Continuous purification method of hydrogen peroxide and hydrogen peroxide prepared by continuous purification method
By using ultra-low temperature and ultrasonic oscillation combined with membrane filtration during the hydrogen peroxide purification process, the problem of poor purification effect in the prior art was solved, and efficient removal of organic matter and achieving high purity hydrogen peroxide production.
Patent Information
- Application Number
- CN202510295067.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2023-02-23
- Publication Date
- 2025-06-13
AI Technical Summary
The prior art has problems such as high energy consumption, complex operation and poor purification effect in the purification process of hydrogen peroxide. Especially when removing organic matter, it is difficult to meet the requirements of semiconductor-level ultra-high purity.
The method of using ultra-low temperature and ultrasonic oscillation to assist membrane filtration to separate organic matter in hydrogen peroxide, combined with multi-stage sequential treatment, and control the residence time of ultrasonic oscillation in each stage, and the method of combining membrane filtration with multi-stage pore diameters.
It effectively reduces the content of organic impurities in hydrogen peroxide, reaches the ppb level, or even below 10 ppb, improves the purification effect, and extends the service life of subsequent resin towers.
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Figure CN120136039A_ABST
Abstract
Description
[0001] This invention is a divisional application of a Chinese invention patent application with an application date of February 23, 2023, application number 2023101612502, and name “A method for purifying hydrogen peroxide”. Technical Field
[0002] The invention relates to the technical field of hydrogen peroxide purification, and in particular to a continuous purification method for hydrogen peroxide and the hydrogen peroxide prepared therefrom. Background Art
[0003] Hydrogen peroxide, also known as hydrogen peroxide, is a blue viscous liquid that is soluble in water, alcohol, and ether, but insoluble in benzene and petroleum ether. Its aqueous solution is a colorless and transparent liquid. It is an important inorganic chemical product and is widely used in the fields of chemical industry, medicine, electronics, food, textile, papermaking, light industry, military industry, environmental protection, etc. Industrial hydrogen peroxide contains more organic impurities and cannot meet the needs of the electronics industry or the food industry, so it is necessary to remove the organic impurities in hydrogen peroxide.
[0004] At present, the purification method for industrial hydrogen peroxide is mostly to use multiple resin towers in series, and use resin adsorption and resin ion exchange for purification, specifically, an organic matter (TOC) resin adsorption tower, a cation exchange resin tower and an anion exchange resin tower are arranged in series. However, since the organic matter (TOC) content contained in industrial hydrogen peroxide is generally high and there are many ionic impurities, when the above-mentioned resin adsorption and anion and cation exchange methods are used, there is a large load and high energy consumption, and the resin filler in the resin tower needs to be frequently replaced or regenerated, which is too costly; and the strong oxidizing property, heat sensitivity and instability of hydrogen peroxide limit the application of various conventional purification methods.
[0005] In view of the above problems, Chinese patent CN112723316A discloses a purification method for removing organic matter from hydrogen peroxide at low temperature, which mainly includes a cooling stage and a filtering stage performed in sequence, wherein the cooling stage is to cool the industrial-grade hydrogen peroxide to 0-8°C (preferably 4-8°C), and the filtering stage is to filter the cooled hydrogen peroxide using a membrane filter to remove TOC. However, in the patent document, the organic matter (TOC) content of hydrogen peroxide treated by the purification method is still as high as tens of ppm, which is difficult to meet the high standard requirements of semiconductor-grade ultra-high purity hydrogen peroxide. Summary of the invention
[0006] The object of the present invention is to overcome one or more deficiencies of the prior art and provide an improved continuous purification method for hydrogen peroxide, which can eliminate the need for an additional resin column during the removal of organic matter (TOC) stage, ensure that the hydrogen peroxide entering the subsequent anion and cation resin columns has a high purity, thereby improving the service life of the subsequent resin columns, and the content of organic matter (TOC) in the hydrogen peroxide after treatment is less than 10 ppb.
