A purifying and recycling device for working solution of hydrogen peroxide

Abstract

The utility model discloses a kind of purification and recovery device of working solution for hydrogen peroxide, including cleaning kettle, cleaning kettle is equipped with pure water inlet, lye inlet, working solution inlet and slag outlet, slag outlet connects first sewage pool;Pure water tank and lye tank are communicated with pure water inlet and lye inlet respectively;Alkali separator is equipped with lye inlet, lye outlet and lye discharge port;Two ends of filter are communicated with cleaning kettle and lye inlet respectively;Water scrubbing tower is equipped with treatment liquid inlet, treatment liquid outlet and drain, drain connects second sewage pool, treatment liquid inlet is communicated with lye outlet;Water separator is communicated with treatment liquid outlet, and water separator is connected with third sewage pool and working solution recovery device;Control unit is electrically connected with cleaning kettle, pure water tank and lye tank, alkali separator, filter, water scrubbing tower and water separator respectively.The utility model can automatically recover after removing alkali of working solution, improve processing efficiency, and alkali residual amount≤0.05%.

Description

Technical Field

[0001] This utility model relates to the field of waste liquid recycling technology, and in particular to a purification and recycling device for working fluid used in hydrogen peroxide. Background Technology

[0002] With the rapid development of the electronics industry, especially the increasing integration of integrated circuits, the demand for electronic-grade hydrogen peroxide has grown dramatically. During the production of hydrogen peroxide, a working fluid composed of heavy aromatics and trioctyl phosphate is used as a carrier. After recycling, this working fluid accumulates impurities such as organic matter from degradation. These impurities not only affect the efficiency and quality of subsequent hydrogen peroxide production but may also pose safety hazards. Therefore, the working fluid must be periodically regenerated and purified.

[0003] Existing technologies typically involve adding the working solution to the reactor in batches, followed by multiple intermittent steps such as alkali washing, settling and stratification, slag removal, water washing, and further settling and stratification. However, after use, it was found that this method is not only inefficient and costly, but also prone to incomplete alkali residue washing due to its reliance on long settling and separation times and multiple manual or semi-automatic operations, posing a serious safety hazard. Furthermore, manual operation results in inconsistent quality that fails to meet usage requirements. Utility Model Content

[0004] The purpose of this invention is to overcome the shortcomings of the prior art by providing a purification and recovery device for hydrogen peroxide working fluid, which has low cost, high recovery efficiency and high purification degree.

[0005] To achieve the above objectives, the technical solution adopted by this utility model is: a purification and recovery device for hydrogen peroxide working fluid, comprising:

[0006] A cleaning vessel is provided with a pure water inlet, an alkaline solution inlet, a working fluid inlet, and a slag discharge port. The slag discharge port is connected to a first sewage tank. The cleaning vessel is used to stir and heat the liquid inside it.

[0007] The pure water tank and the alkali solution tank are respectively connected to the pure water inlet and the alkali solution inlet;

[0008] An alkali separator, which has an alkali inlet, an alkali outlet, and an alkali discharge port;

[0009] A filter, the two ends of which are respectively connected to the cleaning tank and the alkali inlet;

[0010] A water washing tower has a water washing inlet, a treatment liquid inlet, a treatment liquid outlet, and a drain outlet. The drain outlet is connected to a second wastewater tank, and the treatment liquid inlet is connected to the alkaline solution outlet.

[0011] A water separator, which is connected to the outlet of the treated liquid, and a third wastewater tank and a working liquid recovery device are connected to the water separator;

[0012] The control unit is electrically connected to the cleaning tank, pure water tank, alkali tank, alkali separator, filter, water washing tower and water separator, respectively.

[0013] Furthermore, the bottom of the washing vessel has a conical structure, and the slag discharge port is located at the bottom of the washing vessel.

[0014] Furthermore, the pure water inlet, alkali solution inlet, and working fluid inlet are all located at the top of the cleaning tank.

[0015] Furthermore, it also includes a phosphoric acid addition unit connected to the water separator.

[0016] Furthermore, the treatment liquid inlet of the water washing tower is located at the bottom of the tower body, and the treatment liquid outlet is located at the top of the tower body.

[0017] Furthermore, the alkali outlet is connected to the alkali tank.

[0018] Furthermore, the water inlet in the water washing tower is connected to the pure water tank.

[0019] Furthermore, the control unit is a DCS system or a PLC system.

