Method for preparing electronic grade hydrogen peroxide

CN122704849BActive Publication Date: 2026-10-13DANUOER (HUBEI) MICROELECTRONIC MATERIALS CO LTD +1
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Patent Information

Application Number
CN202611222935.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2026-08-13
Publication Date
2026-10-13
Estimated Expiration
2046-08-13

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Technical Problem

[0007]为了解决目前双氧水易分解导致纯度下降的问题,本申请提供了一种电子级双氧水的制备方法

Benefits of technology

[0019]进一步的,所述多级精密过滤的滤膜分别为1.0μm、0.2μm及0.1μm。

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Abstract

The application relates to the technical field of hydrogen peroxide, and particularly discloses a preparation method of electronic-grade hydrogen peroxide. The preparation method comprises the following steps: S1, adding a stabilizer into industrial-grade hydrogen peroxide, and then stirring and performing multi-stage precision filtration; S2, filtering the hydrogen peroxide and then passing into an adsorption column for adsorption purification; and S3, after the purification, performing primary filtration membrane and secondary filtration membrane filtration, and then filling to obtain electronic-grade hydrogen peroxide. The industrial-grade hydrogen peroxide is used as raw material, chemical stabilization pretreatment is carried out to inhibit hydrogen peroxide decomposition and passivate trace metal impurities, then multi-stage precision filtration, resin adsorption purification and two-stage super membrane filtration are carried out to remove trace metals, particles and organic impurities in the system, and finally filling is carried out to obtain electronic-grade hydrogen peroxide products, which meets the requirements of stability and high purity.
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Description

Technical Field

[0001] This application relates to the field of hydrogen peroxide technology, specifically to a method for preparing electronic-grade hydrogen peroxide. Background Technology

[0002] Electronic-grade hydrogen peroxide decomposes into water and oxygen after use, leaving no residue or pollution. It is a green and environmentally friendly electronic chemical with an irreplaceable position in high-tech fields such as semiconductors, display panels, and photovoltaics. In semiconductor manufacturing, it accounts for over 65% of applications. Within the semiconductor industry, it is one of the most widely used chemical reagents in wafer cleaning, photoresist stripping, and etching processes. Especially in advanced processes, its strong oxidizing properties effectively remove metallic impurities, organic contaminants, and particulate contaminants from the wafer surface without damaging the wafer's fine structure. In display panel manufacturing, electronic-grade hydrogen peroxide is used in processes such as array cleaning and ITO film etching for TFT-LCD and OLED panels, ensuring the high resolution and stability of display devices. In the photovoltaic field, it is used in the silicon wafer cleaning and texturing processes of high-efficiency photovoltaic cells such as TOPCon / HJT, improving cell conversion efficiency. Furthermore, electronic-grade hydrogen peroxide is also used in pre-packaging cleaning of electronic components and the preparation of optoelectronic materials, providing key material support for the high-quality development of the electronics industry.

[0003] Despite the wide application of electronic-grade hydrogen peroxide, numerous technical challenges remain in its production, storage, and application. Hydrogen peroxide itself is prone to decomposition, especially under conditions of high temperature, light exposure, and metal ion catalysis, which accelerates the decomposition rate. This not only affects the stability of the product concentration but may also pose safety hazards. Furthermore, the high purity of electronic-grade hydrogen peroxide makes it even more sensitive to the catalytic effects of impurities. Therefore, stabilizers are needed to inhibit the decomposition reaction.

[0004] Currently, commonly used stabilizers include inorganic stabilizers, organophosphonic acid stabilizers, polyol and sugar stabilizers, and small molecule carboxylic acid stabilizers. The core function of these stabilizers is to complex and passivate trace transition metal ions such as Fe, Cu, Ni, and Cr, blocking the catalytic decomposition of hydrogen peroxide by these metal ions, thereby inhibiting concentration decay and impurity growth during storage, transportation, and wafer cleaning.