[0007] To achieve the above object, the technical solution adopted by the present invention is: a purification method for hydrogen peroxide, using industrial-grade hydrogen peroxide as a raw material, the purification method comprising:
[0008] Adjust the mass percentage concentration of industrial-grade hydrogen peroxide to 30%-40%, control the feed temperature of the system to be 0-5°C, and then make the treated hydrogen peroxide flow through n organic matter treatment units arranged in series in turn, where n is greater than or equal to 2;
[0009] Each of the organic matter treatment units independently includes an ultrasonic treatment device and a membrane filtration device connected in sequence. In each of the organic matter treatment units, the hydrogen peroxide is subjected to oscillation treatment by the ultrasonic treatment device and filtration treatment by the membrane filtration device in turn;
[0010] Control the residence time of the hydrogen peroxide in the ultrasonic treatment device included in the subsequent organic matter treatment unit to be longer than the residence time of the ultrasonic treatment device included in the previous organic matter treatment unit;
[0011] Control the pore size of the filter element of the membrane filtration device included in the subsequent organic matter treatment unit to be smaller than the pore size of the filter element of the membrane filtration device included in the previous organic matter treatment unit.
[0012] According to some preferred aspects of the present invention, n is 3, 4 or 5.
[0013] According to some preferred aspects of the present invention, the working frequency of the ultrasonic treatment device is 25-40 kHz.
[0014] According to some preferred aspects of the present invention, control the residence time of the hydrogen peroxide in the ultrasonic treatment device included in the subsequent organic matter treatment unit to be 1.2-3 times the residence time of the ultrasonic treatment device included in the previous organic matter treatment unit.
[0015] In some embodiments of the present invention, control the residence time of the hydrogen peroxide in the ultrasonic treatment device included in the subsequent organic matter treatment unit to be 1.2-1.5 times the residence time of the ultrasonic treatment device included in the previous organic matter treatment unit.
[0016] In some embodiments of the present invention, the residence time of hydrogen peroxide in the ultrasonic treatment device included in the latter-stage organic matter treatment unit is controlled to be 1.5 - 2.0 times that in the ultrasonic treatment device included in the former-stage organic matter treatment unit.
[0017] In some embodiments of the present invention, the residence time of hydrogen peroxide in the ultrasonic treatment device included in the latter-stage organic matter treatment unit is controlled to be 2.0 - 3.0 times that in the ultrasonic treatment device included in the former-stage organic matter treatment unit.
[0018] According to some preferred aspects of the present invention, the pore diameter of the filter element of the membrane filtration device included in the latter-stage organic matter treatment unit is controlled to be 0.05 - 0.8 times that of the filter element of the membrane filtration device included in the former-stage organic matter treatment unit.
[0019] In some embodiments of the present invention, the pore diameter of the filter element of the membrane filtration device included in the latter-stage organic matter treatment unit is controlled to be 0.05 - 0.15 times that of the filter element of the membrane filtration device included in the former-stage organic matter treatment unit.
[0020] In some embodiments of the present invention, the pore diameter of the filter element of the membrane filtration device included in the latter-stage organic matter treatment unit is controlled to be 0.2 - 0.35 times that of the filter element of the membrane filtration device included in the former-stage organic matter treatment unit.
[0021] In some embodiments of the present invention, the pore diameter of the filter element of the membrane filtration device included in the latter-stage organic matter treatment unit is controlled to be 0.35 - 0.55 times that of the filter element of the membrane filtration device included in the former-stage organic matter treatment unit.
[0022] In some embodiments of the present invention, the pore diameter of the filter element of the membrane filtration device included in the latter-stage organic matter treatment unit is controlled to be 0.55 - 0.8 times that of the filter element of the membrane filtration device included in the former-stage organic matter treatment unit.
[0023] According to some preferred and specific aspects of the present invention, when n is 3, the treated hydrogen peroxide is made to flow sequentially through a first-stage ultrasonic treatment device, a first-stage membrane filtration device, a second-stage ultrasonic treatment device, a second-stage membrane filtration device, a third-stage ultrasonic treatment device, and a third-stage membrane filtration device arranged in series.
