A treatment system for electronic grade hydrogen peroxide solution

Abstract

The utility model discloses a kind of electronic grade hydrogen peroxide solution processing systems, it is related to hydrogen peroxide processing technical field, including raw material box, raw material box is stored with hydrogen peroxide solution, hydrogen peroxide pump is connected with raw material box, the water inlet of mechanical impurity filtering component is connected with hydrogen peroxide pump, the water inlet of primary reverse osmosis piece is connected with the water outlet of mechanical impurity filtering component, the water inlet of secondary reverse osmosis piece is connected with the water outlet of primary reverse osmosis piece, high-purity product tank is connected with the water outlet of secondary reverse osmosis piece;It can effectively reduce the impurity in industrial hydrogen peroxide, produce the hydrogen peroxide solution satisfying electronic grade requirement, improve production efficiency and resource utilization rate simultaneously, reduce production cost and environmental pollution.

Description

Technical Field

[0001] This utility model relates to the field of hydrogen peroxide treatment technology, specifically to a treatment system for electronic-grade hydrogen peroxide solution. Background Technology

[0002] Currently, the anthraquinone process is a common method for producing hydrogen peroxide solution. This method uses a three-system solvent of aromatics, acetate, and trioctyl phosphate to produce hydrogen peroxide solution, which is then extracted and purified to obtain the product. However, this method produces products containing trace amounts of aromatics, metal ions, and anthraquinones that cannot be removed from the hydrogen peroxide solution, resulting in high levels of impurities, organic carbon, and phosphorus in the produced hydrogen peroxide. In recent years, electronic-grade hydrogen peroxide has been widely used in cleaning and corrosion processes during semiconductor and ultra-large integrated circuit assembly and manufacturing. This necessitates strict control of the impurity content in the hydrogen peroxide aqueous solution to achieve high purity. The hydrogen peroxide solution produced by the anthraquinone process cannot meet the requirements of electronic-grade products. With the rapid development of the electronics industry, the demand for electronic-grade hydrogen peroxide is increasing daily. Therefore, a processing system is needed to reduce the impurities, organic carbon, and phosphorus content of the finished hydrogen peroxide product and produce electronic-grade hydrogen peroxide solution to improve product competitiveness and increase company profits. Utility Model Content

[0003] The purpose of this invention is to provide a treatment system for electronic-grade hydrogen peroxide solution that can effectively reduce impurities in industrial hydrogen peroxide, produce hydrogen peroxide solution that meets electronic-grade requirements, and at the same time improve production efficiency and resource utilization, reduce production costs and environmental pollution.

[0004] The above-mentioned optimized structure of this utility model is achieved through the following technical solution: a processing system for electronic grade hydrogen peroxide solution, including a raw material tank, wherein the raw material tank stores hydrogen peroxide solution;

[0005] A hydrogen peroxide pump, which is connected to the raw material tank;

[0006] A mechanical impurity filter assembly, wherein the inlet of the mechanical impurity filter assembly is connected to the hydrogen peroxide pump;

[0007] A primary reverse osmosis unit, wherein the inlet of the primary reverse osmosis unit is connected to the outlet of the mechanical impurity filtration assembly;

[0008] A secondary reverse osmosis unit, wherein the inlet of the secondary reverse osmosis unit is connected to the outlet of the primary reverse osmosis unit;

[0009] A high-purity product tank is connected to the outlet of the secondary reverse osmosis unit.

[0010] In some embodiments, a pretreatment product tank is also included, which is connected to the outlet of the mechanical impurity filtration assembly;

[0011] A pretreatment product pump is located between the pretreatment product tank and the inlet of the first-stage reverse osmosis unit.

[0012] In some embodiments, a concentrate tank is also included, which is connected to the concentrate outlet of the secondary reverse osmosis unit;

[0013] A concentrate feed pump is provided between the concentrate tank and the pretreated product tank.

[0014] In some embodiments, a concentrate intermediate tank is also included, which is connected to the concentrate outlet of the first-stage reverse osmosis unit;

[0015] A concentrate intermediate pump, which is connected to the concentrate intermediate tank;

[0016] An industrial product tank, which is connected to the intermediate concentrate pump;

[0017] An ultrapure water station is connected to the intermediate concentrate tank.

