets, reducing the diameter of the anthraquinone working solution droplets, increasing the mass transfer area between the two phases, enhancing the mass transfer process, improving extraction efficiency, and thus reducing the height of the mass transfer unit and 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 hydrogen peroxide segmented extraction tower and method described in this invention is significantly higher than that of the traditional sieve plate extraction equipment and process.

[0029] (3) Using the hydrogen peroxide segmented extraction tower described in this invention, a hydrogen peroxide aqueous solution of more than 35 wt% can be directly extracted, and the maximum can reach 70 wt%, thereby eliminating the hydrogen peroxide concentration unit and reducing investment and energy consumption. Attached Figure Description

[0030] Figure 1 This is a schematic diagram of the hydrogen peroxide fractional extraction tower described in this invention;

[0031] Figure 2 This is a schematic diagram of the single corrugated packing sheet described in this invention;

[0032] Figure 3 This is a schematic diagram of the oblique quadrangular prism channel formed by the two corrugated packing sheets described in this invention;

[0033] Figure 4 This is a schematic diagram of the filling angle of the two packing discs.

[0034] Explanation of reference numerals in the attached figures

[0035] 1 Tower body; 2 Plate tower section; 3 Packed tower section; 4 Aqueous phase inlet; 5 Anthraquinone working liquid inlet; 6 Working liquid outlet; 7 Aqueous phase outlet; 31 Corrugated packing sheet; 32 Corrugated crest; 33 Corrugated trough; 34 Inclined quadrangular prism channel. Detailed Implementation

[0036] 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.

[0037] 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.

[0038] The first aspect of this invention provides a hydrogen peroxide fractional extraction tower, such as... Figure 1 As shown, the hydrogen peroxide fractional extraction tower includes a tower body 1, which is provided with a plate tower section 2 and a packed tower section 3 from top to bottom. The upper part of the plate tower section 2 has an aqueous phase inlet 4, and the lower part of the packed tower section 3 has an anthraquinone working liquid inlet 5.

[0039] In this invention, water is used as the extractant, and anthraquinone working solution is used as the extracted substance. The hydrogen peroxide staged extraction tower of this invention includes a plate tower section 2 and a packed tower section 3. Water introduced from the aqueous phase inlet 4 and anthraquinone working solution introduced from the anthraquinone working solution inlet 5 are introduced in a countercurrent contact in the plate tower section 2 and the packed tower section 3 for extraction. Hydrogen peroxide in the anthraquinone working solution is extracted by the water. As the water flows downwards, more and more hydrogen peroxide is extracted, resulting in a higher concentration of the hydrogen peroxide aqueous solution. The plate tower section 2 and the packed tower section 3 respectively yield a low-concentration hydrogen peroxide aqueous solution and a high-concentration hydrogen peroxide aqueous solution, thus isolating 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. Simultaneously, the packing material in the packed tower section 3 is uniquely designed to provide explosion suppression and prevention functions, thereby preventing an explosion when the high-concentration hydrogen peroxide aqueous solution comes into contact with the anthraquinone working solution during the extraction process.

[0040] Specifically, the anthraquinone working solution is introduced from the anthraquinone working solution inlet 5 of the hydrogen peroxide segmented extraction tower, moves upward, and passes through the packed tower section 3 and the plate tower section 2 in sequence before reaching the top of the hydrogen peroxide segmented extraction tower; pure water is introduced from the upper part of the hydrogen peroxide segmented extraction tower through the aqueous phase inlet 4, flows downward, and passes through the plate tower section 2 and the packed tower section 3 in sequence before reaching the bottom of the hydrogen peroxide segmented extraction tower; in the plate tower section 2, during the flow process, water and the upward-moving anthraquinone working solution undergo extraction mass transfer and separation between the tower plates before reaching the next tower plate; in the packed tower section 3, water and the anthraquinone working solution undergo contact mass transfer between the packing materials, and after multiple countercurrent extractions in the tower, the anthraquinone working solution flows out from the top of the hydrogen peroxide segmented extraction tower, and the aqueous phase flows out from the bottom of the hydrogen peroxide segmented extraction tower.

[0041] The plate column section 2 is divided into a descaling residue section and an extraction mass transfer section. The uppermost plate of the plate column section 2 is the descaling residue section. In this area, the extractant phase is pure water, and the extractable phase is the anthraquinone working solution from the packed column section 3. The density difference between the anthraquinone working solution and the aqueous phase in this area is very close, resulting in a small mass transfer driving force and difficulty in mass transfer, requiring a large number of plates for descaling residue. The lower part of the plate column section 2 is the extraction mass transfer section. In this area, the extractant phase is a low-concentration hydrogen peroxide solution from the descaling residue section, and the extractable phase is the anthraquinone working solution from the packed column section 3. The density difference between the anthraquinone working solution and the aqueous phase in this area is greater than that in the descaling residue section, resulting in a greater mass transfer driving force. Extraction separation in this part can increase the hydrogen peroxide concentration of the extractant phase to about 30 wt%.

[0042] In this invention, the packed tower section 3 includes several packing discs, each of which is formed by stacking multiple corrugated packing sheets 31 horizontally. The crests 32 and troughs 33 of adjacent corrugated packing sheets 31 are superimposed to form multiple parallel oblique quadrangular prism channels 34. The inclination angle α of the oblique quadrangular prism channels 34 is 20–80°. In this text, the inclination angle α refers to an acute angle.

[0043] In the packed tower section 3, since there are oblique quadrangular prism channels 34 between adjacent corrugated packing sheets 31, 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 34; furthermore, limiting the peak height h of the corrugated packing sheet 31 to an appropriate range makes the equivalent diameter of the oblique quadrangular prism channel 34 smaller than the explosive critical diameter of the system, which is more conducive to achieving the effect of explosion prevention and suppression.

