Production system for preparing hydrogen peroxide by using fluidized bed hydrogenation anthraquinone method

Abstract

The utility model belongs to the technical field of hydrogen peroxide production, and particularly relates to a production system for preparing hydrogen peroxide by a fluidized bed hydrogenation anthraquinone method, which comprises a hydrogenation reactor, an oxidation tower, an extraction tower, a purification tower and a hydrogen peroxide storage tank, and is internally provided with a first regeneration tower, a second regeneration tower and a standby regeneration tower, the input end of the standby regeneration tower is respectively connected with the output end of the hydrogenation reactor and the output end of the flash tower, and the output end of the standby regeneration tower is respectively connected with the input end of the filter and the input end of the hydrogenation reactor. According to the utility model, the standby regeneration tower is additionally arranged to temporarily replace the regeneration tower to be replaced, so that the whole hydrogen peroxide production system does not need to be frequently started and stopped, the energy loss is avoided, and the production efficiency is improved.

Description

Technical Field

[0001] The utility model belongs to the technical field of hydrogen peroxide production, and particularly relates to a production system for preparing hydrogen peroxide by a fluidized bed hydrogenation anthraquinone method. Background Art

[0002] The anthraquinone process is currently the world's predominant method for producing hydrogen peroxide. It utilizes the property of quinones that can be hydrogenated and reduced to their original form. Using alkyl anthraquinone derivatives as carriers, they are hydrogenated over a palladium catalyst and then oxidized to produce hydrogen peroxide. Currently, the anthraquinone process with palladium catalysts is categorized into two different types: fixed-bed and fluidized-bed hydrogenation, depending on the hydrogenation method. Fluidized-bed hydrogenation offers numerous advantages, including uniform reaction, high safety, and high hydrogenation efficiency, making it the predominant method for producing hydrogen peroxide.

[0003] However, the fluidized bed anthraquinone hydrogenation method generates a large number of by-products during the hydrogenation and oxidation reactions. In order to convert the by-products into effective anthraquinones that can be used to produce hydrogen peroxide, activated alumina must be used for regeneration. Due to the large amount of by-products generated, the regeneration tower needs to be frequently replenished with activated alumina. In addition, the regeneration tower needs to be cooled each time the activated alumina is replaced. Therefore, the entire hydrogen peroxide production system needs to be shut down for a period of time. The frequent start and stop of the production system not only causes a large amount of energy loss, but also reduces production efficiency. Utility Model Content

[0004] In order to solve the problems existing in the above-mentioned prior art, the utility model provides a production system for preparing hydrogen peroxide by the anthraquinone hydrogenation method in a fluidized bed. By adding a spare regeneration tower, when the first regeneration tower or the second regeneration tower needs to replace the activated alumina, the spare regeneration tower is used to temporarily replace the regeneration tower to be replaced, thereby eliminating the need for frequent start and stop of the entire hydrogen peroxide production system, avoiding energy loss and improving production efficiency.

[0005] The specific technical solution adopted in this utility model is:

[0006] A production system for preparing hydrogen peroxide by a fluidized bed hydrogenation anthraquinone process comprises a hydrogenation reactor, an oxidation tower, an extraction tower, a purification tower, and a hydrogen peroxide storage tank connected in sequence. The input end of the hydrogenation reactor is connected to the output end of the hydrogen storage tank, the oxidation tower is also connected to an air compressor, a flash tower is provided between the extraction tower and the hydrogenation reactor, a first regeneration tower, a second regeneration tower, and a spare regeneration tower are provided in the production system, a filter is provided between the hydrogen reactor and the oxidation tower, the input end of the first regeneration tower is connected to the output end of the hydrogenation reactor, the output end of the first regeneration tower is connected to the input end of the filter, the input end of the second regeneration tower is connected to the output end of the flash tower, the output end of the second regeneration tower is connected to the input end of the hydrogenation reactor, the input end of the spare regeneration tower is respectively connected to the output end of the hydrogenation reactor and the output end of the flash tower, and the output end of the spare regeneration tower is respectively connected to the input end of the filter and the input end of the hydrogenation reactor.

[0007] The input end of the first regeneration tower is provided with a first stop valve, the input end of the second regeneration tower is provided with a second stop valve, the input end between the standby regeneration tower and the output end of the hydrogenation reactor is provided with a third stop valve, the input end between the standby regeneration tower and the output end of the flash tower is provided with a fourth stop valve, the input end between the standby regeneration tower and the input end of the filter is provided with a fifth stop valve, and the output end between the standby regeneration tower and the input end of the hydrogenation reactor is provided with a sixth stop valve.