[0018] In some embodiments, the mechanical impurity filtration assembly includes an ultrafiltration membrane filter element, the inlet of which is connected to the hydrogen peroxide pump, and the concentrate outlet of which is connected to the intermediate concentrate tank.

[0019] A nanofiltration membrane filter element, wherein the inlet of the nanofiltration membrane filter element is connected to the outlet of the ultrafiltration membrane filter element, the outlet of the nanofiltration membrane filter element is connected to the inlet of the first-stage reverse osmosis element, and the concentrate outlet of the nanofiltration membrane filter element is connected to the concentrate intermediate tank.

[0020] In some embodiments, the ultrapure water station is connected to the backwash port of the ultrafiltration membrane filter element, the backwash port of the nanofiltration membrane filter element, and the inlet of the primary reverse osmosis element.

[0021] In some embodiments, a primary cooler is also included, which is connected to the hydrogen peroxide pump;

[0022] A secondary cooler is provided between the primary cooler and the inlet of the mechanical impurity filter assembly.

[0023] In some embodiments, a high-purity intermediate tank is also included, which is connected to the outlet of the first-stage reverse osmosis unit;

[0024] A high-purity intermediate pump, which is connected to the high-purity intermediate tank;

[0025] A tertiary cooler is located between the high-purity intermediate pump and the inlet of the secondary reverse osmosis unit.

[0026] In some embodiments, a single-call valve is also included, which is disposed on the high-purity product tank, the pre-treated product tank, the concentrate tank, and the high-purity intermediate tank.

[0027] In summary, this utility model has the following beneficial effects:

[0028] This invention uses ultrafiltration and nanofiltration membranes to filter mechanical impurities in industrial hydrogen peroxide, protects the primary and secondary reverse osmosis units, and achieves a total metal ion removal rate of >99.99% through two-stage reverse osmosis filtration. This effectively reduces impurities in industrial hydrogen peroxide and produces a hydrogen peroxide solution that meets electronic grade requirements. The entire process does not involve any chemical reactions, is simple to operate, has a high impurity removal rate, and produces a high-purity product.

[0029] This invention can simultaneously produce industrial-grade and electronic-grade hydrogen peroxide by adjusting the concentrate yield, meeting different market demands, reducing wastewater treatment load, minimizing raw material loss, improving resource utilization and production efficiency, and lowering production costs. Attached Figure Description

[0030] Figure 1 This is a schematic diagram of the structure of this utility model.

[0031] In the diagram: 1. Raw material tank; 2. Hydrogen peroxide pump; 3. First-stage reverse osmosis unit; 4. Second-stage reverse osmosis unit; 5. High-purity product tank; 6. Pretreatment product tank; 7. Pretreatment product pump; 8. Concentrate tank; 9. Concentrate feed pump; 10. Concentrate intermediate tank; 11. Concentrate intermediate pump; 12. Industrial product tank; 13. Ultrapure water station; 14. Ultrafiltration membrane filter element; 15. Nanofiltration membrane filter element; 16. First-stage cooler; 17. Second-stage cooler; 18. High-purity intermediate tank; 19. High-purity intermediate pump; 20. Tertiary cooler; 21. Single-call valve. Detailed Implementation

[0032] The technical solutions of this utility model will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this utility model, and not all embodiments. Based on the embodiments of this utility model, all other embodiments obtained by those skilled in the art without creative effort are within the protection scope of this utility model.

[0033] refer to Figure 1A system for processing electronic-grade hydrogen peroxide solution includes a raw material tank 1, a hydrogen peroxide pump 2, a mechanical impurity filter assembly, a first-stage reverse osmosis unit 3, a second-stage reverse osmosis unit 4, and a high-purity product tank 5. The raw material tank 1 stores hydrogen peroxide solution. The hydrogen peroxide pump 2 is connected to the raw material tank 1, providing power to pump the solution out of the tank. The inlet of the mechanical impurity filter assembly is connected to the hydrogen peroxide pump 2, sequentially removing large molecular impurities and small molecular ions, thereby removing mechanical impurities from the solution. The inlet of the first-stage reverse osmosis unit 3 is connected to the outlet of the mechanical impurity filter assembly. In the first-stage reverse osmosis unit 3, the solution... The diffusion model is dominant, with H2O2 molecules (molecular weight 34) preferentially permeating through the membrane pores. Impurities are trapped due to size / charge repulsion, allowing for further purification. The inlet of the secondary reverse osmosis unit 4 is connected to the outlet of the primary reverse osmosis unit 3, which can break the concentration polarization layer under high pressure to selectively separate ppb-level trace impurities. Both the primary and secondary reverse osmosis units 3 and 4 can use oxidation-resistant composite reverse osmosis membranes. The primary and secondary reverse osmosis units 3 and 4 are connected in series to achieve deep removal of trace impurities, thereby obtaining electronic-grade hydrogen peroxide solution. The high-purity product tank 5 is connected to the outlet of the secondary reverse osmosis unit 4 and can store electronic-grade hydrogen peroxide solution.