[0044] According to the present invention, the packed tower section 3 having the aforementioned packing structure is a hydrogen peroxide concentration section. In this region, the extraction 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 acquisition of a high-concentration hydrogen peroxide product of 35 wt% or more through enhanced extraction mass transfer. Furthermore, the packed tower section 3 of the present invention uses a structured packing with non-interconnected oblique quadrangular prisms, which can prevent the risk of combustion and explosion when 44 wt% or more of hydrogen peroxide is mixed with the anthraquinone working solution, thus providing explosion suppression and prevention functions.

[0045] According to the present invention, such as Figure 3 As shown, multiple corrugated packing sheets 31 are stacked at an angle to form multiple oblique quadrangular prism channels 34. For example... Figure 2 As shown, the horizontal plane where the wave crest 32 is located is at a higher level than the horizontal plane where the wave trough 33 is located.

[0046] In this invention, under preferred conditions, the oblique quadrangular prism channels 34 in the same packing disc are all the same shape, and the channel directions of the oblique quadrangular prism channels 34 formed by two adjacent corrugated packing sheets 31 are parallel to each other.

[0047] In a preferred embodiment, such as Figure 1As shown, the hydrogen peroxide segmented extraction tower has a working liquid outlet 6 at the top and an aqueous phase outlet 7 at the bottom. After the anthraquinone working liquid and water come into countercurrent contact in the plate column section 2 and the packed column section 3, the concentration of hydrogen peroxide in the extract phase increases as the aqueous phase flows from top to bottom in the plate column section 2 and the packed column section 3, and finally the extract phase flowing out of the aqueous phase outlet 7 has the highest concentration of hydrogen peroxide. Meanwhile, as the anthraquinone working liquid moves from bottom to top in the packed column section 3 and the plate column section 2, the hydrogen peroxide in the anthraquinone working liquid is continuously extracted by the aqueous phase and finally flows out from the working liquid outlet 6.

[0048] In this invention, the number of packing discs in the packing layer of the packed tower section 3 and the number of corrugated packing sheets 31 forming each packing disc are not limited and can be selected according to the actual height and inner diameter of the packed tower section 3.

[0049] In one specific embodiment, multiple oblique quadrangular prism channels 34 of two adjacent packing discs correspond one-to-one in the vertical direction, and the corresponding oblique quadrangular prism channels 34 intersect each other. The one-to-one correspondence of multiple oblique quadrangular prism channels 34 of two adjacent packing discs in the vertical direction allows the material streams of different channels to be extracted independently along their respective corresponding channels throughout the packing layer, avoiding cross-flow of material streams between different channels, which would affect the mass transfer process between the material streams and reduce the extraction efficiency. The intersecting arrangement of the oblique quadrangular prism channels 34 allows the liquid in each channel to be deflected during the flow process, which is beneficial to enhancing mass transfer.

[0050] 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 layer. Further, each packing disc is formed by stacking multiple corrugated packing sheets 31 of different lengths, and the length of the multiple corrugated packing sheets 31 gradually decreases from the center along the radial direction of the cylindrical packing disc. That is, the corrugated packing sheet 31 passing through the center of the cylindrical packing disc has the longest length, and the length of the corrugated packing sheets 31 extending from the center to the arc direction becomes shorter and shorter, thus forming a cylindrical shape.

[0051] In this invention, a plurality of packing discs are placed in the packing layer, and the number of packing discs is determined according to the height of the packing layer and the height of each packing disc.

[0052] In a preferred embodiment, the height of the packing layer 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 can be 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.

[0053] The packed tower section 3 of the present invention forms an oblique quadrangular prism channel 34 in the packed 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 34 is below the critical quenching diameter, thereby achieving the effect of explosion prevention and suppression, and realizing the inherent safety of the extraction process of the explosion system.

[0054] In some preferred embodiments, the peak height h of each corrugated packing sheet 31 can be 2 to 12 mm, preferably 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 30 mm, preferably 3 to 10 mm, for example 3 mm, 4 mm, 5 mm, 6 mm, 7 mm, 8 mm, 9 mm or 10 mm; the thickness l can be 0.5 mm to 3 mm, for example 0.5 mm, 1 mm, 1.5 mm, 2 mm, 2.5 mm or 3 mm.

[0055] In some preferred embodiments, the included angle β between the two corrugations of the corrugated packing sheet 31 can be 15-85°, preferably 15°, 30°, 45°, 60°, 75° or 85°.

[0056] According to the present invention, under preferred conditions, the corrugated packing sheet 31 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.

[0057] 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 .

[0058] In this invention, the plate column section 2 can be a conventional sieve tray column, wherein the trays are conventionally used trays. In specific embodiments, the number of trays in the plate column section 2 can be adjusted according to actual conditions. Under preferred conditions, the theoretical number of trays in the plate column section 2 can be 10 to 40 layers, preferably 10 to 30 layers, for example 10, 15, 20, 25, or 30 layers.

[0059] The second aspect of the present invention provides a hydrogen peroxide extraction method, which is carried out in the hydrogen peroxide segmented extraction tower described in the first aspect above. The method includes: introducing water from the aqueous phase inlet 4, introducing anthraquinone working solution from the anthraquinone working solution inlet 5, and having the anthraquinone working solution and water in countercurrent contact in the plate tower section 2 and the packed tower section 3.

[0060] In the method described in this invention, water, as both the extraction phase and the heavy phase, is introduced from the aqueous phase inlet 4 at the top of the plate column section 2, flows downwards in the plate column section 2, then flows out from the bottom of the plate column section 2, enters the packed column section 3 from the top, and flows downwards in the packed column section 3. Anthraquinone working solution, as the extracted phase, is introduced from the anthraquinone working solution inlet 5 at the bottom of the packed column section 3, flows upwards in the packed column section 3, exits from the top of the packed column section 3, and enters the plate column section 2 from the bottom, flowing upwards in the plate column section 2. This allows the anthraquinone working solution and water to come into countercurrent contact in the plate column section 2 and the packed column section 3, extracting hydrogen peroxide from the anthraquinone working solution.

