Electronic grade hydrogen peroxide reverse osmosis production device

Abstract

The utility model relates to an electronic grade hydrogen peroxide reverse osmosis production device which can effectively remove organic matters, zwitterion impurities and particulate matters in hydrogen peroxide through multi-stage treatment steps such as cooling, filtering, reverse osmosis and ion exchange. The device comprises a cooler, a super filter, a reverse osmosis device, a cation exchange tower and an anion exchange tower. After being cooled and filtered, industrial-grade hydrogen peroxide firstly enters a primary reverse osmosis device for primary impurity removal, then is finely filtered through secondary reverse osmosis, and finally passes through a cation exchange tower and an anion exchange tower to remove trace ion impurities, so that G3 or G5-grade high-purity hydrogen peroxide is obtained. According to the design of the device, the traditional resin regeneration process is simplified, the generation of pollutants is reduced, and the production safety and efficiency are improved. The method is suitable for application scenes with strict requirements on high-purity hydrogen peroxide, such as semiconductor and electronic manufacturing.

Description

Technical Field

[0001] The utility model relates to the technical field of reverse osmosis production devices, in particular to an electronic-grade hydrogen peroxide reverse osmosis production device. Background Art

[0002] Electronic-grade hydrogen peroxide is a colorless liquid and strong oxidant used in microelectronics manufacturing and processing. It is an essential electronic chemical raw material in large-scale integrated circuit production. It can be used in semiconductor silicon wafer cleaning, etching, and photoresist removal processes.

[0003] The traditional electronic-grade hydrogen peroxide production process uses industrial-grade hydrogen peroxide as raw material. After cooling, it enters a macroporous adsorption resin column to remove TOC. After cooling again, it enters anion and cation exchange columns to remove anionic and cationic impurities in the hydrogen peroxide. Finally, it is ultrafiltered to remove particulate matter to obtain electronic-grade hydrogen peroxide, as described in Chinese patents CN1184138C and CN1699144A.

[0004] Traditional processes rely primarily on resin purification, which requires chemical regeneration, generating large amounts of waste methanol, acid, alkali, and wastewater. This process is unsafe, particularly during anion resin exchange, which requires complex regeneration and transformation. Incomplete transformation can easily lead to explosions. Furthermore, pure resin purification, due to the high impurity content in hydrogen peroxide, results in a short saturation cycle and requires repeated regeneration. This can also cause explosions if the chemicals used for regeneration are not rinsed thoroughly after regeneration.

[0005] In view of the above situation, the utility model proposes an electronic grade hydrogen peroxide production device. Utility Model Content

[0006] The purpose of this section is to summarize some aspects of the embodiments of the present invention and briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section and in the abstract and title of the utility model to avoid obscuring the purpose of this section, the abstract and the title of the utility model, and such simplifications or omissions shall not be used to limit the scope of the present invention.

[0007] In view of the following technical problems in the prior art: an electronic-grade hydrogen peroxide reverse osmosis production device, comprising a cooler, a super filter, a reverse osmosis device, a cation exchange tower and an anion exchange tower, the cooler being connected to the super filter, the super filter being connected to the reverse osmosis device, the reverse osmosis device being connected to the cation exchange tower, and the cation exchange tower being connected to the anion exchange tower.

[0008] As an optimal technical solution for an electronic-grade hydrogen peroxide reverse osmosis production device, it also includes a cation exchange tower cooler and an anion exchange tower cooler. The reverse osmosis device is connected to the cation exchange tower through the cation exchange tower cooler, and the cation exchange tower is connected to the anion exchange tower through the anion exchange tower cooler.

[0009] As an optimal technical solution for an electronic-grade hydrogen peroxide reverse osmosis production device, the reverse osmosis device includes a primary reverse osmosis device and a secondary reverse osmosis device, the super filter is connected to the primary reverse osmosis device, the primary reverse osmosis device is connected to the secondary reverse osmosis device through a secondary filter, and the secondary reverse osmosis device is connected to the cation exchange tower cooler.

[0010] As an optimal technical solution for an electronic-grade hydrogen peroxide reverse osmosis production device, a liquid inlet is provided on the cooler on a side away from the super filter, and a liquid outlet is provided on the anion exchange tower on a side away from the cation exchange tower.

[0011] As an optimal technical solution for an electronic-grade hydrogen peroxide reverse osmosis production device, a first-stage interception liquid outlet is provided on the side of the first-stage reverse osmosis device close to the super filter, a second-stage interception liquid outlet is provided on the side of the second-stage reverse osmosis device close to the second-stage filter, and a G3 quality electronic hydrogen peroxide liquid outlet is provided on the pipeline between the second-stage reverse osmosis device and the cation exchange tower cooler.

[0012] The utility model production device produces G3 grade electronic grade hydrogen peroxide, adopts two-stage reverse osmosis membrane filtration, does not require chemical reagents, and the production process is safe and stable without generating pollutants.

