CN111003757A - Magnetic graphene aerogel particle electrode and preparation method thereof - Google Patents

Magnetic graphene aerogel particle electrode and preparation method thereof Download PDF

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Publication number
CN111003757A
CN111003757A CN201911112532.3A CN201911112532A CN111003757A CN 111003757 A CN111003757 A CN 111003757A CN 201911112532 A CN201911112532 A CN 201911112532A CN 111003757 A CN111003757 A CN 111003757A
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particle electrode
aerogel particle
graphene aerogel
deionized water
magnetic graphene
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滕厚开
谢陈鑫
任春燕
赵慧
钱光磊
雷太平
李旗
周立山
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CNOOC Energy Technology and Services Ltd
CNOOC Tianjin Chemical Research and Design Institute Co Ltd
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CNOOC Energy Technology and Services Ltd
CNOOC Tianjin Chemical Research and Design Institute Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/46Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104Devices therefor; Their operating or servicing
    • C02F1/46109Electrodes
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/12Halogens or halogen-containing compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2201/00Apparatus for treatment of water, waste water or sewage
    • C02F2201/46Apparatus for electrochemical processes
    • C02F2201/461Electrolysis apparatus
    • C02F2201/46105Details relating to the electrolytic devices
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00Controlling or monitoring parameters in water treatment
    • C02F2209/20Total organic carbon [TOC]

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Catalysts (AREA)

Abstract

The invention discloses a magnetic graphene aerogel particle electrode and a preparation method thereof. The particle electrode is prepared from graphene oxide, ferroferric oxide and manganese dioxide serving as raw materials by a hydrothermal synthesis method to prepare three-dimensional porous graphene hydrogel loaded with catalytic active components, and the three-dimensional porous graphene hydrogel is subjected to freeze drying and roasting reduction in an inert atmosphere to obtain the magnetic graphene aerogel particle electrode. The magnetic graphene aerogel particle electrode has good catalytic activity and good removal effect on chloride ions and TOC in the chloropropylene glycol wastewater; and the particle electrode can be recovered by using an external magnetic field after being used, so that the particle electrode is convenient to reuse and has strong stability.