[0061] The low-concentration hydrogen peroxide aqueous solution obtained by countercurrent contact of anthraquinone working solution and water in the plate column section 2 enters the packed column section 3 and is countercurrently contacted 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 packed column section 3 is led out from the aqueous phase outlet 7. In this extraction method, as the extractant phase flows downwards in plate column section 2, the concentration of hydrogen peroxide in the extractant phase increases. After entering packed column section 3, the extractant phase continues to flow downwards in packed column section 3, with the highest concentration of hydrogen peroxide at the bottom of packed column section 3. Therefore, plate column section 2 yields a low-concentration hydrogen peroxide solution, while packed column section 3 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 packed column section 3 and plate column section 2. This reduces the amount of material affected by explosion and eliminates the explosion risk of the high-concentration hydrogen peroxide solution contacting the anthraquinone working solution during the extraction process.

[0062] According to the present invention, the conditions under which the material undergoes countercurrent extraction in plate column section 2 and packed column section 3 have a certain influence on the extraction efficiency of hydrogen peroxide.

[0063] Under preferred conditions, the countercurrent contact conditions in the plate tower section 2 include: the temperature can be 50-55℃, for example 50℃, 51℃, 52℃, 53℃, 54℃ or 55℃; and the pressure can be atmospheric pressure.

[0064] Under preferred conditions, the countercurrent contact conditions in the packed tower section 3 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.

[0065] 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.

[0066] According to the present invention, limiting the ratio of the extractant to the 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 aqueous phase inlet 4 to the anthraquinone working liquid introduced from the anthraquinone working liquid inlet 5 can be 1:30 to 70, for example, 1:30, 1:35, 1:40, 1:45, 1:50, 1:55, 1:60, 1:65, or 1:70.

[0067] The present invention will be described in detail below through embodiments, but the scope of protection of the present invention is not limited thereto.

[0068] Example 1

[0069] Example 1 was carried out in the following hydrogen peroxide fractional extraction tower, such as... Figure 1-4 As shown:

[0070] The hydrogen peroxide fractional extraction tower includes a plate tower section 2 and a packed tower section 3. The plate tower section 2 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%.

[0071] The upper part of the plate tower section 2 has an aqueous phase inlet 4, and the lower part of the packed tower section 3 has an anthraquinone working liquid inlet 5; the top of the hydrogen peroxide segmented extraction tower is provided with a working liquid outlet 6, and the bottom of the hydrogen peroxide segmented extraction tower is provided with an aqueous phase outlet 7.

[0072] The packing layer of the packed tower section 3 includes 20 cylindrical packing discs. Each packing disc is formed by stacking corrugated packing sheets 31 of different lengths horizontally. The lengths of the corrugated packing sheets 31 gradually decrease from the center along the radius of the cylindrical packing disc. Multiple parallel oblique quadrangular prism channels 34 are formed by overlapping the crests 32 and troughs 33 of adjacent corrugated packing sheets 31. The inclination angle α of the oblique quadrangular prism channels 34 is 40°. The multiple oblique quadrangular prism channels 34 between adjacent packing discs... The vertical directions are one-to-one correspondences, and the corresponding oblique quadrangular prism channels 34 intersect each other; the height of the packing layer of the packed tower section 3 is 2m; the height of each packing disc is 100mm; the peak height h of each corrugated packing sheet 31 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 15°; the corrugated packing sheet 31 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 .

[0073] Hydrogen peroxide extraction methods include:

[0074] Water is introduced from the aqueous phase inlet 4, and anthraquinone working solution is introduced from the anthraquinone working solution inlet 5. The anthraquinone working solution and water are in countercurrent contact in the plate column section 2 and the packed column section 3. The hydrogen peroxide aqueous solution obtained from the countercurrent contact of the anthraquinone working solution and water in the plate column section 2 flows out from the bottom of the plate column section 2 and enters the packed column section 3 from the top 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 packed column section 3 is drawn out from the top of the packed column section 3 and then enters the plate column section 2 from the bottom to have countercurrent contact with the hydrogen peroxide aqueous solution.

[0075] The countercurrent contact conditions in the plate column section 2 include: a temperature of 52°C and a pressure of atmospheric pressure; the countercurrent contact conditions in the packed column section 3 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 aqueous phase inlet 4. 3 / h, the volume of anthraquinone working fluid introduced from the anthraquinone working fluid inlet 5 is 1300m³. 3 / h, the volume ratio of water to anthraquinone working solution is 1:65.

[0076] After extraction, the hydrogen peroxide concentration obtained from the aqueous phase outlet 7 at the bottom of the hydrogen peroxide segmented extraction tower is 52.8 wt%, and the residual hydrogen peroxide content in the raffinate drawn from the working liquid outlet 6 at the top of the hydrogen peroxide segmented extraction tower is 0.09 g / L.

[0077] Example 2

[0078] Example 2 was carried out in the following hydrogen peroxide fractional extraction tower, such as... Figure 1-4 As shown:

[0079] The hydrogen peroxide fractional extraction tower includes a plate tower section 2 and a packed tower section 3. The plate tower section 2 is a sieve plate tower with a theoretical number of 12 plates. The opening diameter on the surface of the sieve plate is Ф2.2mm and the opening rate is 14%.

[0080] The upper part of the plate tower section 2 has an aqueous phase inlet 4, and the lower part of the packed tower section 3 has an anthraquinone working liquid inlet 5; the top of the hydrogen peroxide segmented extraction tower is provided with a working liquid outlet 6, and the bottom of the hydrogen peroxide segmented extraction tower is provided with an aqueous phase outlet 7.

