Process method for preparing hydrogen peroxide with different standard grades from industrial-grade hydrogen peroxide

Abstract

The invention belongs to the technical field of hydrogen peroxide production, and provides a process method for preparing hydrogen peroxide with different standard grades from industrial-grade hydrogen peroxide, and the process method comprises the following steps: S1, preparing primary raw material hydrogen peroxide; s2, enabling the primary raw material hydrogen peroxide to pass through a purification tower, a coalescence separator, a resin exchange column and a resin filter to obtain G1 food-grade and reagent-grade hydrogen peroxide; s3, enabling G1 food-grade and reagent-grade hydrogen peroxide to pass through an RO (Reverse Osmosis) unit to obtain G2 electronic-grade hydrogen peroxide; s4, passing the G2 electronic-grade hydrogen peroxide through 1 #, 2 # and 3 # ion exchange columns and a G3 filter to obtain G3 electronic-grade hydrogen peroxide; s5, enabling the G3 electronic-grade hydrogen peroxide to pass through 4 #, 5 #, 6 # and 7 # ion exchange columns and a G4 filter to obtain G4 electronic-grade hydrogen peroxide; s6, enabling the G4 electronic-grade hydrogen peroxide to pass through 8 #, 9 #, 10 #, 11 # and 12 # ion exchange columns and a G5 filter to obtain G5 electronic-grade hydrogen peroxide. By means of the single production line, product diversification can be achieved, in addition, the product quality can be improved, and the production cost can be saved.

Description

Technical Field

[0001] The invention relates to the technical field of hydrogen peroxide production, and in particular to a process for preparing hydrogen peroxide of different standard grades from industrial-grade hydrogen peroxide. Background Art

[0002] With the rapid development of the electronics industry, especially with the high integration of integrated circuits, the demand for electronic-grade hydrogen peroxide has increased dramatically. Electronic-grade hydrogen peroxide is widely used in the electronics industry and is one of the electronic chemicals necessary for the production of integrated circuits. Its purity has a very important impact on the yield, electrical properties and reliability of integrated circuits. However, my country's high-purity electronic-grade hydrogen peroxide companies generally have small production scales and low technical levels, which cannot meet the needs of the high-end market.

[0003] The invention patent application with publication number CN118651823A discloses a production process of ultra-high purity electronic grade hydrogen peroxide, which uses industrial hydrogen peroxide as raw material and can fully remove impurities in industrial hydrogen peroxide through specific process treatment, thereby preparing an ultra-high purity electronic grade hydrogen peroxide, which can meet the use requirements in the integrated circuit preparation process. In the prior art, adsorption resin or ion exchange resin is generally used for purification in a multi-stage series manner, or distillation and concentration, etc., but this method has limited purification effect and cannot meet the use standard of electronic grade hydrogen peroxide. In addition, the resin is not regenerated, the service life of the resin is short, the amount of solid waste treatment is large, and the product standard grade is vague, collectively referred to as ultra-high purity electronic grade hydrogen peroxide, and different grades of hydrogen peroxide cannot be accurately obtained. Summary of the invention

[0004] In view of the technical problems in the prior art, the present invention provides a process for preparing hydrogen peroxide of different standard grades from industrial-grade hydrogen peroxide, comprising the following steps: S1, pre-treating the industrial-grade hydrogen peroxide in the industrial-grade hydrogen peroxide storage tank to obtain primary raw material hydrogen peroxide; S2, the primary raw material hydrogen peroxide is passed through a purification tower, a coalescing separator, a resin exchange column and a resin filter to obtain G1 food grade and reagent grade hydrogen peroxide; S3, G1 food grade and reagent grade hydrogen peroxide are passed through an RO reverse osmosis unit to obtain G2 electronic grade hydrogen peroxide; S4, passing the G2 electronic grade hydrogen peroxide through a 1# ion exchange column, a 2# ion exchange column, a 3# ion exchange column and a G3 hydrogen peroxide filter in sequence to obtain a G3 electronic grade hydrogen peroxide; S5, passing the G3 electronic grade hydrogen peroxide through a 4# ion exchange column, a 5# ion exchange column, a 6# ion exchange column, a 7# ion exchange column and a G4 hydrogen peroxide filter in sequence to obtain a G4 electronic grade hydrogen peroxide; S6. G5 electronic grade hydrogen peroxide is obtained by passing G4 electronic grade hydrogen peroxide through 8# ion exchange column, 9# ion exchange column, 10# ion exchange column, 11# ion exchange column, 12# ion exchange column and G5 hydrogen peroxide filter in sequence.

