Working solution reaction device for anthraquinone process hydrogen peroxide

By constructing multiple containment chambers and adding a flow guide tube inside the outer reaction cylinder, the problems of increased bed resistance and catalyst accumulation in traditional fixed-bed hydrogenation devices were solved, achieving uniform contact between the working fluid and hydrogen, and improving reaction efficiency and product quality.

CN223766092UActive Publication Date: 2026-01-06NANTONG QIANGYE CHEMICAL CO LTD
View PDF 0 Cites 0 Cited by

Patent Information

Application Number
CN202420556243.2
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-03-21
Publication Date
2026-01-06
Estimated Expiration
2034-03-21

AI Technical Summary

Technical Problem

Traditional fixed-bed hydrogenation units are prone to problems such as increased bed resistance and catalyst agglomeration in the anthraquinone process for hydrogen peroxide production, which affect reaction efficiency and product quality.

Method used

Multiple containment chambers are constructed inside the outer reaction cylinder, and guide tubes are added to some of the containment chambers. The guide tubes are made of stainless steel wire mesh, with liquid permeation holes smaller than the particle size of palladium catalyst. The diameter increases layer by layer downwards, and the staggered arrangement increases the porosity to ensure uniform contact between the working fluid and hydrogen.

Benefits of technology

It reduces bed resistance, avoids channeling and liquid accumulation, improves reaction efficiency, reduces hydrogen peroxide and catalyst buildup, and improves the performance of the outer reaction cylinder.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN223766092U_ABST
    Figure CN223766092U_ABST
Patent Text Reader

Abstract

The utility model discloses a working solution reaction device for anthraquinone process hydrogen peroxide. The working solution reaction device comprises a vertically arranged reaction outer cylinder, each partition plate comprises two grating plates which are oppositely arranged up and down, the outer edges of the grating plates are connected to the inner wall of the reaction outer cylinder, a containing bin is formed between the two grating plates, and the four partition plates are arranged at intervals in the axial direction of the reaction outer cylinder; each flow guide cylinder is provided with two closed ends and is provided with a plurality of liquid penetrating holes, the hole diameter of each liquid penetrating hole is smaller than the particle size of a palladium catalyst, a plurality of flow guide cylinders are installed in the containing bins except the containing bin on the top layer, the flow guide cylinders are arranged in the axial direction of the reaction outer cylinder, and the diameters of the flow guide cylinders are gradually increased downwards layer by layer; and the number of the guide cylinders arranged in each layer of accommodating bin is the same. The utility model solves the problems that the resistance of a bed layer is increased and a catalyst is easy to block after a fixed bed in a working solution hydrogenation stage in the production process of hydrogen peroxide by an anthraquinone process is used for a period of time.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] This utility model relates to the field of hydrogen peroxide preparation technology, specifically to a working solution reaction device for anthraquinone hydrogen peroxide. Background Technology

[0002] The anthraquinone process for hydrogen peroxide production uses alkyl anthraquinones as a carrier and heavy aromatic hydrocarbons, trioctyl phosphate, methylcyclohexyl acetate, tetrabutylurea, etc., as solvents to prepare a working solution. This working solution undergoes continuous cycling through hydrogenation, oxidation, extraction, and post-treatment to produce hydrogen peroxide. Through further processes such as formulation and concentration, hydrogen peroxide products of various concentrations are obtained.

[0003] Hydrogenation of the working fluid is the initial and crucial stage of the production process. Traditional fixed-bed hydrogenation involves randomly packing spherical palladium catalyst particles with a particle size of Ø2 to Ø3 into the column to form a fixed bed with a height of 4000 to 6000 mm. The working fluid and hydrogen gas simultaneously enter the column from the top and are evenly sprayed onto the catalyst surface by a distributor, partially converting 2-ethylanthraquinone into hydrogen anthraquinone, forming a hydrogenated liquid that reaches the bottom of the column. After separation by a separator, it proceeds to the next process.

[0004] Fixed-bed design has always been a technological challenge. A large aspect ratio results in high bed resistance, leading to liquid accumulation and hindering the reaction; a small aspect ratio results in low spray density, causing channeling and other problems. Therefore, regardless of the optimal aspect ratio, the following phenomena will occur in actual production: after a period of use, the bed resistance increases, reaction efficiency decreases, localized over-hydrogenation occurs, and more hydrogenated degradation products are produced. Especially in alkaline units and alumina beds with high dust levels, the catalyst clumps, requiring catalyst regeneration frequently, and sometimes even requiring the catalyst to be removed and screened, severely impacting production, increasing the consumption of palladium catalyst and various raw materials, and significantly degrading product quality.

[0005] The information disclosed in this background section is intended only to enhance the understanding of the overall background of this utility model and should not be construed as an admission or in any way implying that the information constitutes prior art known to those skilled in the art. Utility Model Content

[0006] To overcome the shortcomings of existing technologies, a working fluid reaction device for anthraquinone hydrogen peroxide production is provided to solve the problem that the fixed bed in the hydrogenation stage of the working fluid in the anthraquinone hydrogen peroxide production process is prone to increased bed resistance and catalyst accumulation after a period of use.

