Purification method of hydrogen peroxide

Through the combination of multi-stage distillation, photocatalytic reaction and membrane separation, combined with intelligent control, the problem of insufficient purity and stability of hydrogen peroxide is solved, and high-purity and high-stability hydrogen peroxide production is achieved, reducing energy consumption and improving production efficiency.

CN119591055APending Publication Date: 2025-03-11JIANGSU LEE & MAN CHEM
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Patent Information

Application Number
CN202411959785.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-30
Publication Date
2025-03-11

AI Technical Summary

Technical Problem

The existing hydrogen peroxide production technology is difficult to achieve extremely high purity and stability, especially in terms of stability.

Method used

Multi-stage distillation combined with photocatalytic reaction and membrane separation is used to remove macromolecular impurities through primary distillation, and secondary distillation is further purified. The photocatalytic reaction increases the stability of hydrogen peroxide, and membrane separation removes residual small molecule impurities, and realizes automatic management throughout the process through intelligent control.

Benefits of technology

It significantly improves the purity and chemical stability of hydrogen peroxide, extends the storage period, reduces energy consumption, improves production efficiency and product quality, and achieves a win-win situation for both economic and environmental protection.

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Abstract

The invention discloses a hydrogen peroxide purification method which comprises the following steps: S100, primary rectification: preliminarily removing macromolecular impurities; s200, carrying out secondary rectification, and further purifying; s300, photocatalytic reaction: under illumination of a specific wavelength, TiO2 is used as a photocatalyst to promote free radical recombination, and the stability of hydrogen peroxide is improved; s400, performing membrane separation to remove residual small molecular impurities; and S500, intelligent control is carried out, operation conditions are automatically adjusted according to material properties, and whole-course automatic management is achieved. The purity of the hydrogen peroxide is obviously improved; the chemical stability of the hydrogen peroxide is greatly enhanced, and the storage life of the hydrogen peroxide can be greatly prolonged even under extreme conditions; and due to the application of an intelligent management system and a waste heat recovery technology, the energy consumption is obviously reduced, and the economic and environment-friendly win-win situation is realized.
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Description

Technical Field

[0001] The invention relates to the technical field of hydrogen peroxide processing, in particular to a method for purifying hydrogen peroxide. Background Art

[0002] Hydrogen peroxide is widely used in fine chemicals, pharmaceuticals, environmental protection and other industries. At present, the production technology of hydrogen peroxide mainly relies on the traditional single distillation process, which separates the impurities in hydrogen peroxide from the hydrogen peroxide by heating. Due to the different boiling points of hydrogen peroxide and other impurities, hydrogen peroxide can be evaporated by controlling the temperature, and then condensed to obtain hydrogen peroxide with higher purity. Although the existing technology can remove impurities to a certain extent, it is often difficult to meet the requirements of extremely high purity, especially in terms of stability. With the growing demand for the purity and stability of hydrogen peroxide in the industrial field, traditional purification technologies and methods have gradually revealed their limitations. Summary of the invention

[0003] The purpose of the invention is to solve the technical problems of insufficient concentration and stability of existing hydrogen peroxide.

[0004] To achieve the purpose of the present invention, the present invention adopts the following technical solutions:

[0005] A method for purifying hydrogen peroxide comprises the following steps:

[0006] S100: primary distillation, preliminary removal of macromolecular impurities;

[0007] S200: secondary distillation for further purification;

[0008] S300: Photocatalytic reaction, under specific wavelength light, using TiO2 as a photocatalyst to promote free radical recombination and increase the stability of hydrogen peroxide;

[0009] S400: membrane separation to remove residual small molecule impurities;

[0010] S500: Intelligent control, automatically adjusts operating conditions according to material properties, and realizes full-process automated management.

[0011] In some embodiments, the heating method in step S100 is segmented heating, so as to achieve precise control and energy saving; the distillation tower is divided into a primary distillation zone, a main distillation zone and a side line reflux zone, and the heating intensity and temperature range are set for each zone to optimize the separation effect.

[0012] In some embodiments, the photocatalytic reaction in step S300 is optimized to be a TiO2 photocatalytic reaction under irradiation of a UV-A light source of a specific wavelength to accelerate the free radical recombination process.

[0013] In some embodiments, the light source wavelength ranges from 360 to 420 nm, the TiO2 nanoparticle size is 5 to 50 nm, and the surface area is greater than 150 m^2 / g to improve photocatalytic activity and conversion rate.

[0014] In some embodiments, the membrane separation in step S400 uses a hydrophilic microporous filtration membrane, which selectively transmits and further removes trace organic small molecule impurities; the membrane pore size range is 0.1-1μm, the material is polyethersulfone, and the surface is modified to increase hydrophobicity to prevent clogging and increase filtration rate.

[0015] In some embodiments, the intelligent control in step S50 uses integrated multiple sensor monitoring and artificial intelligence algorithm prediction models to adjust the system operation status in real time to ensure high-quality continuous production. Sensor types include temperature, pressure, flow meter, etc. The artificial intelligence algorithm is based on a deep learning neural network, and the training data comes from actual production conditions to achieve dynamic optimization.

