Hydrogenation reactor for producing hydrogen peroxide by anthraquinone process

By designing a hydrogenation reactor with built-in catalyst separator and external circulation system, the problems of low catalyst utilization and low reaction efficiency in fixed-bed catalytic hydrogenation reaction are solved, and efficient hydrogenation reaction and high-quality production of hydrogen peroxide products are achieved.

CN222658615UActive Publication Date: 2025-03-25PINGXIANG CHENGSONG ENVIROMENT PROTECTING PACKING CO LTD
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Patent Information

Application Number
CN202421352210.2
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-06-14
Publication Date
2025-03-25
Estimated Expiration
2034-06-14

AI Technical Summary

Technical Problem

In the anthraquinone method, during the fixed bed catalytic hydrogenation reaction, the catalyst is fixed and the contact area between the reaction material and the catalyst is limited, resulting in low hydrogenation reaction efficiency, low product yield, low effective utilization rate of the catalyst and high operating cost.

Method used

A hydrogenation reactor including a hydrogenation tower and internal and external pipelines is designed, with a built-in catalyst separator and an external circulation system. The uniform distribution and utilization of hydrogen and working fluid are achieved through the hydrogen distributor and the working fluid distributor, thereby improving the reaction efficiency.

Benefits of technology

Through the design of the built-in separator and external circulation system, continuous and stable operation of reaction and separation is achieved, the efficiency of hydrogenation reaction and the quality of hydrogen peroxide products are improved, and the production cost is reduced.

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Abstract

The utility model relates to the technical field of hydrogenation reactors, in particular to a hydrogenation reactor for producing hydrogen peroxide by an anthraquinone process. A hydrogenation reactor for producing hydrogen peroxide by an anthraquinone process comprises a hydrogenation tower, an inner pipeline and an outer pipeline, and a hydrogen inlet is formed in the outer surface of the bottom of the hydrogenation tower; a hydrogen distributor is arranged on the bottom plane in the hydrogenation tower and is communicated with a hydrogen inlet through an internal pipeline. The design of the hydrogenation reactor makes full use of the advantages of the hydrogenation tower (fluidized bed) technology, improves the efficiency of hydrogenation reaction and the quality of hydrogen peroxide products, and reduces the production cost at the same time.
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Description

Technical Field

[0001] The utility model relates to the technical field of hydrogenation reactors, in particular to a hydrogenation reactor for producing hydrogen peroxide by an anthraquinone process. Background Art

[0002] Hydrogen peroxide (hydrogen peroxide) is suitable for surface disinfection, food disinfection, odor removal and other functions. With the increasing demand for supporting development of chemical products such as caprolactam, propylene oxide, and adipic acid in my country's papermaking industry, fine chemicals, there are currently two main types of equipment for producing hydrogen peroxide in China: fixed bed and fluidized bed. At present, the fixed bed production process is mainly based on: a palladium catalyst support is installed in the fixed bed. The fixed palladium catalyst bed is hydrogenated with the alkyl anthraquinone in the organic solvent to obtain the corresponding alkyl hydroanthraquinone, which is then oxidized to generate H2O2, and the alkyl hydroanthraquinone is converted back to alkyl anthraquinone. The generated H2O2 is extracted with pure water to obtain the product, and the remaining alkyl anthraquinone solution can be recycled after treatment.

[0003] The advantages of the anthraquinone method are low energy consumption, environmental protection, good safety, and suitability for large-scale production. However, in the fixed-bed catalytic hydrogenation reaction process, since the catalyst is in a fixed state, the contact area between the reactants and the catalyst is limited, the hydrogenation reaction efficiency is low, and the product yield is low; there are also phenomena such as biased flow and channel flow, which lead to unbalanced reactions, high resistance and high temperature, many side reactions and by-products, and the quality of hydrogen peroxide products is affected. The effective utilization rate of the catalyst is low, the operating cost is high, and the amount of catalyst added at one time is large, and the catalyst cannot be replaced at any time. In view of this, it is of great significance to make structural improvements to the hydrogenation reactor in the anthraquinone method. Utility Model Content

[0004] In order to overcome the above-mentioned shortcomings, the technical problem to be solved is: to provide a hydrogenation reactor for producing hydrogen peroxide by anthraquinone method.

