Production process of ultra-pure electronic-grade hydrogen peroxide

Abstract

The invention is suitable for the technical field of preparation of ultra-pure electronic grade hydrogen peroxide, and provides an ultra-pure electronic grade hydrogen peroxide production process, which comprises the following steps: step (1), dilution: pumping industrial grade hydrogen peroxide with the mass fraction of 50% temporarily stored in a hydrogen peroxide storage tank into a workshop blending diluter through a centrifugal pump, adding pure water for dilution, pumping into a cooler for cooling, and controlling the temperature of hydrogen peroxide; (2) adsorption: pumping the diluted hydrogen peroxide into a reverse osmosis membrane, an anion exchange bed and a cation exchange bed in sequence, and adsorbing to remove macromolecular organic matters, anion impurities and cation impurities in the hydrogen peroxide; (3) filtering: pumping the hydrogen peroxide subjected to adsorption purification into a precision filter, and filtering; and step (4), filling: filling qualified products after filtration. According to the scheme, the operation is simple, the flow is few, the production efficiency is improved, the production cost is reduced, and meanwhile, the product quality is ensured to meet the strict requirements of the electronic-grade hydrogen peroxide.

Description

Technical Field

[0001] The invention relates to the technical field of ultra-high purity electronic grade hydrogen peroxide preparation, in particular to a production process of ultra-high purity electronic grade hydrogen peroxide. Background Art

[0002] Hydrogen peroxide, chemically known as hydrogen peroxide and with the chemical formula H2O2, is a common chemical substance widely used in disinfection, cleaning, bleaching, etc. It is a colorless liquid with a slight pungent odor and is soluble in water.

[0003] Ultra-high purity electronic grade hydrogen peroxide, commonly known as electronic grade hydrogen peroxide or electronic grade H2O2, is a highly pure hydrogen peroxide that is specifically used in high-tech industries such as semiconductors, microelectronics, and photovoltaics, especially in chip manufacturing, photovoltaic panel production, etc. Compared with conventional hydrogen peroxide, electronic grade hydrogen peroxide has extremely strict requirements on purity and impurity control, usually requiring a purity of 99.999% or higher.

[0004] Ultra-high purity electronic grade hydrogen peroxide has extremely high purity, low impurity content and stability. It has several main applications:

[0005] ①. Semiconductor manufacturing: Ultra-high purity electronic grade hydrogen peroxide is used for cleaning and surface treatment of silicon wafers. During the wafer production process, high-purity hydrogen peroxide is needed to remove organic matter and metal impurities on the surface of the wafer to ensure the accuracy and quality of subsequent processes.

[0006] ②. Photovoltaic industry: In the production process of solar cells, ultra-high purity electronic grade hydrogen peroxide is used to clean the surface of silicon wafers, remove tiny impurities and pollutants, and ensure battery efficiency.

[0007] ③. Cleaning and etching: In the manufacturing process of integrated circuits, ultra-high purity electronic grade hydrogen peroxide is used as an etching solution or cleaning agent to remove excess material layers or contaminants to ensure the fineness of the circuit.

[0008] ④. Chemical synthesis and analysis: In some high-precision chemical synthesis reactions, ultra-high purity electronic grade hydrogen peroxide is also used as an oxidant, which requires extremely high purity to avoid interference from impurities.

[0009] The production process of ultra-high purity electronic grade hydrogen peroxide is usually more complicated than that of conventional hydrogen peroxide. Special equipment and technology are required during the production process to ensure high purity and avoid contamination by impurities such as dust and metal ions in the air.

[0010] At present, common methods for producing ultra-high purity electronic-grade hydrogen peroxide on the market include distillation, ion exchange, membrane separation, etc. These methods have their own advantages and disadvantages, but they all face the challenges of high cost, low efficiency and difficulty in achieving higher purity. Therefore, it is urgent to develop a new production process to improve production efficiency, reduce costs, and ensure product quality. To this end, the present invention proposes a production process for ultra-high purity electronic-grade hydrogen peroxide. Summary of the invention

[0011] The purpose of the present invention is to provide a process for producing ultra-high purity electronic-grade hydrogen peroxide to solve the problems that most common ultra-high purity electronic-grade hydrogen peroxide production methods in the prior art face the challenges of high cost, low efficiency and difficulty in achieving higher purity.