[0034] In some embodiments, the system further includes a pretreatment product tank 6 and a pretreatment product pump 7. The pretreatment product tank 6 is connected to the outlet of the mechanical impurity filter assembly and can store the pretreated hydrogen peroxide solution. The pretreatment product pump 7 is located between the pretreatment product tank 6 and the inlet of the first-stage reverse osmosis unit 3 and can pump the hydrogen peroxide solution in the pretreatment product tank 6 into the first-stage reverse osmosis unit 3.

[0035] In some embodiments, the system also includes a concentrate tank 8 and a concentrate feed pump 9. The concentrate tank 8 is connected to the concentrate port of the secondary reverse osmosis unit 4 and can store the concentrate generated during the filtration process of the secondary reverse osmosis unit 4. The concentrate feed pump 9 is located between the concentrate tank 8 and the pretreatment product tank 6 and can send the concentrate in the concentrate tank 8 back to the pretreatment product tank 6 for recycling and purification.

[0036] In some embodiments, the system further includes a concentrate intermediate tank 10, a concentrate intermediate pump 11, an industrial product tank 12, and an ultrapure water station 13. The concentrate intermediate tank 10 is connected to the concentrate outlet of the first-stage reverse osmosis unit 3 and can store the concentrate produced by the first-stage reverse osmosis. The concentrate intermediate pump 11 is connected to the concentrate intermediate tank 10 and can pump the concentrate out of the concentrate intermediate tank 10. The industrial product tank 12 is connected to the concentrate intermediate pump 11 and can store the hydrogen peroxide solution of industrial grade products. The ultrapure water station 13 is connected to the concentrate intermediate tank 10 and can be connected to a water pump to deliver pure water to the concentrate intermediate tank 10 and mix it with the concentrate in the concentrate intermediate tank 10 to form the hydrogen peroxide solution of industrial grade products.

[0037] In some embodiments, the mechanical impurity filtration assembly includes an ultrafiltration membrane filter element 14 and a nanofiltration membrane filter element 15. The inlet of the ultrafiltration membrane filter element 14 is connected to the hydrogen peroxide pump 2. The ultrafiltration membrane filter element 14 can be an ultrafiltration membrane with a molecular weight cutoff of 5-50 kDa and a pore size of 0.01-0.1 μm. It removes colloids, microorganisms, and large organic molecules such as anthraquinone polymers through sieving, protecting the subsequent nanofiltration membrane filter element 15, primary reverse osmosis unit 3, and secondary reverse osmosis unit 4 from mechanical damage. The concentrate outlet of the ultrafiltration membrane filter element 14 is connected to the concentrate intermediate tank 10, allowing the retained material to be recycled to industrial-grade products, reducing waste. The inlet of the nanofiltration membrane filter element 15 is connected to the outlet of the ultrafiltration membrane filter element 14. The nanofiltration membrane filter element 15 can be a nanofiltration membrane with a pore size of 0.001-0.005 μm. Based on the Donnan effect and pore size sieving, it removes divalent ions such as Ca²⁺. + SO4² - It allows the passage of small molecule organic compounds such as acetate, while also allowing H2O2 molecules with a molecular weight of 34 to pass through. The outlet of the nanofiltration membrane filter element 15 is connected to the inlet of the first-stage reverse osmosis element 3, and the concentrate outlet of the nanofiltration membrane filter element 15 is connected to the concentrate intermediate tank 10.

[0038] In some embodiments, the ultrapure water station 13 is connected to the backwash port of the ultrafiltration membrane filter element 14, the backwash port of the nanofiltration membrane filter element 15, and the inlet of the first-stage reverse osmosis element 3, which can provide backwash water and supplement the first-stage reverse osmosis feed water.