Description

Magnetic graphene aerogel particle electrode and preparation method thereof
Technical Field
The invention relates to the technical field of electrocatalysis, in particular to a magnetic graphene aerogel particle electrode for removing organic pollutants in wastewater and a preparation method thereof.
Background
In recent years, electrocatalytic technology has been widely used in the field of wastewater treatment. The technique utilizes the oxidation reaction of the anode and OH and ClO generated in the experimental process-And Cl-The active oxidation substances directly and indirectly degrade pollutants in the wastewater. The electrocatalytic oxidation technology has the advantages of simple operation, mild reaction conditions, no secondary pollution and the like, shows high-efficiency degradation capability in the aspect of treating refractory wastewater, and gradually becomes a research hotspot in the field of sewage treatment. The traditional two-dimensional flat plate electrode has the defects of small surface area ratio, high power consumption, low current efficiency, low mass transfer rate and the like, so that the three-dimensional electrode is produced. The three-dimensional electrode requires that a granular or scrap-like particle electrode material is filled between electrodes to become a new one, and the surface thereof is charged to cause a chemical reaction on the surface thereof. The particle electrodes can increase the surface area ratio of the three-dimensional electrodes, and because the distance between the particle electrodes is small, the mass transfer process of substances is greatly improved, the reaction rate is accelerated, and the electrocatalysis efficiency is further improved. Therefore, the existing three-dimensional electrode can not meet the requirements, and the particle electrode with higher catalytic activity is obtained by carrying out structural modification or research on the three-dimensional electrode reactor.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a magnetic graphene aerogel particle electrode which has the characteristics of high catalytic activity, strong stability, simple preparation method and the like. The existence of the graphene can accelerate the transfer speed of electrons, the existence of the ferroferric oxide and the manganese dioxide can catalyze hydrogen peroxide generated in situ in a cathode region to generate hydroxyl radicals, and the ferroferric oxide can endow the particle electrode with magnetism and is convenient to recycle after use.
The technical scheme adopted by the invention is as follows: preparation method of magnetic graphene aerogel particle electrode, and packageThe method comprises the following steps: mixing 8-15 mg/mL-1Adding the graphene oxide slurry, the ferroferric oxide nanoparticles and the manganese dioxide nanoparticles into a beaker according to the mass ratio of 1: 1-5: 1-5, ultrasonically dispersing and uniformly mixing, then transferring into a hydrothermal synthesis kettle for hydrothermal synthesis at the temperature of 120-; and then carrying out thermal reduction treatment at the temperature of 400-800 ℃ in a hydrogen atmosphere to obtain the magnetic graphene aerogel particle electrode.
The preparation method of the magnetic graphene aerogel particle electrode preferably comprises the following steps:
(1) preparing ferroferric oxide nano particles: preparing ferroferric oxide nano particles by a one-step coprecipitation method. Dissolving ferric trichloride and ferrous chloride in deionized water, ultrasonically dispersing for 5min, adding into a four-neck flask equipped with a condenser tube, removing oxygen with nitrogen for 30min, heating to 90-100 deg.C, and pumping with a peristaltic pump at a flow rate of 1 mL/min-1Dropwise adding an ammonia water solution at the speed of (1) till the pH value is 7-12, and reacting for 1-5 h. And (3) performing solid-liquid separation by using an external magnetic field, washing the precipitate for more than 2 times by using deionized water and ethanol, and freeze-drying to obtain the ferroferric oxide nanoparticles.
(2) Preparing manganese dioxide nano particles: dissolving potassium permanganate, a hydrochloric acid solution and a reducing agent in deionized water, transferring the solution to a hydrothermal synthesis kettle, keeping the solution at the temperature of 100-150 ℃ for 8-15 h, naturally cooling to room temperature, washing the precipitate with the deionized water and ethanol for more than 2 times, and freeze-drying to obtain the manganese dioxide nanoparticles.
(3) Graphene oxide is prepared according to an improved Hummers method, and then prepared to have a concentration of 8-15 mg/mL-1The slurry of (1). Adding the graphene oxide slurry, ferroferric oxide and manganese dioxide into a beaker according to the mass ratio of 1: 1-5: 1-5, performing ultrasonic dispersion for 15min, then transferring the mixture into a hydrothermal synthesis kettle, heating to 120 ℃ and 150 ℃, and preserving heat for 1-5 h. Separating with magnet, washing precipitate with deionized water and ethanol for more than 2 times, and freeze drying to obtain magnetic stoneAn graphene aerogel particle electrode precursor.
(4) And heating the obtained magnetic graphene aerogel particle electrode precursor to 400-800 ℃ in a hydrogen atmosphere for thermal reduction treatment for 30-60 min to obtain the magnetic graphene aerogel particle electrode.
In the above preparation method of the magnetic graphene aerogel particle electrode, the molar ratio of the ferrous chloride to the ferric chloride in the step (1) of the method is preferably 1: 1-3.