[0081] The packing layer of the packed tower section 3 includes 24 cylindrical packing discs. Each packing disc is formed by stacking corrugated packing sheets 31 of different lengths horizontally. The length of the corrugated packing sheets 31 gradually decreases from the center along the radius of the cylindrical packing disc. The crests 32 and troughs 33 of adjacent corrugated packing sheets 31 overlap to form multiple parallel oblique quadrangular prism channels 34. The inclination angle α of the oblique quadrangular prism channels 34 is 40°. The multiple oblique quadrangular prism channels 34 of adjacent packing discs are vertically aligned. The straight directions correspond one-to-one, and the corresponding oblique quadrangular prism channels 34 intersect each other; the height of the packing layer of the packed tower section 3 is 2.4m; the height of each packing disc is 100mm; the peak height h of each corrugated packing sheet 31 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 15°; the corrugated packing sheet 31 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 .

[0082] Hydrogen peroxide extraction methods include:

[0083] Water is introduced from the aqueous phase inlet 4, and anthraquinone working solution is introduced from the anthraquinone working solution inlet 5. The anthraquinone working solution and water are in countercurrent contact in the plate column section 2 and the packed column section 3. The hydrogen peroxide aqueous solution obtained from the countercurrent contact of the anthraquinone working solution and water in the plate column section 2 flows out from the bottom of the plate column section 2 and enters the packed column section 3 from the top 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 packed column section 3 is drawn out from the top of the packed column section 3 and then enters the plate column section 2 from the bottom to have countercurrent contact with the hydrogen peroxide aqueous solution.

[0084] The countercurrent contact conditions in the plate column section 2 include: a temperature of 53°C and a pressure of atmospheric pressure; the countercurrent contact conditions in the packed column section 3 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 aqueous phase inlet 4. 3 / h, the volume of anthraquinone working fluid introduced from the anthraquinone working fluid inlet 5 is 600m³. 3 / h, the volume ratio of water to anthraquinone working solution is 1:30.

[0085] After extraction, the hydrogen peroxide concentration obtained from the aqueous phase outlet 7 at the bottom of the hydrogen peroxide segmented extraction tower is 44.1 wt%, and the residual hydrogen peroxide content in the raffinate drawn from the working liquid outlet 6 at the top of the hydrogen peroxide segmented extraction tower is 0.10 g / L.

[0086] Example 3

[0087] Example 3 was carried out in the following hydrogen peroxide fractional extraction tower, such as... Figure 1-4 As shown:

[0088] The hydrogen peroxide fractional extraction tower includes a plate tower section 2 and a packed tower section 3. The plate tower section 2 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%.

[0089] The upper part of the plate tower section 2 has an aqueous phase inlet 4, and the lower part of the packed tower section 3 has an anthraquinone working liquid inlet 5; the top of the hydrogen peroxide segmented extraction tower is provided with a working liquid outlet 6, and the bottom of the hydrogen peroxide segmented extraction tower is provided with an aqueous phase outlet 7.

[0090] The packing layer of the packed tower section 3 includes 32 cylindrical packing discs. Each packing disc is formed by stacking corrugated packing sheets 31 of different lengths horizontally. The lengths of the corrugated packing sheets 31 gradually decrease from the center along the radius of the cylindrical packing disc. Multiple parallel oblique quadrangular prism channels 34 are formed by overlapping the crests 32 and troughs 33 of adjacent corrugated packing sheets 31. The inclination angle α of the oblique quadrangular prism channels 34 is 40°. The multiple oblique quadrangular prism channels 34 between adjacent packing discs... The vertical directions are one-to-one correspondences, and the corresponding oblique quadrangular prism channels 34 intersect each other; the height of the packing layer of the packed tower section 3 is 3.2m; the height of each packing disc is 100mm; the peak height h of each corrugated packing sheet 31 is 5mm, the peak width d is 6mm, the thickness is mm, and the included angle β between the two corrugations of each corrugated packing sheet 31 is 15°; the corrugated packing sheet 31 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 .

[0091] Hydrogen peroxide extraction methods include:

[0092] Water is introduced from the aqueous phase inlet 4, and anthraquinone working solution is introduced from the anthraquinone working solution inlet 5. The anthraquinone working solution and water are in countercurrent contact in the plate column section 2 and the packed column section 3. The hydrogen peroxide aqueous solution obtained from the countercurrent contact of the anthraquinone working solution and water in the plate column section 2 flows out from the bottom of the plate column section 2 and enters the packed column section 3 from the top 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 packed column section 3 is drawn out from the top of the packed column section 3 and then enters the plate column section 2 from the bottom to have countercurrent contact with the hydrogen peroxide aqueous solution.

[0093] The countercurrent contact conditions in the plate tower section 2 include: a temperature of 54°C and a pressure of atmospheric pressure; the countercurrent contact conditions in the packed tower section 3 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 aqueous phase inlet 4. 3 / h, the volume of anthraquinone working fluid introduced from the anthraquinone working fluid inlet 5 is 800m³. 3 / h, the volume ratio of water to anthraquinone working solution is 1:40.

[0094] After extraction, the hydrogen peroxide concentration obtained from the aqueous phase outlet 7 at the bottom of the hydrogen peroxide segmented extraction tower is 46.5 wt%, and the residual hydrogen peroxide content in the raffinate drawn from the working liquid outlet 6 at the top of the hydrogen peroxide segmented extraction tower is 0.07 g / L.

[0095] Example 4

[0096] Example 4 was carried out in the following hydrogen peroxide fractional extraction tower, such as... Figure 1-4 As shown:

[0097] The hydrogen peroxide fractional extraction tower includes a plate tower section 2 and a packed tower section 3. The plate tower section 2 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%.

[0098] The upper part of the plate tower section 2 has an aqueous phase inlet 4, and the lower part of the packed tower section 3 has an anthraquinone working liquid inlet 5; the top of the hydrogen peroxide segmented extraction tower is provided with a working liquid outlet 6, and the bottom of the hydrogen peroxide segmented extraction tower is provided with an aqueous phase outlet 7.