[0005] Furthermore, the pretreatment in step S1 includes cooling the industrial-grade hydrogen peroxide in an industrial-grade hydrogen peroxide cooler, adding a stabilizer, and statically mixing the industrial-grade hydrogen peroxide with the cooled ultra-high purity water, followed by cooling and filtering the industrial-grade hydrogen peroxide with a raw material filter.

[0006] Furthermore, the purification tower and the coalescing separator in step S2 are both made of 316L / EP.

[0007] Furthermore, the material of the 1# ion exchange column, 2# ion exchange column, 3# ion exchange column and G3 hydrogen peroxide filter in step S4 is 316L / EP+lined with PTFE.

[0008] Furthermore, the materials of the 4# ion exchange column, 5# ion exchange column, 6# ion exchange column, 7# ion exchange column and G4 hydrogen peroxide filter in step S5 are all 316L / EP+lined with PFA.

[0009] Furthermore, the materials of the 8# ion exchange column, 9# ion exchange column, 10# ion exchange column, 11# ion exchange column and 12# ion exchange column in step S6 are all 316L / EP+lined with PFA, and the material of the G5 hydrogen peroxide filter is 316L / EP.

[0010] Furthermore, the total organic carbon of the G1 food grade and reagent grade hydrogen peroxide is less than 70 ppm, the total organic carbon of the G2 electronic grade hydrogen peroxide, G3 electronic grade hydrogen peroxide and G4 electronic grade hydrogen peroxide are all less than 20 ppm, and the total organic carbon of the G5 electronic grade hydrogen peroxide is less than 10 ppm.

[0011] Beneficial effects: 1. In the present invention, a single production line can achieve product diversification and a high degree of automatic integration. In addition, the use of professional equipment with improved materials combined with relevant technologies can improve product quality and reduce the number of replacements of membranes, resins, and filter elements, thereby saving production costs.

[0012] 2. In the present invention, by setting the concentration of total organic carbon in hydrogen peroxide, the product standard grade can be clarified, so that the corresponding grade of hydrogen peroxide can be reasonably matched for different purposes. Specifically, G1 food-grade and reagent-grade hydrogen peroxide are used in food additives, disinfection, cleaning and laboratory additives; G2 electronic-grade hydrogen peroxide is used in the cleaning and texturing process of photovoltaic cells to remove impurities on the surface of silicon wafers; G3 electronic-grade hydrogen peroxide is used in the cleaning of photovoltaic cells and the cleaning of display panels to remove impurities on the surface; G4 electronic-grade hydrogen peroxide is used in the cleaning process of display panel manufacturing process, the solution cleans the surface of the substrate, and removes impurities such as metal foreign matter; G5 electronic-grade hydrogen peroxide is used in the cleaning process of chip manufacturing process, the solution cleans the surface of the substrate, and removes impurities such as metal foreign matter. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0014] Figure 1 It is a flow chart of the present invention. DETAILED DESCRIPTION

[0015] In order to make the above-mentioned purposes, features and advantages of the present application more obvious and easy to understand, the specific implementation methods of the present application are described in detail below in conjunction with the accompanying drawings. In the following description, many specific details are set forth to facilitate a full understanding of the present application. However, the present application can be implemented in many other ways different from those described herein, and those skilled in the art can make similar improvements without violating the connotation of the present application, so the present application is not limited by the specific embodiments disclosed below.

[0016] In the description of the present application, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present application and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation on the present application.

[0017] In addition, the terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features defined as "first" and "second" may explicitly or implicitly include at least one of the features. In the description of this application, the meaning of "plurality" is at least two, such as two, three, etc., unless otherwise clearly and specifically defined.

[0018] In this application, unless otherwise clearly specified and limited, the terms "installed", "connected", "connected", "fixed" and the like should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements, unless otherwise clearly defined. For ordinary technicians in this field, the specific meanings of the above terms in this application can be understood according to specific circumstances.

[0019] In the present application, unless otherwise clearly specified and limited, a first feature being “above” or “below” a second feature may mean that the first and second features are in direct contact, or the first and second features are in indirect contact through an intermediate medium. Moreover, a first feature being “above”, “above”, and “above” a second feature may mean that the first feature is directly above or obliquely above the second feature, or simply means that the first feature is higher in level than the second feature. A first feature being “below”, “below”, and “below” a second feature may mean that the first feature is directly below or obliquely below the second feature, or simply means that the first feature is lower in level than the second feature.