[0005] However, the water-soluble chelates formed by organophosphonic acids and metal ions are too small to be effectively retained by microfiltration membranes. Furthermore, phosphonic acid molecules can undergo bond breakage and degradation in the free radical environment catalyzed by hydrogen peroxide and trace metals, producing orthophosphate impurities. Strong acidity can also damage the carrier structure. Inorganic chelates, represented by sodium silicate, are highly dependent on alkaline environments for stability. They are easily hydrolyzed or acidified in the weakly acidic system where hydrogen peroxide is most stable, losing their colloidal adsorption function. Polyols and sugars rely solely on weak hydrogen bonds or solvation effects for physical adsorption, exhibiting almost zero passivation ability for trace metals. Moreover, their own oxidation and degradation by hydrogen peroxide significantly increases total organic carbon (TOC). Carboxylic acids, due to their monodentate coordination chelation equilibrium constant being much lower than that of organophosphonic acids (polydentate coordination), have insufficient complexation strength. The dosage required for effective passivation inevitably leads to severely excessive TOC levels. They also lack a carrier-retention mechanism for physically removing the complexed metal from the liquid phase, making them impractical in electronic-grade processes.

[0006] Therefore, the key is to solve the stability problem while ensuring the purity of hydrogen peroxide. Summary of the Invention

[0007] To address the problem of hydrogen peroxide's easy decomposition leading to decreased purity, this application provides a method for preparing electronic-grade hydrogen peroxide.

[0008] This invention uses industrial-grade hydrogen peroxide as raw material. Through chemical stabilization pretreatment, hydrogen peroxide decomposition is inhibited and trace metal impurities are passivated. Then, through multi-stage precision filtration, resin adsorption purification, and two-stage super membrane filtration, trace metals, particles, and organic impurities in the system are removed. Finally, electronic-grade hydrogen peroxide is obtained through bottling, which takes into account both stability and high purity requirements.

[0009] This invention uses sodium-based montmorillonite as a layered carrier. After acid washing to remove impurities and activation, it reacts with sodium organophosphonate salts. Subsequent ultrasonic dispersion further promotes the dispersion and exfoliation of the layers. In the hydrogen peroxide system, the nanosheets are stably dispersed due to the electrostatic repulsion effect of the negative surface charge, preventing agglomeration and precipitation. Utilizing the acidified and exfoliated montmorillonite nanosheets, strong coordination bonds and hydrogen bonds are formed with organophosphonate ions through numerous Al-OH and Si-OH active sites on their edges and surfaces. This efficiently and stably loads organophosphonates onto the surface of the nano-montmorillonite nanosheets, constituting a novel composite stabilizer. When trace metal ions are present in the hydrogen peroxide system, the liquid-phase metal ions preferentially bind to the vacant coordination sites of organophosphonate ions. Through coordination competition, organophosphonate ions anchored on the surface or edge active sites of the montmorillonite nanosheets undergo a certain degree of coordination exchange and recoordination, chelating metal ions. This effectively passivates metal impurities, preventing the catalytic decomposition of hydrogen peroxide and ensuring long-term stability of its purity. After pretreatment with chemical stabilizers, the montmorillonite nanosheets loaded with organophosphonates are effectively removed through multiple filtration processes, including multi-stage filtration and adsorption purification. This reduces the residual stabilizer in the final hydrogen peroxide solution and minimizes its impact on subsequent use.

[0010] Phosphonic acid groups exhibit significantly higher complexation stability constants for transition metal ions such as Fe, Cu, and Ni compared to inorganic acid groups, effectively passivating the catalytic decomposition activity of metal ions. Furthermore, their molecular size is well-suited to the surface and edge active sites of the nanosheets exposed after montmorillonite exfoliation, allowing for strong adsorption at these sites through coordination and hydrogen bonding. The carbon chains of phosphonates also provide steric hindrance, further enhancing the stabilizing effect. Compared to directly using free organophosphonic acids, this invention employs sodium organophosphonates, which helps to mitigate the strong acidity of free organophosphonic acids on the structure and loading process of montmorillonite, enabling the organophosphonates to interact with activated montmorillonite more gently and uniformly in an aqueous system. After dissolving in water, sodium organophosphonates form phosphonate species with varying degrees of protonation depending on the system pH, participating in multi-site coordination of metal ions. While the coordination between sodium ions and phosphonates is relatively weak, the presence of transition metal ions such as Fe, Cu, and Ni in the system allows the phosphonic acid groups to further coordinate with these metal ions, thereby achieving passivation and stabilization of impurity metals.

[0011] When disodium hydroxyethylidene diphosphonate and tetrasodium aminotrimethylidene phosphonate are mixed, the high chelating strength of disodium hydroxyethylidene diphosphonate results in a prominent chelating effect on metal ions, while the tetrasodium aminotrimethylidene phosphonate has a wide complexing range and can simultaneously complex multiple metal ions with strong coordination stability. The combination of the two forms a synergistic effect of strong chelation and wide complexation, which can enhance the stability of the stabilizer in multi-metal complex pollution systems and extend the stability period of electronic-grade hydrogen peroxide.