In the above method for preparing the magnetic graphene aerogel particle electrode, the reducing agent in step (2) of the method is preferably one or a mixture of hydrazine hydrate, urea and glucose.
In the above method for preparing a magnetic graphene aerogel particle electrode, the concentration of hydrochloric acid in the step (2) of the method is preferably 2mol · L-1
In the above method for preparing the magnetic graphene aerogel particle electrode, the mass ratio of the reducing agent to potassium permanganate in step (2) of the method is preferably 1: 1-6.
The preparation method of the magnetic graphene aerogel particle electrode provided by the invention has the advantages of simplicity in operation, good stability and the like, and the magnetic graphene aerogel particle electrode prepared according to the preparation method has a good removal effect on chloride ions and TOC in chloropropylene glycol wastewater, and is low in energy consumption.
Detailed Description
The technical solutions of the present invention will be described in detail with reference to specific examples, which should not be construed as limiting the scope of the present invention.
Examples 1 to 4 are the preparation of a magnetic graphene aerogel particle electrode, example 5 is the performance evaluation of the three-dimensional particle electrodes prepared in examples 1 to 4, and example 6 is the stability test of the three-dimensional particle electrodes prepared.
Example 1
(1) Preparing ferroferric oxide nano particles: preparing ferroferric oxide nano particles by a one-step coprecipitation method. Dissolving 2.71g ferric trichloride and 2.78g ferrous chloride in deionized water, ultrasonically dispersing for 5min, and addingPutting into a four-neck flask with condenser tube, removing oxygen with nitrogen for 30min, heating to 90 deg.C, and pumping with peristaltic pump at a flow rate of 1 mL/min-1Then ammonia solution is added dropwise until the pH value is 8, and the reaction is carried out for 1 h. Performing solid-liquid separation by using an external magnetic field, washing the precipitate for 3 times by using deionized water and ethanol, and freeze-drying to obtain ferroferric oxide nanoparticles A1
(2) Preparing manganese dioxide nano particles: dissolving 0.11g of potassium permanganate, 2mL of hydrochloric acid solution and 0.05g of urea in deionized water, transferring the solution to a hydrothermal synthesis kettle, keeping the temperature at 110 ℃ for 8 hours, naturally cooling to room temperature, washing the precipitate with deionized water and ethanol for 3 times, and freeze-drying to obtain manganese dioxide nanoparticles B1
(3) Graphene oxide was prepared according to the modified Hummers method, and then formulated to a concentration of 8 mg-mL-1Slurry C of1(ii) a Mixing 30mL of C1、0.25g A1And 0.24g B1Adding into a beaker, carrying out ultrasonic dispersion for 15min, then transferring into a hydrothermal synthesis kettle, heating to 120 ℃, and keeping the temperature for 1 h. Separating with a magnet, washing the precipitate with deionized water and ethanol for 3 times, and freeze-drying to obtain a magnetic graphene aerogel particle electrode precursor D1
(4) D obtained1And (3) heating to 400 ℃ in a hydrogen atmosphere, and carrying out thermal reduction treatment for 30min to obtain the magnetic graphene aerogel particle electrode I.
Example 2
(1) Preparing ferroferric oxide nano particles: preparing ferroferric oxide nano particles by a one-step coprecipitation method. Dissolving 2.71g ferric trichloride and 2.78g ferrous chloride in deionized water, ultrasonically dispersing for 5min, adding into a four-neck flask equipped with a condenser tube, removing oxygen with nitrogen for 30min, heating to 90 deg.C, and pumping with a peristaltic pump at 1 mL/min-1Then ammonia solution is added dropwise until the pH value is 9, and the reaction is carried out for 2 h. Performing solid-liquid separation by using an external magnetic field, washing the precipitate for 3 times by using deionized water and ethanol, and freeze-drying to obtain ferroferric oxide nanoparticles A2
(2) Preparing manganese dioxide nano particles: 0.15g of potassium permanganate and 3mL of hydrochloric acidDissolving the solution and 0.05g of urea in deionized water, transferring the solution to a hydrothermal synthesis kettle, keeping the temperature at 120 ℃ for 10 hours, naturally cooling to room temperature, washing precipitates with the deionized water and ethanol for 3 times, and freeze-drying to obtain manganese dioxide nanoparticles B2
(3) Graphene oxide was prepared according to the modified Hummers method, and then formulated to a concentration of 8 mg-mL-1Slurry C of2(ii) a Mixing 30mL of C2、0.48g A2And 0.47g B2Adding into a beaker, carrying out ultrasonic dispersion for 15min, then transferring into a hydrothermal synthesis kettle, heating to 120 ℃, and keeping the temperature for 2 h. Separating with a magnet, washing the precipitate with deionized water and ethanol for 3 times, and freeze-drying to obtain a magnetic graphene aerogel particle electrode precursor D2
(4) D obtained2And (3) heating to 400 ℃ in a hydrogen atmosphere, and carrying out thermal reduction treatment for 45min to obtain a magnetic graphene aerogel particle electrode II.
Example 3
(1) Preparing ferroferric oxide nano particles: preparing ferroferric oxide nano particles by a one-step coprecipitation method. Dissolving 4.03g of ferric trichloride and 2.78g of ferrous chloride in deionized water, ultrasonically dispersing for 5min, adding into a four-neck flask with a condenser tube, deoxidizing with nitrogen for 30min, heating to 90 ℃, and using a peristaltic pump to perform 1 mL/min-1Then ammonia solution is added dropwise until the pH value is 10, and the reaction is carried out for 2 h. Performing solid-liquid separation by using an external magnetic field, washing the precipitate for 3 times by using deionized water and ethanol, and freeze-drying to obtain ferroferric oxide nanoparticles A3