[0007] To achieve the above objectives, a working solution reaction apparatus for anthraquinone hydrogen peroxide is provided, comprising:

[0008] The reaction outer cylinder is arranged vertically. The upper end of the reaction outer cylinder has an inlet for inputting the working solution of anthraquinone hydrogen peroxide and an inlet for inputting hydrogen gas. The lower end of the reaction outer cylinder has an outlet.

[0009] The four partition plates each include two grid plates arranged opposite each other, the outer edge of the grid plates is connected to the inner wall of the outer reaction cylinder, and a accommodating chamber for palladium catalyst filling is formed between the two grid plates. The four partition plates are spaced apart along the axial direction of the outer reaction cylinder.

[0010] The guide tube has two closed ends and multiple liquid permeation holes. The diameter of the liquid permeation holes is smaller than the particle size of the palladium catalyst. Multiple guide tubes are installed in each of the accommodating chambers except the top accommodating chamber. The guide tubes are arranged along the axial direction of the outer reaction cylinder. The diameter of the guide tubes increases layer by layer downwards. The number of guide tubes is the same in each accommodating chamber.

[0011] Furthermore, multiple guide tubes in the adjacent two-layer containment chambers are staggered.

[0012] Furthermore, the diameter of the guide tube is 50-100 mm.

[0013] Furthermore, the guide tube is centrally positioned between the two grid plates.

[0014] Furthermore, the distance between the end of the guide tube and the grid plate is 100mm.

[0015] Furthermore, the diameter of the liquid permeation hole is less than 2 mm.

[0016] Furthermore, the guide tube is a stainless steel wire mesh tube.

[0017] The beneficial effects of this invention are as follows: the working fluid reaction device for anthraquinone hydrogen peroxide uses multiple containment chambers for filling palladium catalysts within the outer reaction cylinder. Furthermore, by adding guide tubes to some of these chambers, the porosity of the outer reaction cylinder is increased, reducing bed resistance. Under high spray density, this ensures that the working fluid and hydrogen gas are in full and uniform contact within the catalyst layer, preventing channeling and liquid accumulation, thus reducing hydrogen peroxide and catalyst buildup and significantly improving the performance of the outer reaction cylinder. Attached Figure Description

[0018] Other features, objects, and advantages of this application will become more apparent from the following detailed description of non-limiting embodiments with reference to the accompanying drawings:

[0019] Figure 1 This is a schematic diagram of the working solution reaction device for the anthraquinone method of hydrogen peroxide according to an embodiment of this utility model.

[0020] Figure 2 for Figure 1 The sectional view at point AA. Detailed Implementation

[0021] The present application will now be described in further detail with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the relevant utility model and not intended to limit the scope of the utility model. Furthermore, it should be noted that, for ease of description, only the parts relevant to the utility model are shown in the accompanying drawings.

[0022] It should be noted that, unless otherwise specified, the embodiments and features described in this application can be combined with each other. This application will now be described in detail with reference to the accompanying drawings and embodiments.

[0023] Reference Figure 1 and Figure 2 As shown, this utility model provides a working solution reaction device for anthraquinone hydrogen peroxide, including: an outer reaction cylinder 1, a partition plate, and a guide cylinder 3.

[0024] The outer reaction cylinder 1 is cylindrical. The outer reaction cylinder 1 is vertically oriented. The upper end of the outer reaction cylinder 1 has an inlet for the working solution of anthraquinone hydrogen peroxide and an inlet for hydrogen gas. The lower end of the outer reaction cylinder 1 has an outlet.

[0025] Four partition plates divide the interior of the outer reaction cylinder into multiple sections. Specifically, each partition plate includes two grid plates 21 arranged vertically opposite each other. The outer edge of the grid plate 21 is connected to the inner wall of the outer reaction cylinder 1. A receiving chamber for filling palladium catalyst is formed between the two grid plates 21. The pore size of the grid plate is smaller than the particle size of the palladium catalyst. The four partition plates are spaced apart along the axial direction of the outer reaction cylinder 1.

[0026] The guide tube 3 is cylindrical. The guide tube 3 has two closed ends. The guide tube 3 has multiple liquid permeation holes. The diameter of the liquid permeation holes is smaller than the particle size of the palladium catalyst.

[0027] As a preferred embodiment, the diameter of the liquid permeation hole is less than 2 mm.

[0028] In this embodiment, the guide tube 3 is a stainless steel wire mesh tube.

[0029] Except for the top-level container, each of the other containers is equipped with multiple guide tubes 3. The guide tubes 3 are arranged along the axial direction of the outer reaction cylinder 1. The diameter of the guide tubes 3 increases progressively downwards. The number of guide tubes 3 is the same in each container.

[0030] Multiple guide tubes 3 are staggered in the upper and lower adjacent containment chambers.

[0031] In this embodiment, the diameter of the guide tube 3 is 50-100mm. The guide tube 3 is centrally located between the two grid plates 21. The distance between the end of the guide tube 3 and the grid plate 21 is 100mm.