[0024] According to some preferred and specific aspects of the present invention, the residence times of the primary ultrasonic treatment device, the secondary ultrasonic treatment device, and the tertiary ultrasonic treatment device are controlled to be 5 - 15 min, 15 - 25 min, and 25 - 35 min respectively.
[0025] Furthermore, the residence times of the primary ultrasonic treatment device, the secondary ultrasonic treatment device, and the tertiary ultrasonic treatment device are controlled to be 8 - 12 min, 18 - 22 min, and 28 - 32 min respectively.
[0026] According to a specific aspect of the present invention, the residence times of the primary ultrasonic treatment device, the secondary ultrasonic treatment device, and the tertiary ultrasonic treatment device are controlled to be 10 min, 20 min, and 30 min respectively.
[0027] According to some preferred and specific aspects of the present invention, the pore diameters of the filter elements of the primary membrane filtration device, the secondary membrane filtration device, and the tertiary membrane filtration device are controlled to be 0.04 - 0.06 μm, 0.005 - 0.015 μm, and 0.5 - 10 nm respectively.
[0028] According to some specific aspects of the present invention, when the pore diameter of the filter element of the primary membrane filtration device is 0.04 - 0.06 μm, it can be abbreviated as a microfiltration membrane filtration device; when the pore diameter of the filter element of the secondary membrane filtration device is 0.005 - 0.015 μm, it can be abbreviated as an ultrafiltration membrane filtration device; when the pore diameter of the filter element of the tertiary membrane filtration device is 0.5 - 10 nm, it can be abbreviated as a RO reverse osmosis membrane filtration device.
[0029] According to some preferred aspects of the present invention, the material of the filter element of the membrane filtration device is polytetrafluoroethylene.
[0030] According to some preferred and specific aspects of the present invention, the filtration pressure of the membrane filtration device is 0.5 - 0.8 MPa.
[0031] According to some preferred aspects of the present invention, the ultrasonic treatment device includes an ultrasonic generator and a pipeline disposed in the ultrasonic generator, and the length of the pipeline is controlled to control the residence time of hydrogen peroxide in the ultrasonic treatment device.
[0032] According to some preferred and specific aspects of the present invention, the flow rate of the hydrogen peroxide after treatment in the organic matter treatment unit is 100 L / h to 200 L / h.
[0033] In some embodiments of the present invention, the specific process of controlling this purification method is carried out at an ambient temperature less than or equal to 25°C.
[0034] Due to the application of the above technical solution, the present invention has the following advantages compared with the prior art:
[0035] Based on the problems existing in the prior art, such as high energy consumption, complex operation, and unsatisfactory purification effect in the purification of hydrogen peroxide, especially in the removal of organic substances in hydrogen peroxide, the present invention innovatively adopts a method of using ultra-low temperature and ultrasonic oscillation and then assisting membrane filtration to separate organic substances in hydrogen peroxide. Further combined with multi-stage sequential treatment, and controlling the residence time of ultrasonic oscillation in each stage and adopting a matching mode of multi-stage pore sizes of membrane filtration, it can not only greatly and effectively reduce the content of organic impurities in hydrogen peroxide to the ppb level, even as low as below 10 ppb, so that high-purity hydrogen peroxide with qualified quality can be produced on the premise of ensuring continuous and stable production. Moreover, the method of the present invention does not require additional passing through a resin tower, ensuring that the hydrogen peroxide entering the subsequent anion and cation resin towers has a high purity, thereby improving the service life of the subsequent resin towers. BRIEF DESCRIPTION OF THE DRAWINGS
[0036] Figure 1 is a process flow chart adopted for the purification method of hydrogen peroxide in the embodiment of the present invention;
[0037] In the attached drawing reference numerals, 1, pretreatment device; 2, primary ultrasonic treatment device; 3, primary membrane filtration device; 4, secondary ultrasonic treatment device; 5, secondary membrane filtration device; 6, tertiary ultrasonic treatment device; 7, tertiary membrane filtration device; 8, ultrasonic generator; 9, pipeline. DETAILED DESCRIPTION OF THE EMBODIMENTS