[0020] It should be noted that when an element is referred to as being "fixed to" or "disposed on" another element, it may be directly on the other element or there may be a central element. When an element is considered to be "connected to" another element, it may be directly connected to the other element or there may be a central element at the same time. The terms "vertical", "horizontal", "upper", "lower", "left", "right" and similar expressions used herein are for illustrative purposes only and are not intended to be the only implementation method.

[0021] The present invention provides a process for preparing different standard grades of hydrogen peroxide from industrial grade hydrogen peroxide, such as Figure 1 As shown, the following steps are included: S1. Pre-treating the industrial-grade hydrogen peroxide in the industrial-grade hydrogen peroxide storage tank to obtain primary raw material hydrogen peroxide, wherein the pre-treatment includes cooling the industrial-grade hydrogen peroxide in an industrial-grade hydrogen peroxide cooler, adding a stabilizer, and statically mixing the industrial-grade hydrogen peroxide with the cooled ultra-high purity water, and then cooling and filtering the raw material filter, wherein the raw material filter is used to remove impurities in the material, and the primary raw material hydrogen peroxide can be further processed according to user needs to obtain products of different concentrations; S2. The primary raw material hydrogen peroxide is passed through a purification tower, a coalescing separator, a resin exchange column and a resin filter to obtain G1 food grade and reagent grade hydrogen peroxide. The purification tower and the coalescing separator are both made of 316L / EP. The purification tower is used to purify and remove impurities, and the coalescing separator is used to reduce the total organic carbon (TOC) content. S3, G1 food-grade and reagent-grade hydrogen peroxide is passed through a RO reverse osmosis unit to obtain G2 electronic-grade hydrogen peroxide, wherein the RO reverse osmosis unit includes an oxidation-resistant desalination membrane and a brackish water desalination membrane, which can remove more than 97% of organic carbon impurities and anions and cations; S4, G2 electronic grade hydrogen peroxide is passed through 1# ion exchange column, 2# ion exchange column, 3# ion exchange column and G3 hydrogen peroxide filter in sequence to obtain G3 electronic grade hydrogen peroxide, wherein the material of 1# ion exchange column, 2# ion exchange column, 3# ion exchange column and G3 hydrogen peroxide filter is 316L / EP+lined with PTFE, wherein the ion exchange column is used to remove metal ions in hydrogen peroxide, and a convenient unloading design is adopted inside; S5, G3 electronic grade hydrogen peroxide is passed through 4# ion exchange column, 5# ion exchange column, 6# ion exchange column, 7# ion exchange column and G4 hydrogen peroxide filter in sequence to obtain G4 electronic grade hydrogen peroxide, wherein the materials of 4# ion exchange column, 5# ion exchange column, 6# ion exchange column, 7# ion exchange column and G4 hydrogen peroxide filter are all 316L / EP+lined with PFA; S6. G4 electronic grade hydrogen peroxide is sequentially passed through an 8# ion exchange column, a 9# ion exchange column, a 10# ion exchange column, a 11# ion exchange column, a 12# ion exchange column and a G5 hydrogen peroxide filter to obtain G5 electronic grade hydrogen peroxide. The materials of the 8# ion exchange column, the 9# ion exchange column, the 10# ion exchange column, the 11# ion exchange column and the 12# ion exchange column are all 316L / EP+lined with PFA, and the material of the G5 hydrogen peroxide filter is 316L / EP.

[0022] In this embodiment, a single production line can achieve product diversification with a high degree of automatic integration. In addition, the use of professional equipment with improved materials combined with related technologies can improve product quality and reduce the number of replacement times of membranes, resins, and filter elements, thereby saving production costs.

[0023] In the present invention, preferably, Figure 1 As shown, the total organic carbon of the G1 food grade and reagent grade hydrogen peroxide is less than 70 ppm, the total organic carbon of the G2 electronic grade hydrogen peroxide, the G3 electronic grade hydrogen peroxide and the G4 electronic grade hydrogen peroxide are all less than 20 ppm, and the total organic carbon of the G5 electronic grade hydrogen peroxide is less than 10 ppm. For specific parameters, see Table 1.

[0024] Table 1

[0025] In this embodiment, by setting the concentration of total organic carbon in hydrogen peroxide, the product standard grade can be clarified, so that the corresponding grade of hydrogen peroxide can be reasonably matched for different purposes. Specifically, G1 food-grade and reagent-grade hydrogen peroxide uses: mainly used in food additives, disinfection, cleaning and laboratory additives; G2 electronic-grade hydrogen peroxide uses: mainly used in the cleaning and texturing process of photovoltaic cells to remove impurities on the surface of silicon wafers; G3 electronic-grade hydrogen peroxide uses: mainly used in the cleaning of photovoltaic cells and the cleaning of display panels to remove impurities on the surface; G4 electronic-grade hydrogen peroxide uses: mainly used in the cleaning process of display panel manufacturing process, the solution cleans the surface of the substrate, and removes impurities such as metal foreign matter; G5 electronic-grade hydrogen peroxide uses: mainly used in the cleaning process of chip manufacturing process, the solution cleans the surface of the substrate, and removes impurities such as metal foreign matter.