[0099] The packing layer of the packed tower section 3 includes 36 cylindrical packing discs. Each packing disc is formed by stacking corrugated packing sheets 31 of different lengths horizontally. The length of the corrugated packing sheets 31 gradually decreases from the center along the radius of the cylindrical packing disc. The crests 32 and troughs 33 of adjacent corrugated packing sheets 31 overlap to form multiple parallel oblique quadrangular prism channels 34. The inclination angle α of the oblique quadrangular prism channels 34 is 40°. The multiple oblique quadrangular prism channels 34 of adjacent packing discs are vertically aligned. The straight directions correspond one-to-one, and the corresponding oblique quadrangular prism channels 34 intersect each other; the height of the packing layer of the packed tower section 3 is 3.6m; the height of each packing disc is 100mm; the peak height h of each corrugated packing sheet 31 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 35°; the corrugated packing sheet 31 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 .

[0100] Hydrogen peroxide extraction methods include:

[0101] Water is introduced from the aqueous phase inlet 4, and anthraquinone working solution is introduced from the anthraquinone working solution inlet 5. The anthraquinone working solution and water are in countercurrent contact in the plate column section 2 and the packed column section 3. The hydrogen peroxide aqueous solution obtained from the countercurrent contact of the anthraquinone working solution and water in the plate column section 2 flows out from the bottom of the plate column section 2 and enters the packed column section 3 from the top 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 packed column section 3 is drawn out from the top of the packed column section 3 and then enters the plate column section 2 from the bottom to have countercurrent contact with the hydrogen peroxide aqueous solution.

[0102] The countercurrent contact conditions in the plate tower section 2 include: a temperature of 55°C and a pressure of atmospheric pressure; the countercurrent contact conditions in the packed tower section 3 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 aqueous inlet 4. 3 / h, the volume of anthraquinone working fluid introduced from the anthraquinone working fluid inlet 5 is 1000m³. 3 / h, the volume ratio of water to anthraquinone working solution is 1:50.

[0103] After extraction, the hydrogen peroxide concentration obtained from the aqueous phase outlet 7 at the bottom of the hydrogen peroxide segmented extraction tower is 48.5 wt%, and the residual hydrogen peroxide content in the raffinate drawn from the working liquid outlet 6 at the top of the hydrogen peroxide segmented extraction tower is 0.09 g / L.

[0104] Example 5

[0105] Example 5 was carried out in the following hydrogen peroxide fractional extraction tower, such as... Figure 1-4 As shown:

[0106] The hydrogen peroxide fractional extraction tower includes a plate tower section 2 and a packed tower section 3. The plate tower section 2 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 rate is 14%.

[0107] The upper part of the plate tower section 2 has an aqueous phase inlet 4, and the lower part of the packed tower section 3 has an anthraquinone working liquid inlet 5; the top of the hydrogen peroxide segmented extraction tower is provided with a working liquid outlet 6, and the bottom of the hydrogen peroxide segmented extraction tower is provided with an aqueous phase outlet 7.

[0108] The packing layer of the packed tower section 3 includes 40 cylindrical packing discs. Each packing disc is formed by stacking corrugated packing sheets 31 of different lengths horizontally. The lengths of the corrugated packing sheets 31 gradually decrease from the center along the radius of the cylindrical packing disc. Multiple parallel oblique quadrangular prism channels 34 are formed by overlapping the crests 32 and troughs 33 of adjacent corrugated packing sheets 31. The inclination angle α of the oblique quadrangular prism channels 34 is 40°. The multiple oblique quadrangular prism channels 34 between adjacent packing discs... The vertical directions are one-to-one correspondences, and the corresponding oblique quadrangular prism channels 34 intersect each other; the height of the packing layer of the packed tower section 3 is 4m; the height of each packing disc is 100mm; the peak height h of each corrugated packing sheet 31 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 45°; the corrugated packing sheet 31 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 .

[0109] Hydrogen peroxide extraction methods include:

[0110] Water is introduced from the aqueous phase inlet 4, and anthraquinone working solution is introduced from the anthraquinone working solution inlet 5. The anthraquinone working solution and water are in countercurrent contact in the plate column section 2 and the packed column section 3. The hydrogen peroxide aqueous solution obtained from the countercurrent contact of the anthraquinone working solution and water in the plate column section 2 flows out from the bottom of the plate column section 2 and enters the packed column section 3 from the top 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 packed column section 3 is drawn out from the top of the packed column section 3 and then enters the plate column section 2 from the bottom to have countercurrent contact with the hydrogen peroxide aqueous solution.

[0111] The countercurrent contact conditions in the plate column section 2 include: a temperature of 50°C and a pressure of atmospheric pressure; the countercurrent contact conditions in the packed column section 3 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 aqueous phase inlet 4. 3 / h, the volume of anthraquinone working fluid introduced from the anthraquinone working fluid inlet 5 is 1300m³. 3 / h, the volume ratio of water to anthraquinone working solution is 1:65.

[0112] After extraction, the hydrogen peroxide concentration obtained from the aqueous phase outlet 7 at the bottom of the hydrogen peroxide segmented extraction tower is 53.9 wt%, and the residual hydrogen peroxide content in the raffinate drawn from the working liquid outlet 6 at the top of the hydrogen peroxide segmented extraction tower is 0.06 g / L.

[0113] Example 6

[0114] Example 6 was carried out in the following hydrogen peroxide fractional extraction tower, such as... Figure 1-4 As shown:

[0115] The hydrogen peroxide fractional extraction tower includes a plate tower section 2 and a packed tower section 3. The plate tower section 2 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%.

[0116] The upper part of the plate tower section 2 has an aqueous phase inlet 4, and the lower part of the packed tower section 3 has an anthraquinone working liquid inlet 5; the top of the hydrogen peroxide segmented extraction tower is provided with a working liquid outlet 6, and the bottom of the hydrogen peroxide segmented extraction tower is provided with an aqueous phase outlet 7.