[0005] The technical scheme of the utility model is as follows: a hydrogenation reactor for producing hydrogen peroxide by anthraquinone method, comprising a hydrogenation tower and internal and external pipelines, wherein a hydrogen inlet is arranged on the outer surface of the bottom of the hydrogenation tower; a hydrogen distributor is arranged on the inner bottom plane of the hydrogenation tower, and the hydrogen inlet is connected through an internal pipeline; a catalyst feeding port is arranged on the lower outer surface of the hydrogenation tower; a working liquid distributor is arranged at the lower part of the hydrogenation tower; a working liquid inlet is arranged on the lower outer surface of the hydrogenation tower, and the working liquid distributor is connected through an internal pipeline; a catalyst separator is arranged in the middle of the hydrogenation tower; a low-position hydrogenation liquid outlet and a high-low position hydrogenation liquid outlet are arranged on the outer surface of the middle part of the hydrogenation tower, both of which are located above the catalyst separator and are used to extract hydrogenation liquid at different heights; a coalescer is arranged on the upper part of the hydrogenation tower, and is used to merge liquid droplets; a gas outlet is arranged on the top of the hydrogenation tower; an air inlet is arranged on the upper outer surface of the hydrogenation tower, and the air inlet is located below the coalescer.

[0006] As a preferred technical solution of the utility model, the external pipeline includes a primary filter air pipeline, a primary filter air outlet and a primary filter which are connected in sequence; the other end of the primary filter air pipeline is connected to the air inlet of the hydrogenation tower; a primary filter clear liquid outlet is provided on the upper outer surface of the primary filter, and the primary filter clear liquid outlet is connected to the interface of the subsequent process; a primary filter membrane separator is provided in the middle of the primary filter; a primary filter hydrogenation liquid inlet is provided on the lower outer surface of the primary filter, and the primary filter hydrogenation liquid inlet is located below the primary filter membrane separator; the low / high position hydrogenation liquid outlet of the hydrogenation tower is connected to the primary filter hydrogenation liquid inlet through the hydrogenation liquid outlet pipeline; a primary filter backwash outlet is provided at the bottom of the primary filter, and the primary filter backwash outlet is connected to the backwash reflux inlet on the lower outer surface of the hydrogenation tower through the backwash reflux pipeline.

[0007] As an optimal technical solution of the utility model, the hydrogen distributor is a pipe-type distributor, which is provided with a main pipe and a branch pipe. Small holes are opened downward at intervals of 30° below the main pipe and the branch pipe. The main pipe and the branch pipe are connected by flanges and fixed on the tower bottom plane by brackets.

[0008] As a preferred technical solution of the utility model, the working liquid distributor is a tubular structure extending inward to the center of the tower and bending downward, and the lower end of the tube body is provided with small holes arranged in a ring.

[0009] Compared with the prior art, the utility model has the following advantages: 1. The design of the hydrogenation reactor fully utilizes the advantages of the hydrogenation tower (fluidized bed) technology, improves the efficiency of the hydrogenation reaction and the quality of the hydrogen peroxide product, and reduces the production cost.

[0010] 2. Through the design of built-in separator and external circulation system, continuous and stable operation of reaction and separation is achieved, which has high industrial application value. BRIEF DESCRIPTION OF THE DRAWINGS

[0011] Figure 1 It is a schematic diagram of the planar structure of the utility model.

[0012] Marked in the figure: 1-hydrogenation tower, 2-hydrogen inlet, 3-hydrogen distributor, 4-catalyst feeding port, 5-working liquid distributor, 6-working liquid inlet, 7-catalyst separator, 8-low-position hydrogenation liquid outlet, 9-high-position hydrogenation liquid outlet, 10-coalescer, 11-gas outlet, 12-air inlet, 13-primary filter air pipeline, 14-primary filter air outlet, 15-primary filter, 16-primary filter clear liquid outlet, 17-primary filter membrane separator, 18-hydrogenation liquid outlet pipeline, 19-primary filter hydrogenation liquid inlet, 20-primary filter backwash outlet, 21-backwash reflux pipeline, 22-backwash reflux inlet. DETAILED DESCRIPTION

[0013] Although the present invention can be described with respect to a specific application or industry, those skilled in the art will recognize the broader applicability of the present invention. Those skilled in the art will recognize that terms such as: above, inside, outer surface, etc. are used to describe the drawings, rather than to limit the scope of the present invention as defined by the appended claims.