[0026] The technical features of the above-described embodiments may be arbitrarily combined. To make the description concise, not all possible combinations of the technical features in the above-described embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0027] The above-described embodiments only express several implementation methods of the present application, and the descriptions thereof are relatively specific and detailed, but they cannot be construed as limiting the scope of the patent application. It should be pointed out that, for a person of ordinary skill in the art, several variations and improvements can be made without departing from the concept of the present application, and these all belong to the protection scope of the present application. Therefore, the protection scope of the patent application shall be subject to the attached claims.

Claims

1. A process for preparing hydrogen peroxide of different standard grades from industrial-grade hydrogen peroxide, characterized in that: The following steps are involved: S1, pre-treating the industrial-grade hydrogen peroxide in the industrial-grade hydrogen peroxide storage tank to obtain primary raw material hydrogen peroxide; S2, the primary raw material hydrogen peroxide is passed through a purification tower, a coalescing separator, a resin exchange column and a resin filter to obtain G1 food grade and reagent grade hydrogen peroxide; S3, G1 food grade and reagent grade hydrogen peroxide are passed through an RO reverse osmosis unit to obtain G2 electronic grade hydrogen peroxide; S4, passing the G2 electronic grade hydrogen peroxide through a 1# ion exchange column, a 2# ion exchange column, a 3# ion exchange column and a G3 hydrogen peroxide filter in sequence to obtain a G3 electronic grade hydrogen peroxide; S5, passing the G3 electronic grade hydrogen peroxide through a 4# ion exchange column, a 5# ion exchange column, a 6# ion exchange column, a 7# ion exchange column and a G4 hydrogen peroxide filter in sequence to obtain a G4 electronic grade hydrogen peroxide; S6. G5 electronic grade hydrogen peroxide is obtained by passing G4 electronic grade hydrogen peroxide through 8# ion exchange column, 9# ion exchange column, 10# ion exchange column, 11# ion exchange column, 12# ion exchange column and G5 hydrogen peroxide filter in sequence.

2. A process for preparing hydrogen peroxide of different standard grades from industrial-grade hydrogen peroxide according to claim 1, characterized in that: The pretreatment in step S1 includes cooling the industrial-grade hydrogen peroxide in an industrial-grade hydrogen peroxide cooler, adding a stabilizer, and statically mixing the industrial-grade hydrogen peroxide with the cooled ultra-high-purity water, followed by cooling and filtering with a raw material filter.

3. A process for preparing different standard grades of hydrogen peroxide from industrial grade hydrogen peroxide according to claim 1, characterized in that: The materials of the purification tower and the coalescing separator in step S2 are both 316L / EP.

4. A process for preparing hydrogen peroxide of different standard grades from industrial grade hydrogen peroxide according to claim 1, characterized in that: The material of the 1# ion exchange column, 2# ion exchange column, 3# ion exchange column and G3 hydrogen peroxide filter in step S4 is 316L / EP+lined with PTFE.

5. A process for preparing different standard grades of hydrogen peroxide from industrial grade hydrogen peroxide according to claim 1, characterized in that: The materials of the 4# ion exchange column, 5# ion exchange column, 6# ion exchange column, 7# ion exchange column and G4 hydrogen peroxide filter in step S5 are all 316L / EP+lined with PFA.

6. A process for preparing different standard grades of hydrogen peroxide from industrial grade hydrogen peroxide according to claim 1, characterized in that: The materials of the 8# ion exchange column, 9# ion exchange column, 10# ion exchange column, 11# ion exchange column and 12# ion exchange column in step S6 are all 316L / EP+lined with PFA, and the material of the G5 hydrogen peroxide filter is 316L / EP.

7. The process for preparing hydrogen peroxide of different standard grades from industrial-grade hydrogen peroxide according to claim 1, characterized in that: The total organic carbon of the G1 food grade and reagent grade hydrogen peroxide is less than 70 ppm, the total organic carbon of the G2 electronic grade hydrogen peroxide, the G3 electronic grade hydrogen peroxide and the G4 electronic grade hydrogen peroxide are all less than 20 ppm, and the total organic carbon of the G5 electronic grade hydrogen peroxide is less than 10 ppm.

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