Oxidation residual liquid recovery device for oxidation tower of hydrogen peroxide device

Abstract

The utility model discloses an oxidation residual liquid recovery device for an oxidation tower of a hydrogen peroxide device, which mainly comprises an oxidation tower, an extraction tower and a purification tower, and a hydrogen peroxide feeding pipeline is arranged at the bottom of a lower tower of the oxidation tower and is connected with an industrial-grade hydrogen peroxide pipeline at the bottom of the purification tower or a discharging pipeline at the bottom of the extraction tower; a lower tower residual liquid pipeline of the oxidation tower is connected with a bottom discharge pipeline of the extraction tower. According to the utility model, an oxidation residual liquid collecting tank is not arranged, but circulating hydrogen peroxide from the purification tower is utilized to continuously feed the oxidation tower residual liquid into the purification tower for purification and recovery, so that hydrogen peroxide decomposition caused by enrichment of impurities such as metal ions and the like due to long-time retention of the oxidation tower residual liquid in the oxidation tower can be avoided, and the safety of the system is improved.

Description

Technical Field

[0001] The utility model belongs to the technical field of chemical industry, and relates to a device for recovering residual oxidized liquid from an oxidation tower of a hydrogen peroxide device and application thereof in hydrogen peroxide production. Background Art

[0002] Hydrogen peroxide is an important inorganic chemical raw material. It is widely used in many fields such as papermaking, textiles, chemical synthesis, military industry, electronics, food processing, medicine, cosmetics, environmental protection, metallurgy, etc. Hydrogen peroxide produces water and oxygen after decomposition, which has no secondary pollution to the environment and is a green chemical. At present, the anthraquinone method is widely used to produce hydrogen peroxide at home and abroad. The anthraquinone method for producing hydrogen peroxide uses anthraquinone derivatives as working carriers. Under the action of palladium catalyst, hydrogen is used to hydrogenate anthraquinone derivatives dissolved in organic solvents to generate hydroanthraquinone. Then, hydroanthraquinone is oxidized by oxygen to generate hydrogen peroxide and anthraquinone derivatives. Finally, the hydrogen peroxide in the solvent is extracted with desalted water to obtain a certain concentration of hydrogen peroxide solution, which is then purified by aromatic hydrocarbons to obtain the product. The working solution containing anthraquinone derivatives and organic solvents is recycled after vacuum dehydration and regeneration of the kaolin bed.

[0003] After a long period of accumulation, the residual liquid at the bottom of the oxidation tower will be stratified and enriched with impurities such as metal ions. If it is not discharged in time, it will easily cause the decomposition of hydrogen peroxide and overpressure accidents in the oxidation tower. The residual liquid after discharge contains a large amount of impurities such as metal ions. If it is not properly handled, there is also a risk of decomposition and overpressure.

[0004] In order to reduce the above safety risks, a device and process for recovering residual liquid from oxidation tower was invented to achieve safe production and recover hydrogen peroxide at the same time. Utility Model Content

[0005] In order to overcome the deficiencies of the prior art, the utility model provides a process for recovering residual liquid from an oxidation tower of a hydrogen peroxide device. The device utilizes a purification tower to continuously process residual liquid from the oxidation tower, thereby avoiding the residual liquid from the oxidation tower from staying in the oxidation tower for a long time and improving the safety of the device.

[0006] The technical solution of this utility model:

[0007] A process for recovering oxidation residual liquid from an oxidation tower of a hydrogen peroxide device mainly comprises an oxidation tower, an extraction tower and a purification tower, wherein a hydrogenation liquid pipeline is connected to the lower part of an upper tower of the oxidation tower, a compressed air pipeline is respectively connected to the lower part of the upper tower of the oxidation tower and the lower part of the lower tower of the oxidation tower, the upper part of the upper tower of the oxidation tower is connected to the lower part of the lower tower of the oxidation tower, the lower part of the upper tower of the oxidation tower is connected to the upper part of the lower tower of the oxidation tower, an oxidation tail gas pipeline is connected to the upper part of the upper tower of the oxidation tower, an oxidation liquid discharge pipeline at the upper part of the lower tower of the oxidation tower is connected to an oxidation liquid receiving tank; the oxidation liquid receiving tank is connected to a centrifugal pump; the lower part of the extraction tower is connected to the centrifugal pump, a pure water pipeline is connected to the upper part of the extraction tower, a raffinate pipeline is connected to the upper part of the extraction tower, and the lower part of the extraction tower is connected to the upper part of the purification tower; a fresh aromatics pipeline is connected to the lower part of the purification tower, a recovered aromatics pipeline is connected to the upper part of the purification tower, and an industrial-grade hydrogen peroxide pipeline is connected to the lower part of the purification tower; a hydrogen peroxide feed pipeline is arranged at the bottom of the lower tower of the oxidation tower, and a residual liquid pipeline of the lower tower of the oxidation tower is connected to a discharge pipeline at the bottom of the extraction tower.