[0039] In some embodiments, the system further includes a primary cooler 16 and a secondary cooler 17. The primary cooler 16 is connected to the hydrogen peroxide pump 2 and can initially cool the hydrogen peroxide solution. The secondary cooler 17 is located between the primary cooler 16 and the inlet of the mechanical impurity filter assembly and can further cool the hydrogen peroxide solution. This can lower the temperature of the hydrogen peroxide solution from room temperature to below 15°C, reduce the solution viscosity, reduce concentration polarization in subsequent membrane separation, reduce the thermal motion of H2O2 molecules, inhibit the self-decomposition reaction (2H2O2 → 2H2O + O2), and reduce the swelling degree of the membrane material, thereby increasing the rejection rate (for every 5°C decrease, the RO membrane desalination rate increases by approximately 1.5%).

[0040] In some embodiments, the system further includes a high-purity intermediate tank 18, a high-purity intermediate pump 19, and a tertiary cooler 20. The high-purity intermediate tank 18 is connected to the outlet of the first-stage reverse osmosis unit 3 and can store the hydrogen peroxide solution purified by the first-stage reverse osmosis. The high-purity intermediate pump 19 is connected to the high-purity intermediate tank 18 and can pump out the hydrogen peroxide solution from the high-purity intermediate tank. The tertiary cooler 20 is located between the high-purity intermediate pump 19 and the inlet of the second-stage reverse osmosis unit 4 and can cool the hydrogen peroxide solution entering the second-stage reverse osmosis unit 4, thereby enhancing the retention capacity of the second-stage reverse osmosis unit 4 for trace ions and improving the desalination rate.

[0041] In some embodiments, a single-exit valve 21 is also included. The single-exit valve 21 is provided on the high-purity product tank 5, the pre-treatment product tank 6, the concentrate tank 8, and the high-purity intermediate tank 18, and can maintain stable pressure inside the tank.

[0042] The specific working principle is as follows:

[0043] Industrial-grade hydrogen peroxide solution is drawn from raw material tank 1 via hydrogen peroxide pump 2 and sequentially passed through primary cooler 16 and secondary cooler 17 to cool to approximately 15°C. This reduces molecular thermal motion to inhibit decomposition and optimizes subsequent membrane separation performance. The low temperature also reduces the swelling degree of the membrane material and improves the rejection rate. The cooled solution first enters ultrafiltration membrane filter element 14, where large molecular impurities such as anthraquinone polymers and colloids are retained. The concentrated water retaining H2O2 molecules is discharged into the concentrated water intermediate tank 10 for industrial-grade products. The ultrafiltration permeate then enters nanofiltration membrane filter element 15 to remove small molecular ions such as Ca²⁺. + SO4² - Along with some organic matter, the nanofiltration permeate is stored in the pretreatment product tank 6, while the concentrated water retaining H2O2 molecules is discharged into the intermediate concentrated water tank 10 for industrial-grade products.

[0044] The pretreatment product pump 7 delivers the nanofiltration permeate from the pretreatment product tank 6 to the first-stage reverse osmosis unit 3 for deep impurity removal. A regulating valve can be installed at the concentrate outlet of the first-stage reverse osmosis unit 3 to adjust the ratio of concentrate to permeate. This is existing technology and will not be elaborated here. It allows approximately 70% of the solution to permeate through the reverse osmosis membrane, reducing the metal ion concentration to below 100 ppb, and then enters the high-purity intermediate tank 18. The remaining 30% concentrate, which is enriched with impurities, is discharged into the concentrate intermediate tank 10, and an appropriate amount of pure water is introduced through the ultrapure water station 13 to produce industrial-grade products such as 30% hydrogen peroxide.

[0045] The high-purity intermediate pump 19 delivers the first-stage reverse osmosis permeate to the tertiary cooler 20, cooling it to 10°C to enhance the separation efficiency of the second-stage reverse osmosis unit 4. The solution passes through the second-stage reverse osmosis unit 4, where high pressure breaks the concentration polarization layer, selectively separating trace impurities such as Fe³⁺. + Cu² + Cl - The desalination rate is >99.5%, the product water is electronic grade hydrogen peroxide with metal ions ≤1ppb and TOC ≤3ppm, and is stored in the high-purity product tank 5; the concentrate produced by the secondary reverse osmosis unit 4 contains a small amount of H2O2 and is returned to the pretreatment product tank 6 to participate in the purification process again for recycling. The product water and concentrate of the secondary reverse osmosis unit 4 can also be set according to the regulating valve set at the concentrate outlet.