[0038] The process flow chart adopted for the purification method of hydrogen peroxide in the embodiment of the present invention is as Figure 1As shown, the mass percentage concentration of industrial hydrogen peroxide is adjusted to 30%-40% by the pretreatment device 1, and the feed temperature of the system is controlled at 0-5°C, which is lower than the cooling temperature in conventional operations. In the system of the present invention, practice shows that it can better precipitate the organic impurities in hydrogen peroxide, which is more conducive to the combination of ultrasonic vibration and membrane filtration to remove them; then the treated hydrogen peroxide flows through 3 organic matter treatment units arranged in series in turn. Specifically, the treated hydrogen peroxide flows through the first-stage ultrasonic treatment device 2, the first-stage membrane filtration device 3, the second-stage ultrasonic treatment device 4, the second-stage membrane filtration device 5, the third-stage ultrasonic treatment device 6, and the third-stage membrane filtration device 7 arranged in series at a certain flow rate (preferably 100L / h-200L / h). Among them, the residence times of the first-stage ultrasonic treatment device, the second-stage ultrasonic treatment device, and the third-stage ultrasonic treatment device are controlled to be 5-15min, 15-25min, and 25-35min respectively, and the residence time of hydrogen peroxide in the latter-stage ultrasonic treatment device is 1.2-3 times that in the previous-stage ultrasonic treatment device. The pore diameters of the filter elements of the first-stage membrane filtration device, the second-stage membrane filtration device, and the third-stage membrane filtration device are controlled to be 0.04-0.06μm, 0.005-0.015μm, and 0.5-10nm respectively, and the pore diameter of the filter element of the latter-stage membrane filtration device is 0.05-0.8 times that of the filter element of the previous-stage membrane filtration device. By simultaneously controlling the differences in residence time and filter element pore diameter, the removal of organic matter is more comprehensive and thorough, greatly improving the purity, and the organic matter content can be basically below 10ppb, even below 5ppb.
[0039] Furthermore, the ultrasonic treatment device includes an ultrasonic generator 8 and a pipeline 9 arranged in the ultrasonic generator 8. The length of the pipeline 9 is controlled to control the residence time of hydrogen peroxide in the ultrasonic treatment device. Preferably, the pipeline can be arranged in a serpentine shape, so that the length change of the pipeline can be controlled in a limited space without additionally expanding the space occupation ratio of the ultrasonic generator.
[0040] Furthermore, the membrane filter selected in the filtration stage of the present invention is a filter membrane with a special membrane material of polyvinylidene fluoride (PVDF). By utilizing the polarity and surface tension of this material filter membrane and the selection of the filtration accuracy of this filter membrane, the insoluble substances precipitated due to cooling in the previous stage can be completely filtered out. Through the ultrasonic-assisted filtration of three-stage filter elements, the transmittance of organic matter can be effectively reduced, achieving the purpose of nanoscale purification and greatly reducing the organic matter content in the treated hydrogen peroxide. In addition, in some alternative embodiments, the selected filter membrane can also be rinsed with ultrapure water before use, which can minimize the eluate of the filter element and thus make the filtration more effective.
[0041] The method of the present invention can not only meet the strict quality requirements of ultra-high purity hydrogen peroxide products, but also adapt to the characteristics of hydrogen peroxide, without causing potential production safety hazards, and has the advantages of short separation time, high efficiency, convenient operation, etc.
[0042] The above scheme will be further described below in conjunction with specific embodiments; it should be understood that these embodiments are used to illustrate the basic principles, main features and advantages of the present invention, and the present invention is not limited by the scope of the following embodiments; the implementation conditions adopted in the embodiments can be further adjusted according to specific requirements, and the implementation conditions not specified are usually the conditions in conventional experiments.
[0043] Unless otherwise specified in the following embodiments, all raw materials can be obtained from commercial purchases or prepared by conventional methods in the art.
[0044] In the following, unless otherwise specified, the "wt%" mentioned refers to the weight percentage concentration.