(2) Preparing manganese dioxide nano particles: dissolving 0.25g of potassium permanganate, 4mL of hydrochloric acid solution and 0.05g of glucose in deionized water, transferring the solution to a hydrothermal synthesis kettle, keeping the temperature at 120 ℃ for 10 hours, naturally cooling to room temperature, washing the precipitate with deionized water and ethanol for 3 times, and freeze-drying to obtain manganese dioxide nanoparticles B3
(3) Graphene oxide was prepared according to the modified Hummers method, and then formulated to a concentration of 10 mg-mL-1Slurry C of3(ii) a Mixing 30ml of C3、0.91g A3And 0.92g B3Adding into a beaker, carrying out ultrasonic dispersion for 15min, then transferring into a hydrothermal synthesis kettle, heating to 150 ℃, and keeping the temperature for 3 h. Separating with a magnet, washing the precipitate with deionized water and ethanol for 3 times, and freeze-drying to obtain a magnetic graphene aerogel particle electrode precursor D3
(4) D obtained3And (3) heating to 600 ℃ in a hydrogen atmosphere, and carrying out thermal reduction treatment for 45min to obtain a magnetic graphene aerogel particle electrode III.
Example 4
(1) Preparing ferroferric oxide nano particles: preparing ferroferric oxide nano particles by a one-step coprecipitation method. Dissolving 8.11g ferric trichloride and 2.78g ferrous chloride in deionized water, ultrasonically dispersing for 5min, adding into a four-neck flask with a condenser tube, removing oxygen with nitrogen for 30min, heating to 90 deg.C, and pumping with a peristaltic pump at 1 mL/min-1Then, an aqueous ammonia solution was added dropwise at a rate of 12 pH, and the reaction was carried out for 3 hours. Performing solid-liquid separation by using an external magnetic field, washing the precipitate for 3 times by using deionized water and ethanol, and freeze-drying to obtain ferroferric oxide nanoparticles A4
(2) Preparing manganese dioxide nano particles: dissolving 0.31g of potassium permanganate, 5mL of hydrochloric acid solution and 0.05g of hydrazine hydrate in deionized water, transferring the solution to a hydrothermal synthesis kettle, keeping the solution at the temperature of 150 ℃ for 15h, naturally cooling the solution to room temperature, washing the precipitate with deionized water and ethanol for 3 times, and freeze-drying the washed precipitate to obtain manganese dioxide nanoparticles B4
(3) Graphene oxide was prepared according to the modified Hummers method, and then formulated to a concentration of 12 mg/mL-1Slurry C of4(ii) a Mixing 30mL of C4、1.78g A4And 0.72g B4Adding into a beaker, carrying out ultrasonic dispersion for 15min, then transferring into a hydrothermal synthesis kettle, heating to 150 ℃, and keeping the temperature for 3 h. Separating with a magnet, washing the precipitate with deionized water and ethanol for 3 times, and freeze-drying to obtain a magnetic graphene aerogel particle electrode precursor D4
(4) D obtained4Under hydrogen atmosphereAnd heating to 750 ℃ for thermal reduction treatment for 60min to obtain the magnetic graphene aerogel particle electrode IV.
Example 5
At 300 mg.L-1The chloropropylene glycol wastewater is taken as a treatment object, a DSA electrode is taken as a working electrode, a three-dimensional electro-catalysis system is constructed with the particle electrode prepared in the embodiment 1-4 of the invention, and an evaluation test is carried out in an organic glass electrolytic cell. Wherein the volume of the wastewater is 1000mL, the current value is 3A, the voltage value is 3.3V, and the TOC of the inlet water is 108 mg.L-1And the pH value is 7.60, after the electrocatalytic degradation is carried out for 30min, the content of free chlorine in the wastewater is determined by a colorimetric method, and the TOC value of the wastewater is determined by a total organic carbon analyzer. The results are shown in Table 1.
TABLE 1 evaluation results of the Performance of three-dimensional particle electrodes
Examples 1 2 3 4
Chloride ion removal Rate (%) 92.3 93.2 95.6 96.1
TOC removal (%) 80.2 82.6 84.8 86.3
A two-dimensional electrode system is constructed by taking a DSA electrode as a working electrode, an electrocatalytic degradation experiment is carried out on the chloropropylene glycol wastewater under the same condition, and the TOC removal rate of the wastewater is only 5.2% and the chloride ion removal rate is only 11.8% after 30 min. Therefore, the magnetic graphene aerogel particle electrode prepared by the invention has high catalytic efficiency.
Example 6
Stability test of magnetic graphene aerogel particle electrodes for wastewater treatment:
a three-dimensional electro-catalysis system is constructed by using a DSA electrode as a working electrode and a particle electrode prepared in the embodiment 4 of the invention, 1000ml of chloropropylene glycol wastewater is subjected to electro-catalysis treatment, magnetic separation is carried out by using an external magnetic field after treatment for 30min under the condition that the current value is 3A, and the obtained precipitate is washed, freeze-dried and subjected to 5 times of electro-catalysis tests under the same condition. The measured chloride ion removal rate of the chloropropylene glycol is as follows in sequence: 96.1%, 94.3%, 92.1%, 91.8% and 88.3%, and the TOC removal rate is 86.3%, 84.9%, 81.2% and 79.6% in sequence. Therefore, the magnetic graphene aerogel particle electrode prepared by the invention is high in stability and can be repeatedly used.