[0046] The above embodiments are only used to illustrate the technical solutions of this utility model, and are not intended to limit it. Although this utility model 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 utility model.

Claims

1. A system for processing electronic-grade hydrogen peroxide solution, characterized in that: Includes a raw material box (1), which stores hydrogen peroxide solution; Hydrogen peroxide pump (2), which is connected to the raw material tank (1); A mechanical impurity filter assembly, wherein the inlet of the mechanical impurity filter assembly is connected to the hydrogen peroxide pump (2); The inlet of the first-stage reverse osmosis unit (3) is connected to the outlet of the mechanical impurity filtration assembly; Secondary reverse osmosis unit (4), the inlet of which is connected to the outlet of primary reverse osmosis unit (3); A high-purity product tank (5) is connected to the outlet of the secondary reverse osmosis unit (4).

2. The electronic-grade hydrogen peroxide solution treatment system according to claim 1, characterized in that: It also includes a pretreatment product tank (6), which is connected to the outlet of the mechanical impurity filtration assembly; A pretreatment product pump (7) is located between the pretreatment product tank (6) and the inlet of the first-stage reverse osmosis unit (3).

3. The electronic-grade hydrogen peroxide solution treatment system according to claim 2, characterized in that: It also includes a concentrate tank (8), which is connected to the concentrate outlet of the secondary reverse osmosis unit (4); A concentrate feed pump (9) is located between the concentrate tank (8) and the pretreated product tank (6).

4. The electronic-grade hydrogen peroxide solution treatment system according to claim 1, characterized in that: It also includes a concentrate intermediate tank (10), which is connected to the concentrate outlet of the first-stage reverse osmosis unit (3); A concentrate intermediate pump (11) is connected to the concentrate intermediate tank (10); An industrial product tank (12) is connected to the intermediate concentrate pump (11); Ultrapure water station (13), which is connected to the intermediate concentrated water tank (10).

5. The electronic-grade hydrogen peroxide solution treatment system according to claim 4, characterized in that: The mechanical impurity filtration assembly includes an ultrafiltration membrane filter element (14), the inlet of which is connected to the hydrogen peroxide pump (2), and the concentrate outlet of which is connected to the concentrate intermediate tank (10). Nanofiltration membrane filter element (15), the inlet of the nanofiltration membrane filter element (15) is connected to the outlet of the ultrafiltration membrane filter element (14), the outlet of the nanofiltration membrane filter element (15) is connected to the inlet of the first-stage reverse osmosis element (3), and the concentrate outlet of the nanofiltration membrane filter element (15) is connected to the concentrate intermediate tank (10).

6. The electronic-grade hydrogen peroxide solution treatment system according to claim 5, characterized in that: The ultrapure water station (13) is connected to the backwash port of the ultrafiltration membrane filter element (14), the backwash port of the nanofiltration membrane filter element (15), and the inlet of the first-stage reverse osmosis element (3).

7. The electronic-grade hydrogen peroxide solution treatment system according to claim 1, characterized in that: It also includes a primary cooler (16), which is connected to the hydrogen peroxide pump (2); A secondary cooler (17) is provided between the primary cooler (16) and the inlet of the mechanical impurity filter assembly.

8. The electronic-grade hydrogen peroxide solution treatment system according to claim 3, characterized in that: It also includes a high-purity intermediate tank (18), which is connected to the outlet of the first-stage reverse osmosis unit (3); A high-purity intermediate pump (19) is connected to the high-purity intermediate tank (18); The tertiary cooler (20) is located between the inlet of the high-purity intermediate pump (19) and the secondary reverse osmosis unit (4).

9. The electronic-grade hydrogen peroxide solution treatment system according to claim 8, characterized in that: It also includes a single-call valve (21), which is installed on the high-purity product tank (5), the pre-treatment product tank (6), the concentrate tank (8), and the high-purity intermediate tank (18).

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