[0012] To achieve the above object, the present invention provides the following technical solution: a process for producing ultra-high purity electronic grade hydrogen peroxide, comprising the following steps:

[0013] Step (1), dilution:

[0014] The 50% industrial grade hydrogen peroxide temporarily stored in the hydrogen peroxide storage tank is pumped into the workshop mixing and diluting device through a centrifugal pump, diluted with pure water, and pumped into the cooler for cooling, and the temperature of the hydrogen peroxide is controlled;

[0015] Step (2), adsorption:

[0016] The diluted hydrogen peroxide is pumped into the reverse osmosis membrane, the anion exchange bed and the cation exchange bed in sequence to adsorb and remove the macromolecular organic matter, anion impurities and cationic impurities in the hydrogen peroxide;

[0017] Step (3), filtering:

[0018] Pump the purified hydrogen peroxide after adsorption into a precision filter for filtration;

[0019] Step (4), filling:

[0020] Fill the filtered qualified products.

[0021] Preferably, the mass fraction of the diluted hydrogen peroxide in step (1) is 31%.

[0022] Preferably, after dilution and cooling in step (1), the temperature of the hydrogen peroxide solution is controlled to be below 20°C.

[0023] Preferably, the anionic impurities adsorbed and removed in step (2) include SO4 2- PO4 3- 、NO3 - and Cl - .

[0024] Preferably, the cationic impurities removed by adsorption in step (2) include Na + , K + , Fe 3+ and Ca + .

[0025] Preferably, the detailed steps of step (2) are as follows:

[0026] Step (21), pumping the diluted hydrogen peroxide into a reverse osmosis membrane to remove macromolecular organic matter in the hydrogen peroxide, and then transferring it to buffer tank No. 1;

[0027] Step (22), pumping the hydrogen peroxide solution in buffer tank No. 1 into the anion exchange bed to remove anionic impurities in the hydrogen peroxide, and then transferring it to buffer tank No. 2;

[0028] Step (23), pumping the hydrogen peroxide in buffer tank No. 2 into the cation exchange bed to remove the cations in the hydrogen peroxide, and then transferring it to buffer tank No. 3.

[0029] Preferably, the specific steps of filtering in step (3) are as follows:

[0030] The hydrogen peroxide that has been purified by adsorption is pumped into the precision filter, filtered through the filter, and the filter residue enters the filter. After cyclic filtration and testing, the product with qualified particles can be filled. If the particles are unqualified, the cyclic filtration time will be extended.

[0031] Preferably, the filter has a specification of 0.2um.

[0032] Preferably, the filling in step (4) is carried out in a Class 10,000 clean room in the workshop and under a Class 100 laminar flow hood.

[0033] Preferably, the filling in step (4) is carried out at 20±5°C and normal pressure.

[0034] The present invention has at least the following beneficial effects:

[0035] The invention provides an ultra-high purity electronic grade hydrogen peroxide production process, which is simple to operate and has fewer processes, thus not only improving production efficiency but also reducing production costs, while ensuring that product quality meets the strict requirements of electronic grade hydrogen peroxide. BRIEF DESCRIPTION OF THE DRAWINGS

[0036] Figure 1 It is a schematic diagram of the process structure of the present invention. DETAILED DESCRIPTION

[0037] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0038] Example

[0039] like Figure 1 As shown, this embodiment provides a process for producing ultra-high purity electronic grade hydrogen peroxide, comprising the following steps:

[0040] Step (1), dilution:

[0041] The 50% industrial grade hydrogen peroxide temporarily stored in the hydrogen peroxide storage tank is pumped into the workshop mixing and diluting device through a centrifugal pump, diluted with pure water to a concentration of 31% by mass, and pumped into the cooler for cooling (primary circulating cooling water), and the temperature of the hydrogen peroxide is controlled below 20°C;

[0042] Step (2), adsorption:

[0043] The diluted hydrogen peroxide is pumped into the reverse osmosis membrane to remove the macromolecular organic matter in the hydrogen peroxide, and then transferred to the No. 1 buffer tank;

[0044] The hydrogen peroxide solution in buffer tank No. 1 is pumped into the anion exchange bed to remove anionic impurities in the hydrogen peroxide solution, and then transferred to buffer tank No. 2;

[0045] Pump the hydrogen peroxide in buffer tank No. 2 into the cation exchange bed to remove the cations in the hydrogen peroxide, and then transfer it to buffer tank No. 3;

[0046] Among them, anionic impurities include SO4 2- PO4 3- 、NO3 - and Cl - ; cations include Na + , K + , Fe 3+ and Ca + ;

[0047] Step (3), filtering:

[0048] The hydrogen peroxide that has been purified by adsorption is pumped into the precision filter and filtered through a 0.2um filter. The filter residue enters the filter. Products that are found to be qualified after cyclic filtration and particle testing can be filled. If the particles are unqualified, the cyclic filtration time is extended.