Claims (7)

1. The preparation method of the magnetic graphene aerogel particle electrode is characterized by comprising the following steps:
mixing 8-15 mg/mL-1Adding the graphene oxide slurry, the ferroferric oxide nanoparticles and the manganese dioxide nanoparticles into a beaker according to the mass ratio of 1: 1-5: 1-5, ultrasonically dispersing and uniformly mixing, then transferring into a hydrothermal synthesis kettle for hydrothermal synthesis at the temperature of 120-; and then carrying out thermal reduction treatment at the temperature of 400-800 ℃ in a hydrogen atmosphere to obtain the magnetic graphene aerogel particle electrode.
2. The method of claim 1, comprising the steps of:
(1) preparing ferroferric oxide nano particles: the iron tetroxide nano particles are prepared by a one-step coprecipitation method. Dissolving ferric trichloride and ferrous chloride in deionized water, ultrasonically dispersing and uniformly mixing, adding into a four-neck flask provided with a condenser tube, removing oxygen by nitrogen, heating to 90-100 ℃, and heating for 1 mL/min-1Dropwise adding an ammonia water solution at the speed of (1) until the pH value is 7-12, and reacting for 1-5 h; performing solid-liquid separation by using an external magnetic field, washing the precipitate for more than 2 times by using deionized water and ethanol, and freeze-drying to obtain ferroferric oxide nanoparticles;
(2) preparing manganese dioxide nano particles: dissolving potassium permanganate, a hydrochloric acid solution and a reducing agent in deionized water, transferring the solution to a hydrothermal synthesis kettle, keeping the solution at the temperature of 100-150 ℃ for 8-15 h, naturally cooling to room temperature, washing the precipitate with the deionized water and ethanol for more than 2 times, and freeze-drying to obtain manganese dioxide nanoparticles;
(3) graphene oxide is prepared according to an improved Hummers method, and then prepared to have a concentration of 8-15 mg/mL-1The slurry of (4);
(4) adding graphene oxide slurry, ferroferric oxide nanoparticles and manganese dioxide nanoparticles into a beaker according to the mass ratio of 1: 1-5: 1-5, ultrasonically dispersing and uniformly mixing, then transferring into a hydrothermal synthesis kettle, heating to 120-;
(5) and heating the obtained magnetic graphene aerogel particle electrode precursor to 400-800 ℃ in a hydrogen atmosphere for thermal reduction treatment for 30-60 min to obtain the magnetic graphene aerogel particle electrode.
3. The process according to claim 2, wherein the molar ratio of ferrous chloride to ferric chloride in step (1) is 1: 1-3.
4. The preparation method according to claim 2, wherein the reducing agent in step (2) is one or a mixture of hydrazine hydrate, urea and glucose.
5. The process according to claim 2, wherein the concentration of hydrochloric acid in step (2) is 2 mol-L-1
6. The production method according to claim 2, characterized in that the mass ratio of the reducing agent to potassium permanganate in step (2) of the method is 1: 1-6.
7. A magnetic graphene aerogel particle electrode prepared by the preparation method of any one of claims 1 to 6.
CN201911112532.3A 2019-11-14 2019-11-14 Magnetic graphene aerogel particle electrode and preparation method thereof Pending CN111003757A (en)