[0117] The packing layer of the packed tower section 3 includes 44 cylindrical packing discs. Each packing disc is formed by stacking corrugated packing sheets 31 of different lengths horizontally. The length of the corrugated packing sheets 31 gradually decreases from the center along the radius of the cylindrical packing disc. The crests 32 and troughs 33 of adjacent corrugated packing sheets 31 overlap to form multiple parallel oblique quadrangular prism channels 34. The inclination angle α of the oblique quadrangular prism channels 34 is 40°. The multiple oblique quadrangular prism channels 34 of adjacent packing discs are vertically aligned. The straight directions correspond one-to-one, and the corresponding oblique quadrangular prism channels 34 intersect each other; the height of the packing layer of the packed tower section 3 is 4.4m; the height of each packing disc is 100mm; the peak height h of each corrugated packing sheet 31 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 45°; the corrugated packing sheet 31 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 .

[0118] Hydrogen peroxide extraction methods include:

[0119] Water is introduced from the aqueous phase inlet 4, and anthraquinone working solution is introduced from the anthraquinone working solution inlet 5. The anthraquinone working solution and water are in countercurrent contact in the plate column section 2 and the packed column section 3. The hydrogen peroxide aqueous solution obtained from the countercurrent contact of the anthraquinone working solution and water in the plate column section 2 flows out from the bottom of the plate column section 2 and enters the packed column section 3 from the top 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 packed column section 3 is drawn out from the top of the packed column section 3 and then enters the plate column section 2 from the bottom to have countercurrent contact with the hydrogen peroxide aqueous solution.

[0120] The countercurrent contact conditions in the plate column section 2 include: a temperature of 51°C and a pressure of atmospheric pressure; the countercurrent contact conditions in the packed column section 3 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 aqueous phase inlet 4. 3 / h, the volume of anthraquinone working fluid introduced from the anthraquinone working fluid inlet 5 is 1400m³. 3 / h, the volume ratio of water to anthraquinone working solution is 1:70.

[0121] After extraction, the hydrogen peroxide concentration obtained from the aqueous phase outlet 7 at the bottom of the hydrogen peroxide segmented extraction tower is 55.4 wt%, and the residual hydrogen peroxide content in the raffinate drawn from the working liquid outlet 6 at the top of the hydrogen peroxide segmented extraction tower is 0.08 g / L.

[0122] Example 7

[0123] Example 7 was carried out in the following hydrogen peroxide fractional extraction tower, such as... Figure 1-4 As shown:

[0124] The hydrogen peroxide fractional extraction tower includes a plate tower section 2 and a packed tower section 3. The plate tower section 2 is a sieve plate tower with a theoretical number of 32 plates. The opening diameter on the surface of the sieve plate is Ф2.2mm and the opening rate is 14%.

[0125] The upper part of the plate tower section 2 has an aqueous phase inlet 4, and the lower part of the packed tower section 3 has an anthraquinone working liquid inlet 5; the top of the hydrogen peroxide segmented extraction tower is provided with a working liquid outlet 6, and the bottom of the hydrogen peroxide segmented extraction tower is provided with an aqueous phase outlet 7.

[0126] The packing layer of the packed tower section 3 includes 48 cylindrical packing discs. Each packing disc is formed by stacking corrugated packing sheets 31 of different lengths horizontally. The length of the corrugated packing sheets 31 gradually decreases from the center along the radius of the cylindrical packing disc. The crests 32 and troughs 33 of adjacent corrugated packing sheets 31 overlap to form multiple parallel oblique quadrangular prism channels 34. The inclination angle α of the oblique quadrangular prism channels 34 is 40°. The multiple oblique quadrangular prism channels 34 of adjacent packing discs are vertically aligned. The straight directions correspond one-to-one, and the corresponding oblique quadrangular prism channels 34 intersect each other; the height of the packing layer of the packed tower section 3 is 4.8m; the height of each packing disc is 100mm; the peak height h of each corrugated packing sheet 31 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 31 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 .

[0127] Hydrogen peroxide extraction methods include:

[0128] Water is introduced from the aqueous phase inlet 4, and anthraquinone working solution is introduced from the anthraquinone working solution inlet 5. The anthraquinone working solution and water are in countercurrent contact in the plate column section 2 and the packed column section 3. The hydrogen peroxide aqueous solution obtained from the countercurrent contact of the anthraquinone working solution and water in the plate column section 2 flows out from the bottom of the plate column section 2 and enters the packed column section 3 from the top 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 packed column section 3 is drawn out from the top of the packed column section 3 and then enters the plate column section 2 from the bottom to have countercurrent contact with the hydrogen peroxide aqueous solution.

[0129] The countercurrent contact conditions in the plate column section 2 include: a temperature of 53°C and a pressure of atmospheric pressure; the countercurrent contact conditions in the packed column section 3 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 aqueous phase inlet 4. 3 / h, the volume of anthraquinone working fluid introduced from the anthraquinone working fluid inlet 5 is 1300m³. 3 / h, the volume ratio of water to anthraquinone working solution is 1:65.

[0130] After extraction, the hydrogen peroxide concentration obtained from the aqueous phase outlet 7 at the bottom of the hydrogen peroxide segmented extraction tower is 54.5 wt%, and the residual hydrogen peroxide content in the raffinate drawn from the working liquid outlet 6 at the top of the hydrogen peroxide segmented extraction tower is 0.08 g / L.

[0131] Example 8

[0132] Example 8 was carried out in the following hydrogen peroxide fractional extraction tower, such as... Figure 1-4 As shown:

[0133] The hydrogen peroxide fractional extraction tower includes a plate tower section 2 and a packed tower section 3. The plate tower section 2 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%.

[0134] The upper part of the plate tower section 2 has an aqueous phase inlet 4, and the lower part of the packed tower section 3 has an anthraquinone working liquid inlet 5; the top of the hydrogen peroxide segmented extraction tower is provided with a working liquid outlet 6, and the bottom of the hydrogen peroxide segmented extraction tower is provided with an aqueous phase outlet 7.