[0008] The output end of the first regeneration tower and the output end of the standby regeneration tower are respectively connected to the hydrogenation reactor via a heat exchanger. The regeneration liquid is heated by the heat exchanger and enters the hydrogenation reactor for reaction.

[0009] The exhaust end of the hydrogenation reactor is provided with a gas-liquid separator, the liquid phase output end of the gas-liquid separator is connected to the solvent storage tank, and the gas phase output end of the gas-liquid separator is connected to the hydrogenation reactor via a hydrogen circulation compressor.

[0010] The output end of the oxidation tower is provided with a refrigeration recovery device, the gas phase output end of the refrigeration recovery device is connected to the tail gas treatment system, the liquid phase output end of the refrigeration recovery device is connected to the solvent separator, the water phase output end of the solvent separator is connected to the input end of the extraction tower, and the organic phase output end of the solvent separator is connected to the solvent storage tank.

[0011] A resin tower is further provided between the purification tower and the hydrogen peroxide storage tank. The crude hydrogen peroxide outputted from the output end of the purification tower is purified by the resin tower and converted into refined hydrogen peroxide which flows into the hydrogen peroxide storage tank.

[0012] The resin tower includes a first-stage resin tower, a secondary resin tower and a final resin tower connected in series. A valve group is provided between the first-stage resin tower, the secondary resin tower and the final resin tower. The first-stage resin tower, the secondary resin tower and the final resin tower form two towers in series for adsorption with the help of the valve group.

[0013] The beneficial effects of the utility model are:

[0014] The utility model is provided with a spare regeneration tower. When the first regeneration tower or the second regeneration tower needs to replace the activated alumina, the spare regeneration tower is used to temporarily replace the regeneration tower to be replaced. After the regeneration tower to be replaced is cooled and the activated alumina is replaced, the spare regeneration tower is replaced again. Therefore, there is no need to frequently start and stop the entire hydrogen peroxide production system, thereby avoiding energy loss and improving production efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 This is a schematic diagram of the process flow of the utility model;

[0016] Figure 2 This is a schematic diagram of the process flow for purifying crude hydrogen peroxide in a resin tower. DETAILED DESCRIPTION

[0017] The present invention will be further described below with reference to the accompanying drawings and specific embodiments:

[0018] A production system for preparing hydrogen peroxide by a fluidized bed hydrogenation anthraquinone process comprises a hydrogenation reactor, an oxidation tower, an extraction tower, a purification tower, and a hydrogen peroxide storage tank connected in sequence. The input end of the hydrogenation reactor is connected to the output end of the hydrogen storage tank, the oxidation tower is also connected to an air compressor, a flash tower is provided between the extraction tower and the hydrogenation reactor, a first regeneration tower, a second regeneration tower, and a spare regeneration tower are provided in the production system, a filter is provided between the hydrogen reactor and the oxidation tower, the input end of the first regeneration tower is connected to the output end of the hydrogenation reactor, the output end of the first regeneration tower is connected to the input end of the filter, the input end of the second regeneration tower is connected to the output end of the flash tower, the output end of the second regeneration tower is connected to the input end of the hydrogenation reactor, the input end of the spare regeneration tower is respectively connected to the output end of the hydrogenation reactor and the output end of the flash tower, and the output end of the spare regeneration tower is respectively connected to the input end of the filter and the input end of the hydrogenation reactor.

[0019] The fluidized bed anthraquinone hydrogenation process generates a large number of by-products during the hydrogenation and oxidation reactions. In order to convert the by-products into effective anthraquinones that can be used to produce hydrogen peroxide, activated alumina must be used for regeneration. Due to the large amount of by-products generated, the regeneration tower needs to be frequently replenished with activated alumina. In addition, the regeneration tower needs to be cooled each time the activated alumina is replaced. Therefore, the entire hydrogen peroxide production system needs to be shut down for a period of time. The frequent start and stop of the production system not only causes a large amount of energy loss, but also reduces production efficiency.

[0020] Therefore, a spare regeneration tower is added in the utility model. When the first regeneration tower or the second regeneration tower needs to replace the activated alumina, the spare regeneration tower is used to temporarily replace the regeneration tower to be replaced. After the regeneration tower to be replaced is cooled and the activated alumina is replaced, the spare regeneration tower is replaced again. Therefore, there is no need to frequently start and stop the entire hydrogen peroxide production system, which avoids energy loss and improves production efficiency.

[0021] The input end of the first regeneration tower is provided with a first stop valve, the input end of the second regeneration tower is provided with a second stop valve, the input end between the standby regeneration tower and the output end of the hydrogenation reactor is provided with a third stop valve, the input end between the standby regeneration tower and the output end of the flash tower is provided with a fourth stop valve, the input end between the standby regeneration tower and the input end of the filter is provided with a fifth stop valve, and the output end between the standby regeneration tower and the input end of the hydrogenation reactor is provided with a sixth stop valve.