[0045] Example 1
[0046] This example provides a method for purifying hydrogen peroxide, which adopts the Figure 1 process flow shown, and includes the following steps carried out sequentially and continuously:
[0047] (1) Adjust the concentration of industrial hydrogen peroxide (50 wt% from Arkema Chemical Co., Ltd.) to about 30 wt%, and control the feeding temperature of hydrogen peroxide to be 2.5 ± 1 °C;
[0048] (2) Make the hydrogen peroxide treated in step (1) enter the first-stage ultrasonic treatment device at a flow rate of 100 L / h in sequence. The hydrogen peroxide flowing out of the pipeline enters the first-stage membrane filtration device (the filter element is a MILLI microporous filter membrane with a pore size of 0.05 μm, and the filter element material is polyvinylidene fluoride (PVDF)), and then enters the second-stage ultrasonic treatment device. The hydrogen peroxide flowing out of the pipeline enters the second-stage membrane filtration device (the filter element is a columnar ultrafiltration membrane (cut-off molecular weight 1000D) with a pore size of 0.01 μm, and the filter element material is polyvinylidene fluoride (PVDF)), and finally enters the third-stage ultrasonic treatment device. The hydrogen peroxide flowing out of the pipeline enters the third-stage membrane filtration device (the filter element is a Hydranautics reverse osmosis (RO) membrane in the United States with a pore size of 1 nm, and the filter element material is polyvinylidene fluoride (PVDF)), and hydrogen peroxide with organic substances removed is obtained;
[0049] Among them, the filtration pressure is: 0.5 MPa for the first-stage membrane filtration device, 0.5 MPa for the first-stage membrane filtration device, 0.5 MPa for the first-stage membrane filtration device; control the residence time of the first-stage ultrasonic treatment device, the residence time of the second-stage ultrasonic treatment device, and the residence time of the third-stage ultrasonic treatment device to be 10 min, 20 min, and 30 min respectively;
[0050] The operating frequency of the ultrasonic generator of the ultrasonic treatment device is 25 kHz;
[0051] The specific process of controlling this purification method is carried out at an ambient temperature of 20 ± 5 °C;
[0052] For the purified hydrogen peroxide, the detection results of the organic impurity content are shown in Table 1.
[0053] Example 2
[0054] This example provides a method for purifying hydrogen peroxide, which is basically the same as Example 1, and the only difference is that:
[0055] In step (1), the concentration of industrial hydrogen peroxide (50 wt% from Arkema Chemical Co., Ltd.) is adjusted to 35 wt%;
[0056] In step (2), the hydrogen peroxide treated in step (1) enters the first-stage ultrasonic treatment device at a flow rate of 150 L / h in sequence.
[0057] For the purified hydrogen peroxide, the detection results of the organic impurity content are shown in Table 1.
[0058] Example 3
[0059] This example provides a method for purifying hydrogen peroxide, which is basically the same as Example 1, and the only difference is that:
[0060] In step (1), the concentration of industrial hydrogen peroxide (50 wt% from Arkema Chemical Co., Ltd.) is adjusted to 40 wt%;
[0061] In step (2), the hydrogen peroxide treated in step (1) enters the first-stage ultrasonic treatment device at a flow rate of 200 L / h in sequence.
[0062] For the purified hydrogen peroxide, the detection results of the organic impurity content are shown in Table 1.
[0063] Example 4
[0064] This example provides a method for purifying hydrogen peroxide, which is basically the same as Example 1, and the only difference is that the residence times of the first-stage ultrasonic treatment device, the second-stage ultrasonic treatment device, and the third-stage ultrasonic treatment device are controlled to be 10 min, 25 min, and 35 min respectively.
[0065] Comparative Example 1
[0066] This example provides a method for purifying hydrogen peroxide, including the following steps carried out sequentially and continuously:
[0067] (1) Adjust the concentration of industrial hydrogen peroxide (50 wt% from Arkema Chemicals Co., Ltd.) to about 30 wt%, and control the feeding temperature of hydrogen peroxide at 2.5 ± 1 °C;
[0068] (2) Let the treated hydrogen peroxide pass through macroporous adsorption resins (Series A and B macroporous adsorption resins from Tianxing Resin Co., Ltd., Bengbu, Anhui) at a flow rate of 200 L / h in sequence to obtain hydrogen peroxide with organic substances removed. The test results of the organic substance impurity content in the purified hydrogen peroxide are shown in Table 1.