[0012] In a first aspect, the present invention provides a method for preparing electronic-grade hydrogen peroxide, comprising the following steps: S1. Add the stabilizer to industrial-grade hydrogen peroxide, stir for 20-30 minutes, and then perform multi-stage precision filtration; S2. The filtered hydrogen peroxide is passed through adsorption columns filled with aminophosphonic acid chelating resin and strong basic anion exchange resin respectively for adsorption purification. S3. After purification, the hydrogen peroxide is filtered through a primary filtration membrane and a secondary filtration membrane and then bottled to obtain electronic-grade hydrogen peroxide. The stabilizer is obtained by acid washing and purification of sodium montmorillonite, followed by activation, then coordination with sodium organophosphonate, ultrasonic exfoliation, aging, and finally centrifugation, ultrafiltration, and dispersion.

[0013] Furthermore, the method for preparing the stabilizer includes the following steps: X1. Add sodium-based montmorillonite to ultrapure water, stir and disperse for 40-50 min, then add acid to adjust the pH to 4-5, heat to 40-50℃ and stir and acid wash for 1-2 h, let stand and settle, take the upper suspension, vacuum filter, wash and then disperse in ultrapure water to obtain 4-5% montmorillonite suspension, heat to 60-65℃ and add acid to adjust the pH to 4-5, keep warm and activate for 1-2 h; X2. Prepare a 5% aqueous solution of sodium organophosphonate and slowly add it dropwise to the activated montmorillonite suspension. Continue heating to 70-75℃ and stirring for 3-4 hours. After cooling to room temperature, vacuum filter, wash, and redisperse in ultrapure water. Disperse ultrasonically at 200W for 30-40 minutes, let stand for 1-2 hours, centrifuge to discard the lower precipitate, filter the supernatant through a 0.05μm ultrafiltration membrane, collect the filter cake, determine the solid content, and disperse it in ultrapure water to obtain a 5-7% nanocolloid dispersion, which is the stabilizer.

[0014] Furthermore, the mass ratio of the sodium-based montmorillonite to ultrapure water is 1:10-15.

[0015] Furthermore, the sodium organophosphonate is disodium hydroxyethylidene diphosphonate and / or tetrasodium aminotrimethylidene phosphonate.

[0016] Furthermore, the mass ratio of the aqueous solution of the organophosphonate to the dry basis of montmorillonite is 10-13:1.

[0017] Preferably, the sodium organophosphonate is a mixture of disodium hydroxyethylidene diphosphonate and tetrasodium aminotrimethylidene phosphonate in a mass ratio of 1-3:1.

[0018] Furthermore, the amount of stabilizer added is 0.5-1.7% of industrial-grade hydrogen peroxide.

[0019] Furthermore, the filter membranes of the multi-stage precision filtration are 1.0μm, 0.2μm, and 0.1μm, respectively.

[0020] Furthermore, the flow rate when the adsorption column is introduced is 3-4 L / h, and the adsorption temperature is 25-30℃.

[0021] Furthermore, the primary filter membrane and the secondary filter membrane are 0.01 μm and 0.001 μm, respectively.

[0022] Compared with the prior art, the beneficial effects of this application are at least as follows: This invention uses sodium-based montmorillonite as a layered carrier. After treatment, organophosphonic acids are efficiently and stably loaded onto the surface of nano-montmorillonite sheets. When trace metal ions are present in the hydrogen peroxide system, they preferentially bind to vacant coordination sites of organophosphonate ions. Through coordination competition, organophosphonate ions anchored on the surface or edge active sites of the montmorillonite nanosheets undergo a certain degree of coordination exchange and recoordination, effectively removing metal impurities and preventing the hydrogen peroxide from being catalytically decomposed, thus ensuring its long-term purity stability. After pretreatment with chemical stabilizers, the hydrogen peroxide undergoes multiple filtration processes, including multi-stage filtration and adsorption purification, to reduce the residual stabilizer in the final hydrogen peroxide and minimize its impact on subsequent use. Detailed Implementation

[0023] The various embodiments or implementation schemes in this specification are described in a progressive manner, with each embodiment focusing on the differences from other embodiments.