[0135] The packing layer of the packed tower section 3 includes 52 cylindrical packing discs. Each packing disc is formed by stacking corrugated packing sheets 31 of different lengths horizontally. The length of the corrugated packing sheets 31 gradually decreases from the center along the radius of the cylindrical packing disc. The crests 32 and troughs 33 of adjacent corrugated packing sheets 31 overlap to form multiple parallel oblique quadrangular prism channels 34. The inclination angle α of the oblique quadrangular prism channels 34 is 40°. The multiple oblique quadrangular prism channels 34 between adjacent packing discs... The oblique quadrangular prism channels 34 are vertically aligned and intersect each other; the height of the packing layer in the packed tower section 3 is 5.2m; the height of each packing disc is 100mm; the peak height h of each corrugated packing sheet 31 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 31 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 .

[0136] Hydrogen peroxide extraction methods include:

[0137] Water is introduced from the aqueous phase inlet 4, and anthraquinone working solution is introduced from the anthraquinone working solution inlet 5. The anthraquinone working solution and water are in countercurrent contact in the plate column section 2 and the packed column section 3. The hydrogen peroxide aqueous solution obtained from the countercurrent contact of the anthraquinone working solution and water in the plate column section 2 flows out from the bottom of the plate column section 2 and enters the packed column section 3 from the top 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 packed column section 3 is drawn out from the top of the packed column section 3 and then enters the plate column section 2 from the bottom to have countercurrent contact with the hydrogen peroxide aqueous solution.

[0138] The countercurrent contact conditions in the plate column section 2 include: a temperature of 53°C and a pressure of atmospheric pressure; the countercurrent contact conditions in the packed column section 3 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 aqueous phase inlet 4. 3 / h, the volume of anthraquinone working fluid introduced from the anthraquinone working fluid inlet 5 is 1400m³. 3 / h, the volume ratio of water to anthraquinone working solution is 1:70.

[0139] After extraction, the hydrogen peroxide concentration obtained from the aqueous phase outlet 7 at the bottom of the hydrogen peroxide segmented extraction tower is 58.1 wt%, and the residual hydrogen peroxide content in the raffinate drawn from the working liquid outlet 6 at the top of the hydrogen peroxide segmented extraction tower is 0.06 g / L.

[0140] Example 9

[0141] Example 9 was carried out in the following hydrogen peroxide fractional extraction tower, such as... Figure 1-4 As shown:

[0142] The hydrogen peroxide fractional extraction tower includes a plate tower section 2 and a packed tower section 3. The plate tower section 2 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 rate is 14%.

[0143] The upper part of the plate tower section 2 has an aqueous phase inlet 4, and the lower part of the packed tower section 3 has an anthraquinone working liquid inlet 5; the top of the hydrogen peroxide segmented extraction tower is provided with a working liquid outlet 6, and the bottom of the hydrogen peroxide segmented extraction tower is provided with an aqueous phase outlet 7.

[0144] The packing layer of the packed tower section 3 includes 56 cylindrical packing discs. Each packing disc is formed by stacking corrugated packing sheets 31 of different lengths horizontally. The length of the corrugated packing sheets 31 gradually decreases from the center along the radius of the cylindrical packing disc. The crests 32 and troughs 33 of adjacent corrugated packing sheets 31 overlap to form multiple parallel oblique quadrangular prism channels 34. The inclination angle α of the oblique quadrangular prism channels 34 is 40°. The multiple oblique quadrangular prism channels 34 of adjacent packing discs are vertically aligned. The straight directions correspond one-to-one, and the corresponding oblique quadrangular prism channels 34 intersect each other; the height of the packing layer of the packed tower section 3 is 5.6m; the height of each packing disc is 100mm; the peak height h of each corrugated packing sheet 31 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 85°; the corrugated packing sheet 31 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 .

[0145] Hydrogen peroxide extraction methods include:

[0146] Water is introduced from the aqueous phase inlet 4, and anthraquinone working solution is introduced from the anthraquinone working solution inlet 5. The anthraquinone working solution and water are in countercurrent contact in the plate column section 2 and the packed column section 3. The hydrogen peroxide aqueous solution obtained from the countercurrent contact of the anthraquinone working solution and water in the plate column section 2 flows out from the bottom of the plate column section 2 and enters the packed column section 3 from the top 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 packed column section 3 is drawn out from the top of the packed column section 3 and then enters the plate column section 2 from the bottom to have countercurrent contact with the hydrogen peroxide aqueous solution.

[0147] The countercurrent contact conditions in the plate tower section 2 include: a temperature of 54°C and a pressure of atmospheric pressure; the countercurrent contact conditions in the packed tower section 3 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 aqueous phase inlet 4. 3 / h, the volume of anthraquinone working fluid introduced from the anthraquinone working fluid inlet 5 is 1400m³. 3 / h, the volume ratio of water to anthraquinone working solution is 1:70.

[0148] After extraction, the hydrogen peroxide concentration obtained from the aqueous phase outlet 7 at the bottom of the hydrogen peroxide segmented extraction tower is 59.6 wt%, and the residual hydrogen peroxide content in the raffinate drawn from the working liquid outlet 6 at the top of the hydrogen peroxide segmented extraction tower is 0.06 g / L.

[0149] Example 10

[0150] Example 10 was carried out in the following hydrogen peroxide fractional extraction tower, such as... Figure 1-4 As shown:

[0151] The hydrogen peroxide fractional extraction tower includes a plate tower section 2 and a packed tower section 3. The plate tower section 2 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 rate is 14%.

[0152] The upper part of the plate tower section 2 has an aqueous phase inlet 4, and the lower part of the packed tower section 3 has an anthraquinone working liquid inlet 5; the top of the hydrogen peroxide segmented extraction tower is provided with a working liquid outlet 6, and the bottom of the hydrogen peroxide segmented extraction tower is provided with an aqueous phase outlet 7.