[0032] In this embodiment, the four partition plates axially divide the catalyst layer of the outer reaction cylinder into four layers (segments) of containment chambers. The top layer of containment chamber is the low hydrogen efficiency zone a, the second layer of containment chamber is the low-to-medium hydrogen efficiency zone b, the third layer of containment chamber is the medium-to-high hydrogen efficiency zone c, and the fourth layer of containment chamber is the high hydrogen efficiency zone d.

[0033] The first-layer containment chamber does not have a flow guide tube due to its low hydrogen efficiency. The second-layer containment chamber is equipped with a flow guide tube, and its porosity is increased by 5%; the porosity of the third-layer containment chamber is increased by 7.5%, and the porosity of the fourth-layer containment chamber is increased by 10%.

[0034] The flow guide tube is a sealed cylindrical structure made of stainless steel wire mesh (pore size <Ø2mm). The diameter of the flow guide tube ranges from Ø50mm to Ø100mm. The height of the flow guide tube is designed according to the height of the catalyst layer. The flow guide tube is vertically installed on the grid plate inside the outer reaction chamber to prevent catalyst leakage. Multiple flow guide tubes in each containment chamber are arranged in a matrix. The flow guide tubes in the upper and lower containment chambers are staggered.

[0035] Specifically, the number of guide tubes in each layer of the containment chamber is determined by the increased void ratio. Taking a Ø2400 diameter tube as an example, the second layer of the containment chamber has 115 Ø50mm guide tubes installed, the third layer has 115 Ø62mm guide tubes installed, the fourth layer has 115 Ø71mm guide tubes installed, and so on.

[0036] If the catalyst in a single-section reaction outer cylinder is stacked in multiple layers, the guide tube should also be designed in accordance with the above. The length of the guide tube should be 200mm shorter than the height of the catalyst layer, with 100mm clearance at the top and bottom, and it should be buried inside the catalyst layer.

[0037] The working fluid reaction device for anthraquinone hydrogen peroxide of this invention employs multiple containment chambers for filling palladium catalyst within the outer reaction cylinder. Furthermore, by adding guide tubes to some of these chambers, the porosity of the outer reaction cylinder is increased, reducing bed resistance. Under high spray density conditions, this ensures that the working fluid and hydrogen gas are in full and uniform contact within the catalyst layer, preventing channeling and liquid accumulation, thus reducing hydrogen peroxide and catalyst buildup and significantly improving the performance of the outer reaction cylinder.

[0038] The above description is merely a preferred embodiment of this application and an explanation of the technical principles employed. Those skilled in the art should understand that the scope of the utility model involved in this application is not limited to the technical solutions formed by specific combinations of the above-described technical features, but should also cover other technical solutions formed by arbitrary combinations of the above-described technical features or their equivalents without departing from the inventive concept. For example, technical solutions formed by substituting the above features with (but not limited to) technical features with similar functions disclosed in this application.

Claims

1. A working solution reaction device for anthraquinone hydrogen peroxide, characterized by, The application relates to an anthraquinone hydrogen peroxide production device. The reaction outer cylinder is vertically arranged, the upper end of the reaction outer cylinder is provided with a liquid inlet for inputting working liquid of anthraquinone hydrogen peroxide and a gas inlet for inputting hydrogen, and the lower end of the reaction outer cylinder is provided with a liquid outlet. Each of the four partition plates comprises two grid plates arranged oppositely, the outer edges of the grid plates are connected to the inner wall of the reaction outer cylinder, the two grid plates form a containing cavity for filling palladium catalyst, and the four partition plates are arranged along the axial direction of the reaction outer cylinder. The flow guide cylinder has two closed ends, the flow guide cylinder is provided with a plurality of liquid-permeable holes, the diameter of the liquid-permeable holes is smaller than the particle size of the palladium catalyst, a plurality of flow guide cylinders are respectively arranged in the containing cavities except the containing cavities of the top layer, the flow guide cylinders are arranged along the axial direction of the reaction outer cylinder, the diameter of the flow guide cylinders gradually increases layer by layer, and the number of the flow guide cylinders arranged in each layer of the containing cavities is the same.

2. The working solution reactor for anthraquinone process hydrogen peroxide according to claim 1, characterized in that, The plurality of flow guide cylinders in the containing cavities of adjacent two layers are arranged in a staggered mode.

3. The working solution reactor for anthraquinone process hydrogen peroxide according to claim 1, characterized in that, The diameter of the flow guide cylinder is 50-100 mm.

4. The working solution reactor for anthraquinone process hydrogen peroxide according to claim 1, characterized in that, The flow guide cylinder is arranged centrally between the two grid plates.

5. The working solution reactor for anthraquinone process hydrogen peroxide according to claim 4, characterized in that, The distance between the end of the flow guide cylinder and the grid plate is 100 mm.

6. The working solution reactor for anthraquinone process hydrogen peroxide according to claim 1, characterized in that, The diameter of the liquid-permeable hole is smaller than 2 mm.

7. The working solution reactor for anthraquinone process hydrogen peroxide according to claim 6, characterized in that, The flow guide cylinder is a stainless steel wire mesh cylinder.