[0024] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "illustrative embodiment," "example," "specific example," or "some examples," etc., indicate that a specific feature, structure, material, or characteristic described in connection with an embodiment or example is included in at least one embodiment or example of this application. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.

[0025] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one of that feature. In the description of this application, "multiple" means at least two, such as two, three, etc., unless otherwise explicitly specified.

[0026] In this specification, unless otherwise specified, "parts" refers to "parts by weight".

[0027] The following describes embodiments of this application. The embodiments described below are exemplary and are only used to explain this application, and should not be construed as limiting this application. Where specific techniques or conditions are not specified in the embodiments, they are performed according to the techniques or conditions described in the literature in this field or according to the product instructions. Reagents or instruments used, unless otherwise specified, are all conventional products that can be obtained commercially.

[0028] Sodium-based montmorillonite, with an ion exchange capacity ≥90mmol / 100g and a purity ≥98%.

[0029] Aminophosphonic acid chelating resin, model: D402.

[0030] Chlorine-type strong basic anion exchange resin, model: IRA-410.

[0031] Disodium hydroxyethylidene diphosphonate, CAS No.: 7414-83-7.

[0032] Tetrasodium aminotrimethylphosphonate, CAS No.: 20592-85-2.

[0033] Example 1 A method for preparing electronic-grade hydrogen peroxide includes the following steps: S1. Add the stabilizer to industrial-grade hydrogen peroxide at a ratio of 1%, stir for 30 minutes, and then perform multi-stage precision filtration at 1.0μm, 0.2μm and 0.1μm. S2. The filtered hydrogen peroxide was successively passed through adsorption columns filled with aminophosphonic acid chelating resin and chlorine-type strong base anion exchange resin for adsorption purification. The flow rate when passing through the adsorption column was 4L / h and the adsorption temperature was 28℃. S3. After purification, the solution is filtered through a 0.01μm primary filter membrane and a 0.001μm secondary filter membrane before being bottled to obtain electronic-grade hydrogen peroxide. The method for preparing the stabilizer includes the following steps: X1. Add 100 parts of sodium montmorillonite to 1200 parts of ultrapure water, stir and disperse for 45 min, then add dilute hydrochloric acid to adjust the pH to 4.5, heat to 45℃ and stir and acid wash for 2 h, let stand and settle, take the upper suspension, vacuum filter, wash and then disperse in ultrapure water to obtain 4% montmorillonite suspension, heat to 65℃ and add dilute hydrochloric acid to adjust the pH to 4.8, keep warm and activate for 2 h; X2. After preparing a 5% aqueous solution of disodium hydroxyethylidene diphosphonate, it was slowly added dropwise to the activated montmorillonite suspension. The mass ratio of the sodium organophosphonate aqueous solution to the dry montmorillonite was 12:1. The temperature was further increased to 75℃, and the mixture was stirred for 3.5 hours. After cooling to room temperature, it was vacuum filtered, washed, and redispersed in ultrapure water. It was ultrasonically dispersed at 200W for 40 minutes, allowed to stand for 2 hours, centrifuged to remove the lower precipitate, and the supernatant was filtered through a 0.05μm ultrafiltration membrane. The filter cake was collected, and after determining the solid content, it was dispersed in ultrapure water to obtain a 5% nanocolloid dispersion, which is the stabilizer.

[0034] Example 2 It is basically the same as Example 1, except that the disodium hydroxyethylidene diphosphonate is replaced with an equal mass of tetrasodium aminotrimethylidene phosphonate.

[0035] Example 3 It is basically the same as Example 1, except that the disodium hydroxyethylidene diphosphonate is replaced with a mixture of equal mass of disodium hydroxyethylidene diphosphonate and tetrasodium aminotrimethylidene phosphonate in a mass ratio of 1:1.

[0036] Example 4 It is basically the same as Example 1, except that the disodium hydroxyethylidene diphosphonate is replaced with a mixture of equal mass of disodium hydroxyethylidene diphosphonate and tetrasodium aminotrimethylidene phosphonate in a mass ratio of 1.5:1.

[0037] Example 5 The example is essentially the same as Example 1, except that disodium hydroxyethylidene diphosphonate is replaced with a mixture of equal masses of disodium hydroxyethylidene diphosphonate and tetrasodium aminotrimethylidene phosphonate in a mass ratio of 3:1.