[0153] The packing layer of the packed tower section 3 includes 60 cylindrical packing discs. Each packing disc is formed by stacking corrugated packing sheets 31 of different lengths horizontally. The lengths of the corrugated packing sheets 31 gradually decrease from the center along the radius of the cylindrical packing disc. Multiple parallel oblique quadrangular prism channels 34 are formed by overlapping the crests 32 and troughs 33 of adjacent corrugated packing sheets 31. The inclination angle α of the oblique quadrangular prism channels 34 is 40°. The multiple oblique quadrangular prism channels 34 between adjacent packing discs... The vertical directions are one-to-one correspondences, and the corresponding oblique quadrangular prism channels 34 intersect each other; the height of the packing layer of the packed tower section 3 is 6m; the height of each packing disc is 100mm; the peak height h of each corrugated packing sheet 31 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 85°; the corrugated packing sheet 31 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 .

[0154] Hydrogen peroxide extraction methods include:

[0155] Water is introduced from the aqueous phase inlet 4, and anthraquinone working solution is introduced from the anthraquinone working solution inlet 5. The anthraquinone working solution and water are in countercurrent contact in the plate column section 2 and the packed column section 3. The hydrogen peroxide aqueous solution obtained from the countercurrent contact of the anthraquinone working solution and water in the plate column section 2 flows out from the bottom of the plate column section 2 and enters the packed column section 3 from the top 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 packed column section 3 is drawn out from the top of the packed column section 3 and then enters the plate column section 2 from the bottom to have countercurrent contact with the hydrogen peroxide aqueous solution.

[0156] The countercurrent contact conditions in the plate column section 2 include: a temperature of 51°C and a pressure of atmospheric pressure; the countercurrent contact conditions in the packed column section 3 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 aqueous phase inlet 4. 3 / h, the volume of anthraquinone working fluid introduced from the anthraquinone working fluid inlet 5 is 1400m³. 3 / h, the volume ratio of water to anthraquinone working solution is 1:70.

[0157] After extraction, the hydrogen peroxide concentration obtained from the aqueous phase outlet 7 at the bottom of the hydrogen peroxide segmented extraction tower is 60.2 wt%, and the residual hydrogen peroxide content in the raffinate drawn from the working liquid outlet 6 at the top of the hydrogen peroxide segmented extraction tower is 0.05 g / L.

[0158] Comparative Example

[0159] 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.

[0160] 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.

[0161] 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.

[0162] 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 method for hydrogen peroxide extraction, characterized in that, This method is carried out in a hydrogen peroxide fractional extraction tower; The hydrogen peroxide fractional extraction tower includes a tower body (1), which is provided with a plate tower section (2) and a packed tower section (3) from top to bottom. The upper part of the plate tower section (2) has an aqueous phase inlet (4), and the lower part of the packed tower section (3) has an anthraquinone working liquid inlet (5). The packed tower section (3) includes several packing discs. Each packing disc is formed by stacking multiple corrugated packing sheets (31) in the horizontal direction. The crests (32) and troughs (33) of two adjacent corrugated packing sheets (31) are superimposed to form multiple parallel oblique quadrangular prism channels (34). The inclination angle α of the oblique quadrangular prism channels (34) is 20~80°. In the packed tower section (3), multiple oblique quadrangular prism channels (34) of two adjacent packing discs correspond one-to-one in the vertical direction, and the corresponding oblique quadrangular prism channels (34) intersect each other; The peak height h of each corrugated packing sheet (31) is 2~12mm, the peak width d is 3~30mm, and the thickness is 0.5mm~3mm; The hydrogen peroxide fractional extraction tower is provided with a working liquid outlet (6) at the top and an aqueous phase outlet (7) at the bottom. The method includes: introducing water from the aqueous phase inlet (4), introducing anthraquinone working solution from the anthraquinone working solution inlet (5), the anthraquinone working solution and water being contacted countercurrently in the plate column section (2) and the packed column section (3), obtaining a raffinate with a low hydrogen peroxide concentration and an aqueous hydrogen peroxide solution with a high hydrogen peroxide concentration in the plate column section (2) and the packed column section (3), respectively, and obtaining an aqueous hydrogen peroxide solution with a concentration greater than 44% from the aqueous phase outlet (7) at the bottom of the hydrogen peroxide fractional extraction column; The hydrogen peroxide concentration in the anthraquinone working solution is 6~20 g / L; The volume ratio of water introduced from the aqueous phase inlet (4) to anthraquinone working solution introduced from the anthraquinone working solution inlet (5) is 1:30~70.

2. The method according to claim 1, characterized in that, Each packing disc is cylindrical and is composed of multiple corrugated packing sheets (31) of different lengths stacked together. The length of the multiple corrugated packing sheets (31) gradually decreases from the center along the radius of the cylindrical packing disc.

3. The method according to claim 1, characterized in that, The height of the packing layer in the packed tower section (3) is 2~6m.

4. The method according to claim 3, characterized in that, The height of the packing layer in the packed tower section (3) is 3~5m.

5. The method according to claim 1, characterized in that, The height of each packing disc is 30~500mm.

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

7. The method according to claim 1, characterized in that, The included angle β between the two corrugations of the corrugated packing sheet (31) is 15~85°.

8. The method according to claim 1, characterized in that, The corrugated packing sheet (31) is a plate mesh corrugated packing sheet, wherein the wire diameter of the plate mesh is 0.1~4mm.

9. The method according to claim 8, characterized in that, The mesh shape of the plate mesh is rectangular or rhomboid, and the mesh area is (3~20) x (3~20) mm. 2 .

10. The method according to claim 1, characterized in that, The plate tower section (2) is a sieve plate tower with a theoretical number of 10 to 40 plates.

11. The method according to claim 1, characterized in that, The countercurrent contact conditions in the plate tower section (2) include: a temperature of 50~55℃ and a pressure of atmospheric pressure.

12. The method according to claim 1, characterized in that, The conditions for countercurrent contact in the packed tower section (3) include: temperature of 50~55℃ and pressure of atmospheric pressure.

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