[0008] A hydrogen peroxide feeding pipeline is arranged at the bottom of the lower tower of the oxidation tower and is connected to the industrial-grade hydrogen peroxide pipeline at the bottom of the purification tower or to the discharging pipeline at the bottom of the extraction tower.

[0009] In the hydrogen peroxide device oxidation tower oxidation residual liquid recovery process, the hydrogenated liquid and the compressed air flow in parallel in the upper tower of the oxidation tower to undergo oxidation reaction, and then enter the lower tower of the oxidation tower to continue to flow in parallel with the compressed air to undergo oxidation reaction.

[0010] The hydrogen peroxide device oxidation tower oxidation residual liquid recovery device discharges the oxidation liquid from the upper part of the lower tower of the oxidation tower into the oxidation liquid receiving tank.

[0011] In the hydrogen peroxide device oxidation tower oxidation residual liquid recovery device, the oxidation liquid in the oxidation liquid receiving tank enters the lower part of the extraction tower through a centrifugal pump.

[0012] In the hydrogen peroxide device oxidation tower oxidation residual liquid recovery device, pure water and oxidation liquid are countercurrently extracted in the extraction tower, the raffinate flows out from the upper part of the extraction tower, and the crude hydrogen peroxide flows out from the lower part of the extraction tower.

[0013] In the hydrogen peroxide device oxidation tower oxidation residual liquid recovery device, aromatic hydrocarbons and crude hydrogen peroxide are countercurrently extracted in the purification tower, and the recovered aromatic hydrocarbons flow out from the upper part of the purification tower, and industrial-grade hydrogen peroxide flows out from the lower part of the purification tower.

[0014] The hydrogen peroxide device oxidation tower oxidation residual liquid recovery device purifies the industrial-grade hydrogen peroxide at the bottom of the tower and returns a stream to the lower tower of the oxidation tower.

[0015] The hydrogen peroxide device oxidation tower oxidation residual liquid recovery device, the oxidation residual liquid at the bottom of the oxidation tower enters the bottom of the extraction tower for discharge.

[0016] Application of oxidation tower oxidation residual liquid recovery process in hydrogen peroxide production:

[0017] The hydrogenated liquid from the hydrogenation process reacts with compressed air in the oxidation tower to generate an oxidation liquid containing 0.1-1.5% (mass fraction) hydrogen peroxide. After being buffered in the oxidation liquid receiving tank, the oxidation liquid is pressurized by a centrifugal pump and then countercurrently extracted with pure water in the extraction tower to obtain a 25-40% (mass fraction) crude hydrogen peroxide solution and a raffinate. The crude hydrogen peroxide and fresh aromatics are extracted in the purification tower to obtain industrial-grade hydrogen peroxide. The industrial-grade hydrogen peroxide at the bottom of the purification tower returns to the oxidation tower and enters the pipeline from the extraction tower to the purification tower together with the residual liquid of the oxidation tower.

[0018] The residence time of the oxidation tower is 10-20 minutes, the weight ratio of compressed air to oxidation liquid is 0.03-0.08, the temperature of the oxidation tower is 30-55°C, and the operating pressure is 0.05-0.6MPa.G.

[0019] The number of theoretical plates of the extraction tower is 10 to 60, the weight ratio of desalted water to oxidized liquid is 0.005 to 0.02, the temperature of the extraction tower is 45 to 55°C, the operating pressure is normal pressure, and the water content of the raffinate at the top of the extraction tower is 0.35 to 0.5%.

[0020] The number of theoretical plates of the purification tower is 3 to 15, the weight ratio of aromatic hydrocarbon to crude hydrogen peroxide is 0.03 to 0.05, the temperature of the purification tower is 20 to 40° C., and the operating pressure is normal pressure.

[0021] Compared with the prior art, the invented oxidation tower oxidation residual liquid recovery process utilizes a small amount of purified hydrogen peroxide to circulate the oxidation residual liquid to the purification tower for continuous recycling, thereby avoiding the accumulation of impurities such as metal ions in the oxidation residual liquid after a long period of residence in the oxidation tower. This not only recovers the hydrogen peroxide, but also improves the safety of the system. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 Schematic diagram of a hydrogen peroxide device oxidation tower oxidation residual liquid recovery device

[0023] In the figure: 1- oxidation tower, 2- oxidation liquid receiving tank, 3- centrifugal pump, 4- extraction tower, 5- purification tower

[0024] Figure 2 -Existing hydrogen peroxide plant process

[0025] In the figure: 1- oxidation tower, 2- oxidation liquid receiving tank, 3- centrifugal pump, 4- extraction tower, 5- purification tower DETAILED DESCRIPTION

[0026] The present invention will be further described below in conjunction with specific implementations and drawings, but the present invention is not limited to the following examples. Without departing from the scope of the aforementioned purpose, the implementation of changes should be included in the technical scope of the present invention.