[0014] Example 1

[0015] like Figure 1 As shown, a hydrogenation reactor for producing hydrogen peroxide by anthraquinone method comprises a hydrogenation tower 1, a hydrogen inlet 2 and internal and external pipelines, wherein the hydrogen inlet 2 is arranged on the outer surface of the bottom of the hydrogenation tower 1; a hydrogen distributor 3 is arranged on the bottom plane inside the hydrogenation tower 1, and is connected to the hydrogen inlet 2 through an internal pipeline; a catalyst feeding port 4 is arranged on the lower outer surface of the hydrogenation tower 1; a working liquid distributor 5 is arranged at the lower part of the hydrogenation tower 1; a working liquid inlet 6 is arranged on the lower outer surface of the hydrogenation tower 1, and is connected to the working liquid distributor 5 through an internal pipeline; a catalyst separator 7 is arranged in the middle of the hydrogenation tower 1; a low-position hydrogenation liquid outlet 8 and a high-low position hydrogenation liquid outlet 8 are arranged on the outer surface of the middle part of the hydrogenation tower 1, both of which are located above the catalyst separator 7 and are used to extract hydrogenation liquid at different heights; a coalescer 10 is arranged on the upper part of the hydrogenation tower 1 for merging liquid droplets; a gas outlet 11 is arranged on the top of the hydrogenation tower 1; an air inlet 12 is arranged on the upper outer surface of the hydrogenation tower 1, and the air inlet 12 is located below the coalescer 10.

[0016] The hydrogenation reactor adopts the structure of the hydrogenation tower 1 and the separator technology, and the catalyst and the working liquid are caused to tumble and flow up and down inside the hydrogenation tower 1 by the power of hydrogen, thereby realizing the hydrogenation reaction. The hydrogenation tower 1 is equipped with a catalyst separator 7, which can effectively separate the hydrogenation liquid from the catalyst, ensure that the catalyst can be recycled, and at the same time improve the purity of the hydrogen peroxide.

[0017] The hydrogenation reaction is a hydrogenation reaction between alkyl anthraquinone and hydrogen under the action of a palladium catalyst to generate alkyl hydroanthraquinone, which is then oxidized to generate hydrogen peroxide.

[0018] The hydrogen distributor 3 is a pipe-type distributor, which is provided with a main pipe and a branch pipe. Small holes are opened downward at intervals of 30 degrees between the main pipe and the branch pipe. The main pipe and the branch pipe are connected by flanges and fixed on the tower bottom plane by brackets.

[0019] The working liquid distributor 5 is a tubular structure extending inward to the center of the tower and bending downward, and the lower end of the tube body is provided with small holes arranged in a circular manner.

[0020] Example 2

[0021] like Figure 1As shown, on the basis of Example 1, a hydrogenation reactor for producing hydrogen peroxide by anthraquinone method, the external pipeline includes a primary filter air pipeline 13, a primary filter air outlet 14 and a primary filter which are connected in sequence; the other end of the primary filter air pipeline 13 is connected to the air inlet 12 of the hydrogenation tower 1; a primary filter clear liquid outlet 16 is provided on the upper outer surface of the primary filter, and the primary filter clear liquid outlet 16 is connected to the interface of the subsequent process; a primary filter membrane separator 17 is provided in the middle of the primary filter; a primary filter hydrogenation liquid inlet 19 is provided on the lower outer surface of the primary filter, and the primary filter hydrogenation liquid inlet 19 is located below the primary filter membrane separator 17; the low / high position hydrogenation liquid outlet 9 of the hydrogenation tower 1 is connected to the primary filter hydrogenation liquid inlet 19 through the hydrogenation liquid outlet pipeline 18; a primary filter backwash outlet 20 is provided at the bottom of the primary filter, and the primary filter backwash outlet 20 is connected to the backwash reflux inlet 22 on the lower outer surface of the hydrogenation tower 1 through the backwash reflux pipeline 21.

[0022] Working process: The working liquid and hydrogen are continuously added into the fluidized bed. The hydrogen is evenly distributed through the distributor, pushing the catalyst and the working liquid to mix and move upward, resulting in a hydrogenation reaction.

[0023] The mixed solution after the reaction moves upward through the built-in catalyst separator 7, the separated hydrogenated liquid flows out of the reactor, and the catalyst remains in the reactor to continue to participate in the reaction.

[0024] The unreacted hydrogen entrains a small amount of working liquid and escapes from the liquid surface, and after being separated by the agglomerator 10, returns to the fluidized bed to participate in the reaction.

[0025] On the other hand, in order to ensure the continuous operation of the primary filter membrane separator 17, the membrane separator is backwashed regularly to remove the accumulation on the filter membrane.