[0013] In the utility model, before reverse osmosis treatment, part of TOC and impurities are removed by cooling and ultrafiltration, which reduces the problem of easy clogging of the reverse osmosis membrane surface, prolongs the service life of the reverse osmosis membrane, and reduces production costs;

[0014] In the present invention, by adding anion-cation resin exchange columns, the quality can be further improved to G5 grade. Since most of the impurities have been removed by reverse osmosis treatment in the early stage, TOC has reached the G5 grade requirement, and there is no need to use macroporous adsorption resin to remove TOC. Trace amounts of anions and cations are exchanged using disposable anion-cation resins. The saturation cycle is long and no regeneration treatment is required. After saturation, new resins are directly replaced, avoiding the safety risks and quality risks caused by resin regeneration. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings required for describing the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without inventive work. Among them:

[0016] Figure 1 This is a schematic diagram of the overall structure of the device of the utility model;

[0017] Figure numerals: 1. cooler; 2. super filter; 3. primary reverse osmosis device; 4. secondary filter; 5. secondary reverse osmosis device; 6. cation exchange tower cooler; 7. cation exchange tower; 8. anion exchange tower cooler; 9. anion exchange tower; 10. liquid inlet; 11. liquid outlet; 12. primary interception liquid outlet; 13. secondary interception liquid outlet; 14. G3 quality electronic hydrogen peroxide liquid outlet. DETAILED DESCRIPTION

[0018] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the specific implementation methods of the present invention are described in detail below with reference to the accompanying drawings.

[0019] In the following description, many specific details are set forth to facilitate a full understanding of the present invention. However, the present invention may also be implemented in other ways different from those described herein. Those skilled in the art may make similar generalizations without violating the connotation of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below.

[0020] Secondly, the term "one embodiment" or "embodiment" herein refers to a specific feature, structure, or characteristic that may be included in at least one implementation of the present invention. The phrase "in one embodiment" appearing in various places throughout this specification does not necessarily refer to the same embodiment, nor does it refer to a separate or selective embodiment that is mutually exclusive with other embodiments.

[0021] Furthermore, the present invention is described in detail with reference to schematic diagrams. For ease of illustration, when describing embodiments of the present invention, cross-sectional views of device structures may be partially enlarged and not to scale. Furthermore, the schematic diagrams are merely illustrative and should not limit the scope of protection of the present invention. Furthermore, in actual production, three-dimensional dimensions, including length, width, and depth, should be included.

[0022] Please refer to Figure 1As shown, this utility model provides an electronic-grade hydrogen peroxide reverse osmosis production device. This design significantly improves the purity of hydrogen peroxide through optimized cooling, filtration, reverse osmosis, and ion exchange steps, meeting the quality standards of G3 or G5 electronic-grade hydrogen peroxide. By reducing impurity clogging and improving production efficiency, this device addresses a number of issues in traditional hydrogen peroxide production processes, including low production efficiency, poor safety, and inadequate impurity removal. The following describes the device in detail, including its composition, operating principle, and operational procedures.

[0023] The main components of the device include a cooler 1, a super filter 2, a reverse osmosis device, a cation exchange tower 7, and an anion exchange tower 9. Its working principle is to remove organic matter (such as 2-ethylanthraquinone, etc.), anionic and cationic impurities, and other particulate impurities in hydrogen peroxide through a multi-stage reverse osmosis system combined with a cation and anion exchange system to achieve the high purity requirements of electronic-grade hydrogen peroxide. First, the temperature of industrial-grade hydrogen peroxide is reduced to about 5°C by cooler 1. In this low-temperature environment, the solubility of TOC (total organic carbon) impurities in hydrogen peroxide, especially organic impurities such as 2-ethylanthraquinone, is reduced, and some impurities begin to precipitate crystals. Subsequently, these precipitated crystals and other large particulate impurities are removed by super filter 2, effectively reducing the clogging of subsequent reverse osmosis membranes, extending the service life of reverse osmosis membranes, and reducing production costs.

[0024] After cooling and filtration, the hydrogen peroxide enters the primary reverse osmosis unit 3. Using semipermeable membrane technology, the reverse osmosis unit effectively intercepts most of the TOC and anions and cations in the hydrogen peroxide, while allowing small molecules of water and hydrogen peroxide to pass freely. The primary reverse osmosis stage primarily performs the initial impurity removal process, removing most organic matter and anionic and cationic impurities in the hydrogen peroxide, thereby improving the purity of the permeate. The unit's specially designed membrane pore size effectively intercepts impurities, ensuring that the permeated liquid meets the required quality standards. Through the primary reverse osmosis filtration, the vast majority of impurities are trapped on the reverse osmosis membrane surface, significantly improving production efficiency.

[0025] The permeate after the first-stage reverse osmosis is further cooled to 10°C by the cooler 1 and enters the second-stage reverse osmosis device 5 for more refined filtration. The main purpose of the second-stage reverse osmosis is to thoroughly remove the trace organic matter and impurities remaining after the first-stage treatment. According to the product quality requirements, the pore size of the second-stage reverse osmosis membrane can be adjusted to ensure the best balance between purity and water output. The permeate after the second-stage reverse osmosis treatment basically reaches the purity requirements of G3 electronic grade hydrogen peroxide, meeting the needs of most semiconductor and electronic manufacturing processes. The design of the second-stage reverse osmosis makes the permeate purer and the system operation more stable, reducing the problem of membrane clogging caused by impurity accumulation, thereby extending the overall service life of the reverse osmosis device.