[0027] Attached Figure 1The hydrogen peroxide device oxidation tower oxidation residual liquid recovery device shown is mainly composed of an oxidation tower (1), an extraction tower (4), and a purification tower (5).

[0028] Example 1

[0029] The hydrogenated liquid from the hydrogenation process reacts with compressed air in the oxidation tower to generate an oxidation liquid, which contains 0.1-1.5% (mass fraction) of hydrogen peroxide. The residence time of the oxidation tower is 10-20 minutes, and the weight ratio of compressed air to oxidation liquid is 0.03-0.08. The temperature of the oxidation tower is 30-55°C, and the operating pressure is 0.05-0.6MPa.G.

[0030] After the oxidation liquid is buffered in the oxidation liquid receiving tank, it is pressurized by a centrifugal pump and then countercurrently extracted with pure water in the extraction tower to obtain a 25-40% (mass fraction) crude hydrogen peroxide solution and a raffinate. The theoretical number of plates of the extraction tower is 10-60, and the weight ratio of desalted water to oxidation liquid is 0.005-0.02; the temperature of the extraction tower is 45-55°C, and the operating pressure is normal pressure. The water content of the raffinate at the top of the extraction tower is 0.35-0.5%.

[0031] The crude hydrogen peroxide with a concentration of 25-40% and a TOC of 200-800ppm sent from the extraction tower enters the purification tower at the upper part of the tower, and the aromatic hydrocarbons enter the purification tower from the lower part of the tower. The theoretical number of plates of the purification tower is 3-15, and the weight ratio of aromatic hydrocarbons to crude hydrogen peroxide is 0.03-0.05. The temperature of the purification tower is 20-40℃, and the operating pressure is normal pressure.

[0032] The hydrogen peroxide at the bottom of the purification tower is circulated back to the oxidation tower and enters the pipeline from the extraction tower to the oxidation tower together with the residual liquid of the oxidation tower. The weight ratio of the circulating hydrogen peroxide to the residual liquid of the oxidation tower is 1 to 10:1.

[0033] The implementation results show that compared with the existing technology, the residual liquid in the oxidation tower can be reduced by 5kg / ton of hydrogen peroxide, and the hydrogen peroxide yield can be improved.

[0034] Example 2

[0035] The rest is the same as in Example 1, except that the hydrogen peroxide pipeline arranged in the lower tower of the oxidation tower of the oxidation tower oxidation residual liquid recovery device of the hydrogen peroxide device is connected to the discharge pipeline at the bottom of the extraction tower, the hydrogen peroxide circulated to the lower tower of the oxidation tower comes from the hydrogen peroxide at the bottom of the extraction tower, and the weight ratio of the circulating hydrogen peroxide to the oxidation tower residual liquid is 1 to 10:1.

[0036] The implementation results show that compared with the existing technology, the residual liquid in the oxidation tower can be reduced by 5kg / ton of hydrogen peroxide, and the hydrogen peroxide yield can be improved.

[0037] Comparative Example

[0038] As attached Figure 2The conventional hydrogen peroxide concentration and purification device shown is mainly composed of an oxidation tower (1), an extraction tower (4), and a purification tower (5).

[0039] The hydrogenated liquid from the hydrogenation process reacts with compressed air in the oxidation tower to generate an oxidation liquid, which contains 0.1-1.5% (mass fraction) of hydrogen peroxide. The residence time of the oxidation tower is 10-20 minutes, and the weight ratio of compressed air to oxidation liquid is 0.03-0.08. The temperature of the oxidation tower is 30-55°C, and the operating pressure is 0.05-0.6MPa.G.

[0040] After the oxidation liquid is buffered in the oxidation liquid receiving tank, it is pressurized by a centrifugal pump and then countercurrently extracted with pure water in the extraction tower to obtain a 25-40% (mass fraction) crude hydrogen peroxide solution and a raffinate. The theoretical number of plates of the extraction tower is 5-50, and the weight ratio of desalted water to oxidation liquid is 0.005-0.02; the extraction tower temperature is 45-55°C, and the operating pressure is atmospheric pressure. The water content of the raffinate at the top of the extraction tower is 0.35-0.5%.