[0038] Comparative Example 1 A method for preparing electronic-grade hydrogen peroxide includes the following steps: S1. Disodium hydroxyethylidene diphosphonate was prepared into a 5% aqueous solution and then added to industrial-grade hydrogen peroxide at a ratio of 1%. The solution was stirred for 30 minutes and then subjected to multi-stage precision filtration at 1.0 μm, 0.2 μm and 0.1 μm. S2. The filtered hydrogen peroxide is passed into an adsorption column filled with aminophosphonic acid chelating resin and chlorine-type strong base anion exchange resin for adsorption purification. The flow rate when passing into the adsorption column is 4L / h and the adsorption temperature is 28℃. S3. After purification, the solution is filtered through a 0.01μm primary filter membrane and a 0.001μm secondary filter membrane before being bottled to obtain electronic-grade hydrogen peroxide.

[0039] Test section 1. The electronic-grade hydrogen peroxide prepared in the examples and comparative examples was tested for metal ion and anionic impurities; 2. The TOC (Total Organic Carbon) and particle number of the electronic-grade hydrogen peroxide prepared in the examples and comparative examples were tested; 3. The electronic-grade hydrogen peroxide prepared in the examples and comparative examples was subjected to an accelerated aging test at 80°C. Equal volumes of the finished electronic-grade hydrogen peroxide samples from each group were taken, sealed, and placed in a constant-temperature oven at 80°C for 72 hours. The initial hydrogen peroxide mass fraction and the hydrogen peroxide mass fraction after 72 hours of constant temperature were measured using a titration method. Each group of samples was tested in triplicate, and the average value was taken. The decomposition rate of hydrogen peroxide after aging was calculated based on the mass fraction results.

[0040] Table 1

[0041] Table 2

[0042] As can be seen from Tables 1 and 2, after multi-stage gradient filtration, dual resin adsorption, and ultra-precision membrane filtration, the metal ions, anions, TOC, and particulate matter in each embodiment of industrial-grade hydrogen peroxide are all at low levels, and the hydrogen peroxide decomposition rate is low.

[0043] The lower the background concentration of residual trace transition metal catalytic ions in hydrogen peroxide, the better its thermal stability and storage stability.

[0044] Example 1 and Example 2 used disodium hydroxyethylidene diphosphonate and tetrasodium aminotrimethylidene phosphonate, respectively. Compared with Example 2, Example 1 showed better control results for Fe and Cu; compared with Example 1, Example 2 showed better control results for Ni and Al, indicating that the two organophosphonates have different relative compatibility with different metal impurities.

[0045] Examples 3-5 used disodium hydroxyethylidene diphosphonate and tetrasodium aminotrimethylidene phosphonate in different ratios. The ratio used in Example 4 achieved better overall results, indicating that the final purification effect is related to the combined effect of the two organophosphonates under conditions of multiple metal impurities. The ratio in Example 4 effectively balanced the control of different metal impurities, resulting in better performance in terms of overall metal ion content, TOC, particle number, and hydrogen peroxide decomposition rate. The overall results of Examples 3 and 5 were slightly lower than those of Example 4, indicating that the ratio of the two organophosphonates affects the overall compatibility with multiple metal impurities; a ratio of 1.5:1 achieved better overall performance.

[0046] Based on the anion test results, Cl in Examples 1-5 - NO3 - SO4 2- and PO4 3-All levels remained low. In each embodiment, the organophosphonates were pre-loaded onto the treated montmorillonite support. After stabilization and metal ion coordination, the montmorillonite nanosheets loaded with organophosphonates could be further removed during the multi-stage filtration process at the front end, reducing the amount of stabilizers and related substances entering the subsequent resin purification unit. Subsequently, the system was further purified by a chloride-type strong basic anion exchange resin, further controlling the trace anions in the system.

[0047] Comparative Example 1 directly added free disodium hydroxyethylidene diphosphonate without using montmorillonite as a support. The water-soluble chelates formed by free phosphonates and metal ions are nanometer to sub-nanometer in size. The free system not only exhibits poor chelation uniformity and cannot achieve sufficient site-specific passivation, but even if the unretained metal-phosphonate complexes enter the subsequent two-resin unit, their high stability constants result in limited coordination position exchange efficiency. Furthermore, Comparative Example 1 lacks the process of pre-loading organophosphonates onto montmorillonite for front-end separation with the support. Free organophosphonates and related water-soluble substances continue to enter the subsequent resin purification unit, resulting in a difference in the liquid phase composition entering the anion exchange resin compared to the examples. Regarding PO4... 3- Free organophosphonic acids may degrade and generate orthophosphate ions in the hydrogen peroxide and trace metal-catalyzed free radical environment, further increasing the treatment load of phosphorus-containing anions. Although the formed chelates reduce the direct catalytic activity of the metal, the chelates themselves can still slowly decompose in the presence of hydrogen peroxide and trace free radicals, releasing metal ions again. Unchelated free metal ions continue to catalyze the decomposition of hydrogen peroxide, inducing side reactions and resulting in a relatively high decomposition rate of hydrogen peroxide.