[0020] Due to the application of the above technical solution, this utility model has the following advantages compared with the prior art:

[0021] This utility model discloses a purification and recovery device for hydrogen peroxide working fluid. It can automatically remove impurities from the working fluid in a washing tank, filter, remove alkali in an alkali separator and a secondary alkali removal in a water washing tower, and then completely remove the alkali in the working fluid through an acid addition unit for recovery. This eliminates manual steps and improves the working fluid treatment efficiency by more than 40% compared to existing processes. The automated control method ensures that the purity of the working fluid is stably maintained above 98%, and the final pH of the working fluid is stable in the neutral range with a residual alkali content of ≤0.05%. This avoids various safety risks and meets the high purity requirements of electronic-grade hydrogen peroxide production for the working fluid. Attached Figure Description

[0022] The technical solution of this utility model will be further described below with reference to the accompanying drawings:

[0023] Figure 1 This is a three-dimensional structural diagram of an embodiment of the present utility model;

[0024] Figure 2 for Figure 1 Enlarged view of part A in the image;

[0025] Figure 3 This is a schematic diagram of the structure connecting the water washing tower and the water separator in one embodiment of the present invention;

[0026] The system includes: a cleaning tank 1, a pure water inlet 10, an alkali inlet 11, a working fluid inlet 12, a slag discharge outlet 13, a first sewage tank 14, a pure water tank 2, an alkali tank 3, an alkali separator 4, an alkali inlet 40, an alkali outlet 41, and an alkali discharge outlet 42; a filter 5, a water washing tower 6, a treatment fluid inlet 60, a treatment fluid outlet 61, a drain outlet 62, a second sewage tank 63, a water washing inlet 64, a water separator 7, a third sewage tank 70, a working fluid recovery device 71, and a phosphoric acid addition unit 8. Detailed Implementation

[0027] To enable those skilled in the art to better understand the present application, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present application, and not all embodiments. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative effort should fall within the scope of protection of the present application.

[0028] This invention provides a purification and recovery device for hydrogen peroxide working fluid, which solves the problems of intermittent manual or semi-automatic recovery of hydrogen peroxide working fluid in the prior art, as well as incomplete recovery of alkali and low recovery efficiency.

[0029] For ease of understanding, the specific processes in the embodiments of this application are described below. Please refer to [link / reference]. Figures 1 to 3 A purification and recovery device for working fluid of hydrogen peroxide in this application embodiment includes a cleaning tank 1, a pure water tank 2, an alkali tank 3, an alkali separator 4, a filter 5, a water washing tower 6, a water separator 7, and a control unit.

[0030] See Figure 2 The cleaning tank 1 is equipped with a pure water inlet 10, an alkali inlet 11, a working fluid inlet 12, and a slag discharge port 13. The pure water inlet 10 and the alkali inlet 11 are respectively connected to the pure water tank 2 and the alkali tank 3, so that pure water and alkali can enter the interior of the cleaning tank 1. The slag discharge port 13 is connected to the first sewage tank 14 for collecting and subsequently treating the waste residue and wastewater generated in the cleaning tank 1.

[0031] Furthermore, the bottom of the washing vessel 1 has a conical structure, and the slag discharge port 13 is located at the bottom of the washing vessel 1. This structure facilitates the accumulation and smooth discharge of residue from the bottom of the washing vessel 1.

[0032] Furthermore, the pure water inlet 10, the alkali inlet 11, and the working fluid inlet 12 are all located at the top of the cleaning tank 1. This structure facilitates the uniform mixing of pure water flowing in from the pure water inlet 10, alkali solution flowing in from the alkali inlet 11, and working fluid to be recovered flowing in from the working fluid inlet 12 within the cleaning tank 1. The cleaning tank 1 is equipped with a stirring and heating device. Stirring allows the pure water, alkali solution, and working fluid to come into full contact and react, while heating accelerates the reaction process and improves fluidity.

[0033] The alkali separator 4 has an alkali inlet 40, an alkali outlet 41, and an alkali discharge port 42. The function of the alkali separator 4 is to use the density difference of each component in the mixture to separate them by gravity sedimentation. The alkali-water phase with a higher density settles to the bottom and is discharged through the alkali discharge port 42, while the working liquid with a lower density is discharged from the alkali outlet 41.

[0034] Furthermore, the alkali outlet 42 can be connected to the alkali tank 3, thereby enabling partial recycling of the alkali and reducing costs.

[0035] The inlet of filter 5 is connected to the outlet of the cleaning vessel 1 to receive the working liquid after preliminary mixing and cleaning in the cleaning vessel 1. The outlet is connected to the alkali inlet 40 of the alkali separator 4, thereby sending the filtered working liquid into the alkali separator 4. The function of filter 5 is to intercept and remove small solid particles carried out from the cleaning vessel 1, preventing them from entering subsequent precision equipment and causing blockage or wear, thus playing a coarse filtration role.