[0016] In some embodiments, during the distillation process, a high-efficiency heat exchanger is used to recover heat, and the preheating temperature can be increased to 60-90°C.

[0017] In some embodiments, in step S100, the hydrogen peroxide is preheated before distillation to improve the efficiency of the subsequent evaporation process.

[0018] In some embodiments, in step S200, in the distillation tower, the pressure is controlled at 8-9.3 kPa, pure water is used as reflux liquid for distillation, and the bottom temperature is controlled at about 54° C., so that high-concentration hydrogen peroxide can be effectively separated.

[0019] In some embodiments, in step S200, three-stage fillers are used in the distillation tower, and after two times of redistribution, the distillation effect is better.

[0020] The method for purifying hydrogen peroxide provided by the present invention has the following advantages:

[0021] 1) The purity of hydrogen peroxide has been significantly improved; 2) The chemical stability of hydrogen peroxide has been greatly enhanced, and its storage period can be greatly extended even under extreme conditions; 3) The application of intelligent management system and waste heat recovery technology has significantly reduced energy consumption, achieving a win-win situation for economy and environmental protection; 4) The automation upgrade of production process has improved labor productivity, reduced the risk of manual intervention, and ensured the consistency and reliability of product quality; 5) The comprehensive optimization of the system has created higher economic benefits for the enterprise, and also contributed to the green development goals of the society. DETAILED DESCRIPTION

[0022] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments.

[0023] <Example 1>

[0024] The present embodiment provides a method for purifying hydrogen peroxide, comprising the following steps: step 1: primary distillation to preliminarily remove macromolecular impurities; step 2: secondary distillation to further purify; step 3: photocatalytic reaction to utilize TiO 2 As a photocatalyst, it promotes the recombination of free radicals and increases the stability of hydrogen peroxide. Step 4: membrane separation, as a supplementary means, removes residual small molecule impurities. Step 5: intelligent control, automatically adjusts the operating conditions according to the properties of the material, and realizes full automation management. The above technical solution successfully solves the technical bottleneck of high purity and stability of hydrogen peroxide by combining distillation and photocatalysis, and improves production efficiency through intelligent control.

[0025] Furthermore, the heating method in step 1 is preferably segmented heating, that is, the position of the heating source is set according to different components to match their volatility characteristics, so as to achieve precise control and energy saving. Preferably, the distillation tower is divided into a primary distillation zone, a main distillation zone and a side reflux zone, and the heating intensity and temperature range are set for each zone to optimize the separation effect. The photocatalytic reaction in step 3 is optimized to TiO2 under the irradiation of a UV-A light source of a specific wavelength. 2 Photocatalytic reaction to accelerate the free radical recombination process. Preferably, the wavelength range of the light source is 360-420nm, TiO 2 The nanoparticle size is 5-50nm, and the surface area is greater than 150m^2 / g to improve photocatalytic activity and conversion rate. The membrane separation in step 4 is optimized to use a hydrophilic microporous filter membrane, which selectively penetrates to further remove trace organic small molecule impurities. Preferably, the membrane pore size range is 0.1-1μm, the material is polyethersulfone (PES), and the surface modification improves hydrophobicity to prevent clogging and increase the filtration rate. The intelligent control optimization in step 5 is to integrate multiple sensor monitoring and artificial intelligence algorithm prediction models, adjust the system operation status in real time, and ensure high-quality continuous production. Preferably, sensor types include temperature, pressure, flow meter, etc., the artificial intelligence algorithm is based on a deep learning neural network, and the training data comes from actual production conditions to achieve dynamic optimization.

[0026] Furthermore, in step 1, the hydrogen peroxide is preheated before distillation to improve the efficiency of the subsequent evaporation process. In step 2, in the distillation tower, the pressure is controlled at 8-9.3 kPa, pure water is used as the reflux liquid for distillation, and the bottom temperature is controlled at about 54°C, so that high-concentration hydrogen peroxide can be effectively separated. In step 2, three-stage packing is used in the distillation tower, and after two times of recollection and redistribution, the distillation effect is better.

[0027] <Example 2>

[0028] In this embodiment, the same text descriptions are omitted for the parts that are the same as those in the first embodiment.

[0029] Compared with Example 1, the method for purifying hydrogen peroxide provided in this embodiment has the following difference in design: in order to further improve the energy efficiency of the system, a waste heat recovery device can be added on the original basis, and the waste heat generated by the distillation process can be used to preheat raw materials or supply other equipment in the workshop to achieve energy recycling. Preferably, a high-efficiency heat exchanger is used to recover heat, and the preheating temperature can be increased to 60-90°C, saving about 20% of energy consumption. In order to meet the customized needs of specific industries, the system can flexibly configure different types of photocatalysts and reactor structures to adapt to the preparation of different types of hydrogen peroxide. Preferably, in addition to TiO 2 , photocatalysts such as ZnO and CdS can also be considered to expand the application scenarios.