[0069] Comparative Example 2
[0070] This example provides a method for purifying hydrogen peroxide, which is basically the same as Example 1, and the only difference is that: the 3 - stage ultrasonic treatment device is omitted, and the treated hydrogen peroxide passes through a 3 - stage membrane filtration device in sequence. The test results of the organic substance impurity content in the purified hydrogen peroxide are shown in Table 1.
[0071] Comparative Example 3
[0072] This example provides a method for purifying hydrogen peroxide, which is basically the same as Example 1, and the only difference is that: the residence time in the three - stage ultrasonic treatment device is controlled to be the same. The test results of the organic substance impurity content in the purified hydrogen peroxide are shown in Table 1.
[0073] Table 1 Organic substance impurity content in hydrogen peroxide after removing organic substances in Examples 1 - 4 and Comparative Examples 1 - 3
[0074]
[0075] As can be seen from the above, compared with Example 1, the removal of organic substances in Comparative Examples 1 - 3 all decreased significantly. Although the effect of removing organic substances in Comparative Example 1 is relatively good, it uses conventional macroporous adsorption resins, which determines a high frequency of resin desorption and regeneration, resulting in a high cost; the effect of removing organic substances in Comparative Example 2 is the worst, indicating that ultrasonic treatment plays an important role in the method of the present invention. In Comparative Example 3, the residence time in different ultrasonic treatment devices is made the same, which changes the cooperation with different membrane filtration devices, making it difficult to maximize the removal of organic substances, resulting in a still relatively high content of organic substances in the final hydrogen peroxide. While the present invention uses a method of combining ultra - low temperature and ultrasonic oscillation and then assisting membrane filtration to separate organic substances in hydrogen peroxide, further combining multi - stage sequential treatment, and controlling the residence time of ultrasonic oscillation in each stage and using a method of matching multi - stage pore sizes of membrane filtration, achieving efficient removal of organic substances in hydrogen peroxide, and the organic substance content can be basically below 10 ppb, even below 5 ppb.
[0076] The above embodiments are only used to illustrate the technical concept and characteristics of the present invention, and the purpose is to enable those skilled in the art to understand the content of the present invention and implement it accordingly. However, the protection scope of the present invention cannot be limited thereby. Any equivalent changes or modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
[0077] The endpoints and any values disclosed in this article are not limited to the exact ranges or values. These ranges or values should be understood to include values close to these ranges or values. For numerical ranges, the endpoint values of each range, between the endpoint values of each range and individual point values, and between individual point values can be combined with each other to obtain one or more new numerical ranges, and these numerical ranges should be regarded as specifically disclosed in this article.
Claims
1. A continuous purification method for hydrogen peroxide, characterized in that, the purification method comprises: adjusting the mass percentage concentration of industrial-grade hydrogen peroxide to 30%-40% through a pretreatment device, controlling the feed temperature of the system to be 0-5°C, and then allowing the treated hydrogen peroxide to flow through n organic matter treatment units arranged in series in sequence, where n is greater than or equal to 3; each of the organic matter treatment units independently comprises an ultrasonic treatment device and a membrane filtration device connected in sequence. In each of the organic matter treatment units, hydrogen peroxide is successively subjected to oscillation treatment by the ultrasonic treatment device and filtration treatment by the membrane filtration device, and the organic matter content in the purified hydrogen peroxide is below 10 ppb; wherein, the residence time of hydrogen peroxide in the ultrasonic treatment device included in the subsequent-stage organic matter treatment unit is controlled to be greater than the residence time of hydrogen peroxide in the ultrasonic treatment device included in the previous-stage organic matter treatment unit, and the pore diameter of the filter element of the membrane filtration device included in the subsequent-stage organic matter treatment unit is controlled to be smaller than the pore diameter of the filter element of the membrane filtration device included in the previous-stage organic matter treatment unit.