[0041] The concentration of crude hydrogen peroxide sent from the extraction tower is 35%, and the TOC is 200-800ppm. It enters the purification tower at the upper part of the tower, and aromatic hydrocarbons enter the purification tower from the lower part of the tower. The theoretical number of plates of the purification tower is 3-15, and the weight ratio of aromatic hydrocarbons to crude hydrogen peroxide is 0.03-0.05. The temperature of the purification tower is 20-40℃, and the operating pressure is normal pressure.

[0042] The implementation results show that 5kg / ton of hydrogen peroxide is produced per hour as residual liquid in the oxidation tower.

Claims

1. A hydrogen peroxide device oxidation tower oxidation residual liquid recovery device, mainly composed of an oxidation tower (1), an extraction tower (4), and a purification tower (5), wherein a hydrogenated liquid pipeline is connected to the lower part of the upper tower of the oxidation tower (1), a compressed air pipeline is connected to the lower part of the upper tower of the oxidation tower (1) and the lower part of the lower tower of the oxidation tower (1), respectively, the upper part of the oxidation tower (1) is connected to the lower part of the lower tower of the oxidation tower (1), the lower part of the upper tower of the oxidation tower (1) is connected to the upper part of the lower tower of the oxidation tower (1), the oxidation tail gas pipeline is connected to the upper part of the upper tower of the oxidation tower (1), and the oxidation tower (1) The oxidized liquid discharge pipe at the upper part of the lower tower is connected to the oxidized liquid receiving tank (2); the oxidized liquid receiving tank (2) is connected to the centrifugal pump (3); the lower part of the extraction tower (4) is connected to the centrifugal pump (3), the pure water pipe is connected to the upper part of the extraction tower (4), the raffinate pipe is connected to the upper part of the extraction tower (4), the lower part of the extraction tower (4) is connected to the upper part of the purification tower (5); the fresh aromatics pipe is connected to the lower part of the purification tower (5), the aromatics recovery pipe is connected to the upper part of the purification tower (5), and the industrial-grade hydrogen peroxide pipe is connected to the lower part of the purification tower (5); characterized in that A hydrogen peroxide feeding pipeline is arranged at the bottom of the lower tower of the oxidation tower (1), and the residual liquid pipeline of the lower tower of the oxidation tower (1) is connected to the discharge pipeline at the bottom of the extraction tower (4).

2. The hydrogen peroxide device oxidation tower oxidation residual liquid recovery device according to claim 1, characterized in that A hydrogen peroxide feed pipeline is arranged at the bottom of the lower tower of the oxidation tower (1) and is connected to the industrial-grade hydrogen peroxide pipeline at the bottom of the purification tower (5) or to the discharge pipeline at the bottom of the extraction tower (4).

3. The hydrogen peroxide device oxidation tower oxidation residual liquid recovery device according to claim 1, characterized in that The oxidizing liquid is discharged from the upper part of the lower tower of the oxidation tower (1) and enters the oxidizing liquid receiving tank.

4. The hydrogen peroxide device oxidation tower oxidation residual liquid recovery device according to claim 1, characterized in that The oxidizing liquid in the oxidizing liquid receiving tank (2) enters the lower part of the extraction tower (4) through a centrifugal pump.

5. The hydrogen peroxide device oxidation tower oxidation residual liquid recovery device according to claim 1 is characterized in that Pure water and oxidizing liquid are extracted in a countercurrent manner in the extraction tower (4), the raffinate flows out from the upper part of the extraction tower (4), and the crude hydrogen peroxide flows out from the lower part of the extraction tower (4).

6. The hydrogen peroxide device oxidation tower oxidation residual liquid recovery device according to claim 1, characterized in that Aromatic hydrocarbons and crude hydrogen peroxide are countercurrently extracted in a purification tower (5), and recovered aromatic hydrocarbons flow out from the upper part of the purification tower (5), while industrial-grade hydrogen peroxide flows out from the lower part of the purification tower (5).

7. The hydrogen peroxide device oxidation tower oxidation residual liquid recovery device according to claim 1 is characterized in that A stream of industrial-grade hydrogen peroxide from the bottom of the purification tower (5) is returned to the lower tower of the oxidation tower (1).

8. The hydrogen peroxide device oxidation tower oxidation residual liquid recovery device according to claim 1 is characterized in that The oxidation residual liquid at the bottom of the oxidation tower (1) enters the discharge pipe at the bottom of the extraction tower.

9. The hydrogen peroxide device oxidation tower oxidation residual liquid recovery device according to claim 1, characterized in that The extraction tower (4) has a theoretical plate number of 10-60.

10. The hydrogen peroxide device oxidation tower oxidation residual liquid recovery device according to claim 1, characterized in that The purification tower (5) has a theoretical number of plates of 3 to 15.

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