[0048] Finally, it should be noted that the above 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 or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of this application.

Claims

1. A method for preparing electronic-grade hydrogen peroxide, characterized in that, Includes the following steps: S1. Add the stabilizer to industrial-grade hydrogen peroxide, stir for 20-30 minutes, and then perform multi-stage precision filtration; S2. The filtered hydrogen peroxide is passed through adsorption columns filled with aminophosphonic acid chelating resin and strong basic anion exchange resin respectively for adsorption purification. S3. After purification, the hydrogen peroxide is filtered through a primary filtration membrane and a secondary filtration membrane and then bottled to obtain electronic-grade hydrogen peroxide. The stabilizer is obtained by acid washing and purification of sodium montmorillonite, followed by activation, addition of sodium organophosphonate salt for coordination, ultrasonic exfoliation, aging, and then centrifugation, ultrafiltration, and dispersion. The sodium organic phosphonate salt is disodium hydroxyethylidene diphosphonate and / or tetrasodium aminotrimethylidene phosphonate.

2. The method for preparing electronic-grade hydrogen peroxide as described in claim 1, characterized in that, The method for preparing the stabilizer includes the following steps: X1. Add sodium-based montmorillonite to ultrapure water, stir and disperse for 40-50 min, then add acid to adjust the pH to 4-5, heat to 40-50℃ and stir and acid wash for 1-2 h, let stand and settle, take the upper suspension, vacuum filter, wash and then disperse in ultrapure water to obtain 4-5% montmorillonite suspension, heat to 60-65℃ and add acid to adjust the pH to 4-5, keep warm and activate for 1-2 h; X2. Prepare a 5% aqueous solution of sodium organophosphonate and slowly add it dropwise to the activated montmorillonite suspension. Continue heating to 70-75℃ and stirring for 3-4 hours. After cooling to room temperature, vacuum filter, wash, and redisperse in ultrapure water. Disperse ultrasonically at 200W for 30-40 minutes, let stand for 1-2 hours, centrifuge to discard the lower precipitate, filter the supernatant through a 0.05μm ultrafiltration membrane, collect the filter cake, determine the solid content, and disperse it in ultrapure water to obtain a 5-7% nanocolloid dispersion, which is the stabilizer.

3. The method for preparing electronic-grade hydrogen peroxide as described in claim 2, characterized in that, The mass ratio of sodium-based montmorillonite to ultrapure water is 1:10-15.

4. The method for preparing electronic-grade hydrogen peroxide as described in claim 2, characterized in that, The mass ratio of the aqueous solution of the organophosphonate sodium salt to the dry basis of montmorillonite is 10-13:

1.

5. The method for preparing electronic-grade hydrogen peroxide as described in claim 1, characterized in that, The organophosphonate sodium salt is a mixture of disodium hydroxyethylidene diphosphonate and tetrasodium aminotrimethylidene phosphonate in a mass ratio of 1-3:

1.

6. The method for preparing electronic-grade hydrogen peroxide as described in claim 1, characterized in that, The amount of stabilizer added is 0.5-1.7% of industrial-grade hydrogen peroxide.

7. The method for preparing electronic-grade hydrogen peroxide as described in claim 1, characterized in that, The filter membranes of the multi-stage precision filtration system are 1.0 μm, 0.2 μm, and 0.1 μm, respectively.

8. The method for preparing electronic-grade hydrogen peroxide as described in claim 1, characterized in that, The flow rate when the adsorption column is introduced is 3-4 L / h, and the adsorption temperature is 25-30℃.

9. The method for preparing electronic-grade hydrogen peroxide as described in claim 1, characterized in that, The primary and secondary filter membranes have a diameter of 0.01 μm and 0.001 μm, respectively.

Citation Information

Patent Citations

  • Method for producing ultra-pure hydrogen peroxide

    CN102485642A

  • Preparation method and application of adsorbent for purifying hydrogen peroxide

    CN108499524A