[0026] If the purity of hydrogen peroxide needs to be further improved, especially in some applications with higher requirements for product quality, the processing steps of the cation exchange tower 7 and the anion exchange tower 9 can be added. The permeate after the secondary reverse osmosis is cooled to a low temperature of 0 to 5°C by the cation exchange tower cooler 6, and then enters the anion exchange tower 9 to remove residual anionic impurities. Through these two processing steps, trace ionic impurities in the hydrogen peroxide are further removed, and finally G5 electronic grade hydrogen peroxide is obtained. This process can significantly improve the purity of the product, especially for application scenarios requiring extremely high purity. The device can ensure that the product meets strict quality standards.

[0027] To ensure temperature control and operational stability between each process step, the system incorporates multiple coolers at key locations. For example, the reverse osmosis unit is connected to the cation exchange tower 7 via the cation exchange tower cooler 6, ensuring that the permeate reaches the ideal temperature before entering the cation exchange tower 7. A cooler is also connected between the cation exchange tower 7 and the anion exchange tower 9, ensuring that the permeate temperature remains within the optimal range during each process step. This not only helps improve impurity removal efficiency but also ensures continued production stability.

[0028] The device is also designed with multiple interception outlets to facilitate the timely discharge of impurities and optimize the production process. The first and second stages of the reverse osmosis unit are each equipped with a first-stage interception outlet 12 and a second-stage interception outlet 13 for removing impurities from the reverse osmosis process. A G3 electronic-grade hydrogen peroxide outlet 14 is also located on the pipeline between the cation exchange tower cooler 6 and the cation exchange tower 7, facilitating the timely extraction of a product that meets quality standards.

[0029] Compared with the traditional electronic-grade hydrogen peroxide production process, this utility model has significant advantages in terms of safety, economy, and environmental friendliness. Traditional processes usually rely on resin columns for purification, and the resin needs to be regenerated regularly during use. The regeneration process produces a large amount of waste chemicals, such as waste methanol, waste acid, and waste alkali. These are not only harmful to the environment, but also have problems such as complex operation and incomplete regeneration, and may even cause safety accidents. This device replaces the traditional resin regeneration and purification method with a multi-stage reverse osmosis system. No chemical reagents are required during the entire production process, which reduces the generation of pollutants and ensures a green and environmentally friendly production process.

[0030] In traditional processes, resin regeneration can easily lead to hydrogen peroxide decomposition and explosion accidents, especially during anion resin exchange. Incomplete flushing with regeneration chemicals can easily lead to safety hazards. However, the present invention utilizes disposable resin, eliminating the need for regeneration and thus avoiding these potential safety risks. Furthermore, the service life of the reverse osmosis membrane is significantly extended in this device because the initial cooling and filtration steps remove large impurities, reducing the burden on the reverse osmosis membrane.

[0031] The embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present invention may be modified or replaced by equivalents without departing from the spirit and scope of the technical solutions of the present invention, and all of these should be included in the scope of the claims of the present invention.

Claims

1. An electronic grade hydrogen peroxide reverse osmosis production device, characterized in that: The invention comprises a cooler, a super filter, a reverse osmosis device, a cation exchange tower and an anion exchange tower. The cooler is connected to the super filter, the super filter is connected to the reverse osmosis device, the reverse osmosis device is connected to the cation exchange tower, and the cation exchange tower is connected to the anion exchange tower.

2. The electronic-grade hydrogen peroxide reverse osmosis production device according to claim 1, wherein It also includes a cation exchange tower cooler and an anion exchange tower cooler. The reverse osmosis device is connected to the cation exchange tower through the cation exchange tower cooler, and the cation exchange tower is connected to the anion exchange tower through the anion exchange tower cooler.

3. The electronic-grade hydrogen peroxide reverse osmosis production device according to claim 2, wherein The reverse osmosis device includes a primary reverse osmosis device and a secondary reverse osmosis device, the super filter is connected to the primary reverse osmosis device, the primary reverse osmosis device is connected to the secondary reverse osmosis device through a secondary filter, and the secondary reverse osmosis device is connected to the cation exchange tower cooler.

4. The electronic-grade hydrogen peroxide reverse osmosis production device according to claim 3, characterized in that: A liquid inlet is provided on a side of the cooler away from the super filter, and a liquid outlet is provided on a side of the anion exchange tower away from the cation exchange tower.

5. The electronic-grade hydrogen peroxide reverse osmosis production device according to claim 4, characterized in that: A first-stage interception liquid outlet is provided on the side of the first-stage reverse osmosis device close to the super filter, a second-stage interception liquid outlet is provided on the side of the second-stage reverse osmosis device close to the second-stage filter, and a G3 quality electronic hydrogen peroxide liquid outlet is provided on the pipeline between the second-stage reverse osmosis device and the cation exchange tower cooler.

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