[0022] When the activated alumina in the first regeneration tower needs to be replaced, the first stop valve, the fourth stop valve and the sixth stop valve are closed, and the second stop valve, the third stop valve and the fifth stop valve are opened;

[0023] When the activated alumina in the first regeneration tower is replaced, the third stop valve, the fourth stop valve, the fifth stop valve and the sixth stop valve are closed, and the first stop valve and the second stop valve are opened;

[0024] When the second regeneration tower needs to replace the activated alumina, the second stop valve, the third stop valve and the fifth stop valve are closed, and the first stop valve, the fourth stop valve and the sixth stop valve are opened;

[0025] After the activated alumina in the second regeneration tower is replaced, the third stop valve, the fourth stop valve, the fifth stop valve and the sixth stop valve are closed, and the first stop valve and the second stop valve are opened.

[0026] The output end of the first regeneration tower and the output end of the standby regeneration tower are respectively connected to the hydrogenation reactor via a heat exchanger. The regeneration liquid is heated by the heat exchanger and enters the hydrogenation reactor for reaction. The activity of the catalyst in the regeneration liquid decreases after use. Therefore, in order to ensure the hydrogenation efficiency, it is necessary to use a heat exchanger to heat the catalyst to reach the reaction activity temperature, thereby increasing the reaction activity of the catalyst and ensuring the concentration of the hydrogen peroxide extracted by the extraction tower. In addition, a hydrogenation liquid tank is provided at the outlet of the hydrogenation reactor. The regeneration liquid enters and exits the hydrogenation reactor through the hydrogenation liquid tank and is not directly connected to the hydrogenation reactor to avoid causing aluminum oxide powder to be brought into the hydrogenation reactor and affecting the activity of the catalyst.

[0027] The exhaust end of the hydrogenation reactor is equipped with a gas-liquid separator. The liquid phase output end of the gas-liquid separator is connected to the solvent storage tank, and the gas phase output end of the gas-liquid separator is connected to the hydrogenation reactor via a hydrogen recycle compressor. The tail gas of the hydrogenation reactor contains a large amount of hydrogen, so a hydrogen recycle compressor is provided. The gas at the top of the hydrogenation reactor passes through the gas-liquid separator to remove entrained liquid, then enters the hydrogen recycle compressor for compression and recirculation, returning to the hydrogenation reactor to achieve hydrogen recovery and reuse.

[0028] In addition, the hydrogenated liquid at the output end of the hydrogenation reactor carries a certain amount of catalyst. Therefore, before the hydrogenated liquid enters the oxidation tower feed tank, the catalyst must be filtered and backwashed back to the hydrogenation reactor using a filter. The hydrogenated liquid flows from the outside of the filter element into the inside of the filter element, and the catalyst entrained in the hydrogenated liquid is collected on the outside of the filter element. The first-level filter is backwashed by a backwash pump, and the catalyst outside the filter element is backwashed into the hydrogenation reactor to continue to participate in the hydrogenation reaction.

[0029] The output end of the oxidation tower is equipped with a refrigeration recovery device. The gas phase output end of the refrigeration recovery device is connected to the exhaust gas treatment system, the liquid phase output end of the refrigeration recovery device is connected to the solvent separator, the aqueous phase output end of the solvent separator is connected to the input end of the extraction tower, and the organic phase output end of the solvent separator is connected to the solvent storage tank. The exhaust gas after condensation and recovery enters the factory's exhaust gas treatment system for unified treatment. The refrigeration recovery device is a condenser, and the solvent storage tank is connected to the working waste liquid treatment system. It is discharged uniformly after sewage treatment with other waste liquids in the factory. Because the exhaust gas from the oxidation tower contains a certain amount of hydrogen peroxide, the hydrogen peroxide is recovered by the refrigeration recovery device and the solvent separator.

[0030] A resin tower is also located between the purification tower and the hydrogen peroxide storage tank. The crude hydrogen peroxide output from the purification tower is purified by the resin tower and converted into refined hydrogen peroxide, which flows into the hydrogen peroxide storage tank. The crude hydrogen peroxide product from the purification tower typically has a TOC content of 150-350 ppm, which must be reduced to below 100 ppm through purification. The present invention utilizes an antioxidant adsorption resin to adsorb and purify the crude hydrogen peroxide.