[0030] Furthermore, the heating method is improved, and electric heating wires are evenly distributed inside the distillation tower to adjust the heating power and circulating liquid flow rate to optimize the secondary distillation effect. The photocatalytic reactor structure uses an LED array as the light source, accurately controls the wavelength and radiation intensity, and cooperates with modified TiO 2 The coating achieves efficient recombination of free radicals. After multiple experiments, the purity of hydrogen peroxide reaches 99.9%, and it still maintains a high level after being stored for half a year.

[0031] Furthermore, the membrane separation technical parameters were adjusted, and the optimal working pressure and cleaning cycle were selected to ensure continuous and efficient microporous permeability. The purity and stability of the final product were improved, and the service life of the membrane was extended to more than one year. Low-temperature plasma technology was introduced as a pretreatment step before photocatalysis to oxidize and decompose difficult-to-degrade organic pollutants before entering the photocatalytic reactor.

[0032] The embodiment of the present invention adopts an integrated system design of multi-stage distillation and photocatalysis in series to ensure high purity and high stability. The refined control of segmented heating technology is adopted to maximize energy efficiency. The selective purification of membrane separation technology is adopted to eliminate the interference of trace impurities. The dynamic adjustment of the intelligent control system is adopted to ensure the consistency of the production process. The integration of waste heat recovery and energy-saving and environmental protection technology is adopted to embody the concept of sustainable development.

[0033] In the above-mentioned Embodiments 1 and 2, during the working process, as the working environment is different, some technical implementation methods of Embodiments 1 and 2 can be combined or replaced.

[0034] The technical principle of the present invention is described above in combination with specific embodiments, but it should be noted that the above descriptions are only for explaining the principle of the present invention and cannot be interpreted as a specific limitation on the protection scope of the present invention in any way. Based on the explanation here, technicians in this field can think of other specific embodiments or equivalent replacements of the present invention without paying creative work, which will fall within the protection scope of the present invention.

Claims

1. A method for purifying hydrogen peroxide, characterized in that: The following steps are involved: S100: primary distillation, preliminary removal of macromolecular impurities; S200: secondary distillation for further purification; S300: Photocatalytic reaction, under specific wavelength light, using TiO2 as a photocatalyst to promote free radical recombination and increase the stability of hydrogen peroxide; S400: membrane separation to remove residual small molecule impurities; S500: Intelligent control, automatically adjusts operating conditions according to material properties, and realizes full-process automated management.

2. The method for purifying hydrogen peroxide according to claim 1, characterized in that: The heating method in step S100 is segmented heating, so as to achieve precise control and energy saving; the distillation tower is divided into a primary distillation zone, a main distillation zone and a side line reflux zone, and the heating intensity and temperature range are set for each zone to optimize the separation effect.

3. The method for purifying hydrogen peroxide according to claim 2, characterized in that: The photocatalytic reaction in step S300 is optimized as a TiO2 photocatalytic reaction under the irradiation of a UV-A light source of a specific wavelength to accelerate the free radical recombination process.

4. The method for purifying hydrogen peroxide according to claim 3, characterized in that: The light source wavelength ranges from 360-420nm, the TiO2 nanoparticle size is 5-50nm, and the surface area is greater than 150m^2 / g to improve photocatalytic activity and conversion rate.

5. The method for purifying hydrogen peroxide according to claim 4, characterized in that: The membrane separation in step S400 uses a hydrophilic microporous filtration membrane, which selectively permeates and further removes trace organic small molecule impurities; the membrane pore size range is 0.1-1μm, the material is polyethersulfone, and the surface modification improves hydrophobicity to prevent clogging and increase filtration rate.

6. The method for purifying hydrogen peroxide according to claim 5, characterized in that: The intelligent control in step S50 uses integrated multiple sensor monitoring and artificial intelligence algorithm prediction models to adjust the system operation status in real time to ensure high-quality continuous production. Sensor types include temperature, pressure, flow meters, etc. The artificial intelligence algorithm is based on a deep learning neural network, and the training data comes from actual production conditions to achieve dynamic optimization.

7. The method for purifying hydrogen peroxide according to claim 1, characterized in that: During the distillation process, high-efficiency heat exchangers are used to recover heat, and the preheating temperature can be increased to 60-90°C.

8. The method for purifying hydrogen peroxide according to claim 7, characterized in that: In step S100, the hydrogen peroxide solution is preheated before distillation to improve the efficiency of the subsequent evaporation process.

9. The method for purifying hydrogen peroxide according to claim 8, characterized in that: In step S200, in the distillation tower, the pressure is controlled at 8-9.3 kPa, pure water is used as reflux liquid for distillation, and the tower bottom temperature is controlled at about 54°C, so that high-concentration hydrogen peroxide can be effectively separated.

10. The method for purifying hydrogen peroxide according to claim 9, characterized in that: In step S200, three-stage fillers are used in the distillation tower, and after two times of redistribution and collection, the distillation effect is better.