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Cited By (4)

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CN111686679A (en) * 2020-06-01 2020-09-22 山西大学 Preparation method and application of manganese dioxide aerogel material
CN112456634A (en) * 2020-10-15 2021-03-09 南京工业大学 Water body purification system device with photo/bioelectrochemical integrated module and application thereof
WO2022073350A1 (en) * 2021-05-21 2022-04-14 广东省科学院测试分析研究所(中国广州分析测试中心) Method for three-dimensional electro-fenton degredation of antiviral drug residue in water based on magnetic graphene oxide catalytic particle electrode
CN115445565A (en) * 2022-08-15 2022-12-09 中国石油化工股份有限公司 Copper-doped graphene aerogel for adsorbing VOCs (volatile organic compounds) and preparation method thereof

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CN109295716A (en) * 2018-09-14 2019-02-01 晋江瑞碧科技有限公司 A kind of preparation method of magnetic, temperature collaboration stimuli responsive hydrogel
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111686679A (en) * 2020-06-01 2020-09-22 山西大学 Preparation method and application of manganese dioxide aerogel material
CN112456634A (en) * 2020-10-15 2021-03-09 南京工业大学 Water body purification system device with photo/bioelectrochemical integrated module and application thereof
CN112456634B (en) * 2020-10-15 2022-12-27 南京工业大学 Water body purification system device with photo/bioelectrochemical integrated module and application thereof
WO2022073350A1 (en) * 2021-05-21 2022-04-14 广东省科学院测试分析研究所(中国广州分析测试中心) Method for three-dimensional electro-fenton degredation of antiviral drug residue in water based on magnetic graphene oxide catalytic particle electrode
CN115445565A (en) * 2022-08-15 2022-12-09 中国石油化工股份有限公司 Copper-doped graphene aerogel for adsorbing VOCs (volatile organic compounds) and preparation method thereof
CN115445565B (en) * 2022-08-15 2023-12-01 中国石油化工股份有限公司 Copper-doped graphene aerogel for adsorbing VOCs and preparation method thereof

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Application publication date: 20200414