[0036] See Figure 1 and Figure 3 The water washing tower 6 receives the working liquid flowing out of the alkali outlet 41 of the alkali separator 4. The water washing tower 6 has a water washing inlet 64, a treated liquid inlet 60, a treated liquid outlet 61, and a drain outlet 62. The drain outlet 62 is connected to a second wastewater tank 63 for discharging impurities. The treated liquid inlet 60 communicates with the alkali outlet 41 and is used to receive the working liquid separated by the alkali separator.

[0037] The treatment liquid inlet 60 of the water washing tower is located at the bottom of the tower body, and the treatment liquid outlet 61 is located at the top of the tower body. In this way, the working liquid flowing out of the alkali outlet 41 enters the water washing tower 6 through the treatment liquid inlet 60. The liquid slowly rises from the bottom of the tower to the top, while the cleaning water flowing into the water washing tower 6 through the water washing inlet 64 slowly permeates downward from the top of the tower. The two form a "counter-current cross-flow" in the tower, and the contact time is extended by more than 30% compared with the co-current mode. This allows the cleaning water to fully dissolve the trace amounts of alkali remaining in the working liquid and avoids the alkali not being discharged from the second sewage tank 63 with the clean water due to insufficient contact time.

[0038] Furthermore, the water inlet 64 in the water washing tower 6 is connected to the pure water tank to introduce fresh cleaning pure water.

[0039] The water separator 7 is connected to the treated liquid outlet 61, and a third wastewater tank 70 and a working liquid recovery device 71 are connected to the water separator 7. The treated liquid flowing out of the treated liquid outlet 61 of the water washing tower 6 enters the water separator 7. The function of the water separator 7 is to completely separate the trace amounts of water that may be entrained after multiple purification steps from the final qualified treated liquid. The small amount of wastewater separated is discharged into the third wastewater tank 70; the separated pure treated liquid enters the working liquid recovery device 71, such as a storage tank, waiting to be returned to the production system for recycling.

[0040] Furthermore, to adjust the pH of the purified treatment solution and ensure it is the required weakly acidic level to meet production process requirements, this recovery device also includes a phosphoric acid addition unit 8. This phosphoric acid addition unit is connected to the water separator 7 and precisely injects a small amount of phosphoric acid as needed to fine-tune the pH value of the purified treatment solution.

[0041] Secondly, the entire recycling unit is controlled by a control unit, which can be an automatic control system such as a DCS system or a PLC system. Specifically, the control unit is electrically connected to the washing tank 1, pure water tank 2, alkali tank 3, alkali separator 4, filter 5, water washing tower 6, and water separator 7 to realize fully automated operation from feeding, washing, separation, water washing to recycling, ensuring process stability and uniform quality.

[0042] In addition, the separate first sewage tank 14, second sewage tank 63 and third sewage tank 70 facilitate centralized wastewater treatment and reduce environmental protection costs.

[0043] The actual engineering process is as follows:

[0044] During operation, the working solution to be treated enters the cleaning tank 1 through the working solution inlet 12. The water in the pure water tank 2 and the alkaline water in the alkaline solution tank 3 flow into the cleaning tank 1 through the pure water inlet and the alkaline solution inlet, respectively. After stirring and heating, the three liquids are mixed in the cleaning tank 1, so that the alkaline solution reacts with the organic impurities in the working solution to be treated through saponification, neutralization and other reactions, converting them into soluble salts or easily settled solid residues. The solid residues are discharged through the slag outlet 13. Then the working solution enters the filter 5 for preliminary purification, and then enters the alkaline separator 4 for alkaline separation.

[0045] After separation, the working liquid enters the water washing tower 6 for reverse water washing to further remove alkali. Finally, the pure treatment liquid is separated by the water separator. Then, the solenoid valve is opened to allow the phosphoric acid in the phosphoric acid addition unit 8 to enter the water separator, further ensuring that the pure treatment liquid is the required weak acid. Finally, the pure treatment liquid is collected by the working liquid recovery device. Throughout the operation, the control unit coordinates the operation of each component to achieve continuous and automated operation.

[0046] This utility model discloses a purification and recovery device for hydrogen peroxide working fluid. It can achieve continuous and automated removal of impurities from the working fluid through a washing tank, filtration through a filter, alkali removal through an alkali separator, and secondary alkali removal through a water washing tower, thus completely removing alkali from the working fluid. It has low labor costs, high recovery efficiency, and high purity of recovered fluid.

[0047] The above-described embodiments are only used to illustrate the technical solutions of this application, and are not intended to limit them. Although this application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of this application.

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