[0049] Step (4), filling:

[0050] Qualified products are filled in the 10,000-grade clean room in the workshop (temperature is 20±5℃, normal pressure) and the filling is carried out on the filling table under the 100-grade laminar flow hood.

[0051] The products prepared in the above examples were tested for various indicators, and the results are shown in the following table:

[0052]

[0053]

[0054]

[0055] In summary, the production process provided by the present invention ensures the high purity and low impurity content of the final product through a series of purification steps. The process is simple to operate and has few processes, which not only improves production efficiency but also reduces production costs, while ensuring that the product quality meets the strict requirements of electronic-grade hydrogen peroxide. The problems existing in the prior art can be effectively solved, and a new production method of ultra-high-purity electronic-grade hydrogen peroxide is provided for high-tech industries such as semiconductors, microelectronics, and photovoltaics.

[0056] The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention. It is obvious to those skilled in the art that the present invention is not limited to the details of the above exemplary embodiments, and the present invention can be implemented in other specific forms without departing from the spirit or basic features of the present invention. Therefore, no matter from which point of view, the embodiments should be regarded as exemplary and non-restrictive. The scope of the present invention is defined by the appended claims rather than the above description, and it is intended that all changes falling within the meaning and scope of the equivalent elements of the claims are included in the present invention.

[0057] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A process for producing ultra-high purity electronic grade hydrogen peroxide, characterized in that: The following steps are involved: Step (1), dilution: The 50% industrial grade hydrogen peroxide temporarily stored in the hydrogen peroxide storage tank is pumped into the workshop mixing and diluting device through a centrifugal pump, diluted with pure water, and pumped into the cooler for cooling, and the temperature of the hydrogen peroxide is controlled; Step (2), adsorption: The diluted hydrogen peroxide is pumped into the reverse osmosis membrane, the anion exchange bed and the cation exchange bed in sequence to adsorb and remove the macromolecular organic matter, anion impurities and cationic impurities in the hydrogen peroxide; Step (3), filtering: Pump the purified hydrogen peroxide after adsorption into a precision filter for filtration; Step (4), filling: Fill the filtered qualified products.

2. A process for producing ultra-high purity electronic grade hydrogen peroxide according to claim 1, characterized in that: The mass fraction of the diluted hydrogen peroxide in step (1) is 31%.

3. A process for producing ultra-high purity electronic grade hydrogen peroxide according to claim 1, characterized in that: After dilution and cooling in step (1), the temperature of the hydrogen peroxide solution is controlled to be below 20°C.

4. A process for producing ultra-high purity electronic grade hydrogen peroxide according to claim 1, characterized in that: The anionic impurities adsorbed and removed in step (2) include SO4 2 - PO4 3 - 、NO 3- and Cl-.

5. A process for producing ultra-high purity electronic grade hydrogen peroxide according to claim 1, characterized in that: The cationic impurities removed by adsorption in step (2) include Na + , K + , Fe 3+ and Ca + .

6. A process for producing ultra-high purity electronic grade hydrogen peroxide according to claim 1, characterized in that: The detailed steps of step (2) are as follows: Step (21), pumping the diluted hydrogen peroxide into a reverse osmosis membrane to remove macromolecular organic matter in the hydrogen peroxide, and then transferring it to buffer tank No. 1; Step (22), pumping the hydrogen peroxide solution in buffer tank No. 1 into the anion exchange bed to remove anionic impurities in the hydrogen peroxide, and then transferring it to buffer tank No. 2; Step (23), pumping the hydrogen peroxide in buffer tank No. 2 into the cation exchange bed to remove the cations in the hydrogen peroxide, and then transferring it to buffer tank No.

3.

7. A process for producing ultra-high purity electronic grade hydrogen peroxide according to claim 1, characterized in that: The specific steps of filtering in step (3) are as follows: The hydrogen peroxide that has been purified by adsorption is pumped into the precision filter, filtered through the filter, and the filter residue enters the filter. After cyclic filtration and testing, the product with qualified particles can be filled. If the particles are unqualified, the cyclic filtration time will be extended.

8. A process for producing ultra-high purity electronic grade hydrogen peroxide according to claim 7, characterized in that: The specification of the filter is 0.2um.

9. A process for producing ultra-high purity electronic grade hydrogen peroxide according to claim 1, characterized in that: The filling in step (4) is carried out in a Class 10,000 clean room in the workshop and under a Class 100 laminar flow hood.

10. A process for producing ultra-high purity electronic grade hydrogen peroxide according to claim 9, characterized in that: The filling in step (4) is carried out at 20±5°C and normal pressure.

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