[0031] The resin tower includes a primary resin tower, a secondary resin tower, and a final resin tower connected in series. A valve group is provided between the primary, secondary, and final resin towers, forming a two-tower series adsorption system. The valve group includes stop valves A, B, C, D, E, F, and G. Because the resin in the resin towers needs to be replaced, the valve group is provided to connect the primary, secondary, and final resin towers in series, facilitating resin replacement within the resin towers.

[0032] When the resin in the first-stage resin tower needs to be replaced, stop valve B, stop valve E, and stop valve G are opened; stop valve A, stop valve C, stop valve D, and stop valve F are closed;

[0033] When the secondary resin tower needs to replace the resin, stop valve A, stop valve D, and stop valve G are opened; stop valve B, stop valve C, stop valve E, and stop valve F are closed;

[0034] When the resin in the final resin tower needs to be replaced, stop valve A, stop valve C, and stop valve F are opened; stop valve B, stop valve D, stop valve E, and stop valve G are closed.

Claims

1. A production system for preparing hydrogen peroxide by anthraquinone hydrolysis in a fluidized bed, comprising a hydrogenation reactor, an oxidation tower, an extraction tower, a purification tower, and a hydrogen peroxide storage tank connected in sequence, wherein the input end of the hydrogenation reactor is connected to the output end of the hydrogen storage tank, the oxidation tower is further connected to an air compressor, and a flash tower is provided between the extraction tower and the hydrogenation reactor, characterized in that: The production system is provided with a first regeneration tower, a second regeneration tower and a spare regeneration tower. A filter is provided between the hydrogenation reactor and the oxidation tower. The input end of the first regeneration tower is connected to the output end of the hydrogenation reactor, the output end of the first regeneration tower is connected to the input end of the filter, the input end of the second regeneration tower is connected to the output end of the flash tower, the output end of the second regeneration tower is connected to the input end of the hydrogenation reactor, the input end of the spare regeneration tower is respectively connected to the output end of the hydrogenation reactor and the output end of the flash tower, and the output end of the spare regeneration tower is respectively connected to the input end of the filter and the input end of the hydrogenation reactor.

2. The production system for preparing hydrogen peroxide by the fluidized bed hydroanthraquinone method according to claim 1, characterized in that: The input end of the first regeneration tower is provided with a first stop valve, the input end of the second regeneration tower is provided with a second stop valve, the input end between the standby regeneration tower and the output end of the hydrogenation reactor is provided with a third stop valve, the input end between the standby regeneration tower and the output end of the flash tower is provided with a fourth stop valve, the input end between the standby regeneration tower and the input end of the filter is provided with a fifth stop valve, and the output end between the standby regeneration tower and the input end of the hydrogenation reactor is provided with a sixth stop valve.

3. The production system for preparing hydrogen peroxide by the fluidized bed hydroanthraquinone method according to claim 1, characterized in that: The output end of the first regeneration tower and the output end of the standby regeneration tower are respectively connected to the hydrogenation reactor via a heat exchanger. The regeneration liquid is heated by the heat exchanger and enters the hydrogenation reactor for reaction.

4. The production system for preparing hydrogen peroxide by the fluidized bed hydroanthraquinone method according to claim 1, characterized in that: The exhaust end of the hydrogenation reactor is provided with a gas-liquid separator, the liquid phase output end of the gas-liquid separator is connected to the solvent storage tank, and the gas phase output end of the gas-liquid separator is connected to the hydrogenation reactor via a hydrogen circulation compressor.

5. The production system for preparing hydrogen peroxide by the fluidized bed hydroanthraquinone method according to claim 4, characterized in that: The output end of the oxidation tower is provided with a refrigeration recovery device, the gas phase output end of the refrigeration recovery device is connected to the tail gas treatment system, the liquid phase output end of the refrigeration recovery device is connected to the solvent separator, the water phase output end of the solvent separator is connected to the input end of the extraction tower, and the organic phase output end of the solvent separator is connected to the solvent storage tank.

6. The production system for preparing hydrogen peroxide by the fluidized bed hydroanthraquinone method according to claim 1, characterized in that: A resin tower is further provided between the purification tower and the hydrogen peroxide storage tank. The crude hydrogen peroxide outputted from the output end of the purification tower is purified by the resin tower and converted into refined hydrogen peroxide which flows into the hydrogen peroxide storage tank.

7. The production system for preparing hydrogen peroxide by the fluidized bed anthraquinone hydrotreatment method according to claim 6, characterized in that: The resin tower includes a first-stage resin tower, a secondary resin tower and a final resin tower connected in series. A valve group is provided between the first-stage resin tower, the secondary resin tower and the final resin tower. The first-stage resin tower, the secondary resin tower and the final resin tower form two towers in series for adsorption with the help of the valve group.

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