2. The continuous purification method for hydrogen peroxide according to claim 1, characterized in that, the residence time of hydrogen peroxide in the ultrasonic treatment device included in the subsequent-stage organic matter treatment unit is controlled to be 1.2-3 times, further 1.2-1.5 times, the residence time of hydrogen peroxide in the ultrasonic treatment device included in the previous-stage organic matter treatment unit; the pore diameter of the filter element of the membrane filtration device included in the subsequent-stage organic matter treatment unit is controlled to be 0.05-0.8 times, further 0.05-0.15 times, the pore diameter of the filter element of the membrane filtration device included in the previous-stage organic matter treatment unit.
3. The continuous purification method for hydrogen peroxide according to claim 1, characterized in that, the residence time of hydrogen peroxide in the ultrasonic treatment device included in the subsequent-stage organic matter treatment unit is controlled to be 1.5-2.0 times, or 2.0-3.0 times, that of the ultrasonic treatment device included in the previous-stage organic matter treatment unit; and / or, the pore diameter of the filter element of the membrane filtration device included in the subsequent-stage organic matter treatment unit is controlled to be 0.2-0.35 times, or 0.35-0.55 times, or 0.55-0.8 times, that of the filter element of the membrane filtration device included in the previous-stage organic matter treatment unit.
4. The continuous purification method for hydrogen peroxide according to any one of claims 1-3, characterized in that, the ultrasonic treatment device comprises an ultrasonic generator and a pipeline arranged in the ultrasonic generator, and the length of the pipeline is controlled to control the residence time of hydrogen peroxide in the ultrasonic treatment device.
5. The continuous purification method for hydrogen peroxide according to claim 4, characterized in that, the pipeline is distributed in a serpentine shape; and / or, the working frequency of the ultrasonic treatment device is 25-40 kHz.
6. The continuous purification method for hydrogen peroxide according to claim 1, characterized in that, n is 3, 4 or 5; and / or, the flow rate of the treated hydrogen peroxide in the organic matter treatment unit is 100-200 L / h.
7. The continuous purification method of hydrogen peroxide according to claim 1, characterized in that when n is 3, the treated hydrogen peroxide is sequentially passed through a first-stage ultrasonic treatment device, a first-stage membrane filtration device, a second-stage ultrasonic treatment device, a second-stage membrane filtration device, a third-stage ultrasonic treatment device, and a third-stage membrane filtration device which are arranged in series.
8. The continuous purification method of hydrogen peroxide according to claim 7, characterized in that the residence times of the first-stage ultrasonic treatment device, the second-stage ultrasonic treatment device, and the third-stage ultrasonic treatment device are controlled to be 5-15 min, 15-25 min, and 25-35 min respectively. Further, the residence times of the first-stage ultrasonic treatment device, the second-stage ultrasonic treatment device, and the third-stage ultrasonic treatment device are controlled to be 8-12 min, 18-22 min, and 28-32 min respectively; the first-stage membrane filtration device is a microfiltration membrane filtration device with a filter element pore size of 0.04-0.06 μm, the second-stage membrane filtration device is an ultrafiltration membrane filtration device with a filter element pore size of 0.005-0.015 μm, and the third-stage membrane filtration device is a RO reverse osmosis membrane filtration device with a filter element pore size of 0.5-10 nm.
9. The continuous purification method of hydrogen peroxide according to claim 1, characterized in that the organic matter content in the purified hydrogen peroxide is below 5 ppb; and / or, the specific process of controlling this continuous purification method is carried out at an environmental temperature less than or equal to 25 °C; and / or, the filtration pressure of the membrane filtration device is 0.5-0.8 MPa; and / or, the material of the filter element of the membrane filtration device is polytetrafluoroethylene.
10. A hydrogen peroxide prepared by the continuous purification method of hydrogen peroxide according to any one of claims 1-9, and this hydrogen peroxide can be used in the pharmaceutical, electronic, food, textile or paper-making industry.
Citation Information
Patent Citations
Purification method for removing TOC in hydrogen peroxide at low temperature
CN112723316A