[0026] The design of the hydrogenation reactor of the utility model fully utilizes the advantages of the hydrogenation tower 1 (fluidized bed) technology. Through the precisely and reasonably designed internal and external pipelines and distributors, the efficient distribution and utilization of hydrogen, catalyst and working fluid are realized. The internal arrangement design structure of the hydrogenation tower 1 ensures the uniform distribution of reactants and the full progress of the reaction, and also facilitates the recovery and reuse of the catalyst. The efficiency of the hydrogenation reaction and the quality of the hydrogen peroxide product are improved, while the production cost is reduced. Through the design of the built-in separator and the external circulation system, the continuous and stable operation of the reaction and separation is realized, which has a high industrial application value.

[0027] The above-mentioned embodiments only express the preferred implementation of the utility model, and the description thereof is relatively specific and detailed, but it cannot be understood as limiting the scope of the patent of the utility model. It should be pointed out that for ordinary technicians in this field, several modifications, improvements and substitutions can be made without departing from the concept of the utility model, which all belong to the protection scope of the utility model. Therefore, the protection scope of the utility model patent shall be based on the attached claims.

Claims

1. A hydrogenation reactor for producing hydrogen peroxide by anthraquinone process, characterized in that: The invention comprises a hydrogenation tower (1) and internal and external pipelines. The bottom outer surface of the hydrogenation tower (1) is provided with a hydrogen inlet (2); a hydrogen distributor (3) is provided on the bottom plane of the hydrogenation tower (1) and is connected to the hydrogen inlet (2) through the internal pipeline; a catalyst feeding port (4) is provided on the lower outer surface of the hydrogenation tower (1); a working liquid distributor (5) is provided at the lower part of the hydrogenation tower (1); a working liquid inlet (6) is provided on the lower outer surface of the hydrogenation tower (1) and is connected to the working liquid distributor (5) through the internal pipeline; the hydrogenation tower (1) is provided with a hydrogen inlet (7) and is connected to the hydrogen inlet (7) through the internal pipeline. ) is provided in the middle of the hydrogenation tower (1); a low-position hydrogenated liquid outlet (8) and a high-low-position hydrogenated liquid outlet (9) are provided on the outer surface of the middle part of the hydrogenation tower (1), both of which are located above the catalyst separator (7) and are used to extract hydrogenated liquid at different heights; a coalescer (10) is provided on the upper part of the hydrogenation tower (1) for merging liquid droplets; a gas outlet (11) is provided at the top of the hydrogenation tower (1); an air inlet (12) is provided on the outer surface of the upper part of the hydrogenation tower (1), and the air inlet (12) is located below the coalescer (10).

2. A hydrogenation reactor for producing hydrogen peroxide by anthraquinone process as claimed in claim 1, characterized in that: The external pipeline comprises a primary filter air pipeline (13), a primary filter air outlet (14) and a primary filter (15) which are connected in sequence; the other end of the primary filter air pipeline (13) is connected to the air inlet (12) of the hydrogenation tower (1); a primary filter clear liquid outlet (16) is provided on the upper outer surface of the primary filter (15), and the primary filter clear liquid outlet (16) is connected to the interface of the subsequent process; a primary filter membrane separator (17) is provided in the middle of the primary filter (15); a primary filter (15) is provided on the lower outer surface A primary filter hydrogenation liquid inlet (19) is located below the primary filter membrane separator (17); a low / high position hydrogenation liquid outlet (8, 9) of the hydrogenation tower (1) is connected to the primary filter hydrogenation liquid inlet (19) through a hydrogenation liquid outlet pipe (18); a primary filter backwash outlet (20) is provided at the bottom of the primary filter (15), and the primary filter backwash outlet (20) is connected to a backwash reflux inlet (22) on the lower outer surface of the hydrogenation tower (1) through a backwash reflux pipe (21).

3. A hydrogenation reactor for producing hydrogen peroxide by anthraquinone process as claimed in claim 1, characterized in that: The hydrogen distributor (3) is a pipe-type distributor, provided with a main pipe and a branch pipe, small holes are opened downward at intervals of 30 degrees below the main pipe and the branch pipe, and the main pipe and the branch pipe are connected by flanges and fixed on the tower bottom plane by a bracket.

4. A hydrogenation reactor for producing hydrogen peroxide by anthraquinone process as claimed in claim 1, characterized in that: The working liquid distributor (5) is a tubular structure extending inward to the center of the tower and bending downward, and the lower end of the tube body is provided with small holes arranged in a circular pattern.