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Preparation method and application of nitrogen-doped three-dimensional graphene aerogel loaded nano zero-valent iron

A technology of graphene airgel and nano-zero-valent iron, which is applied in chemical instruments and methods, catalyst activation/preparation, special compound water treatment, etc., can solve the problem of hindering nitrogen-doped graphene airgel/zero-valent iron composite Material application, a large amount of chemical sludge, difficult to recycle and other problems, to achieve the effect of being conducive to recycling, high catalytic activity, and no secondary pollution

Pending Publication Date: 2020-11-17
NANKAI UNIV
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  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The preparation method of graphene / iron-based composite material and its application in advanced oxidation technology have been reported. For example, patent document CN108176400A discloses a nanometer zero-valent iron / graphene composite to activate persulfate to remove atrazine in water. The method, this patent solves the problem that the traditional Fenton catalyst is difficult to recycle and produces a large amount of chemical sludge, and avoids the problem of secondary pollution
However, the graphene in this patent has a two-dimensional structure, which is easy to stack and has not been doped with heteroatoms
However, the application of nitrogen-doped three-dimensional graphene airgel / iron-based composites in advanced oxidation technology has not been reported yet.
The above defects and deficiencies have seriously hindered the application of nitrogen-doped graphene airgel / zero-valent iron composites in advanced oxidation and need to be solved urgently

Method used

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  • Preparation method and application of nitrogen-doped three-dimensional graphene aerogel loaded nano zero-valent iron
  • Preparation method and application of nitrogen-doped three-dimensional graphene aerogel loaded nano zero-valent iron
  • Preparation method and application of nitrogen-doped three-dimensional graphene aerogel loaded nano zero-valent iron

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Experimental program
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Effect test

Embodiment 2

[0046] Add 10 mg of nitrogen-doped three-dimensional graphene airgel-loaded nano-zero-valent iron (nano-zero-valent iron, nitrogen-doped graphene, three-dimensional graphene-loaded nano-zero-valent iron) to a 40 mL EPA bottle, add 200 μL, and then add 200 μL concentration 2000ppm of β-666, and finally add 100 μL of 1M sodium persulfate solution to make the molar ratio of the iron content in the three-dimensional graphene airgel-loaded iron to 1:1, and immediately put it in a shaker for reaction, and the oscillation frequency is 150rpm / min, after the reaction started, 0.5 mL was sampled at 0, 1, 2, 5, 7, 10, 20, and 30 min respectively in a 2 mL centrifuge tube, and 1 mL of n-hexane was added immediately for extraction (shaking table for 30 min), and then 0.7 mL was taken in Gas chromatography-mass spectrometry was used in the injection vial for determination. Experimental results such as and figure 2 shown. The results show that the removal rate of β-666 by sodium persulfa...

Embodiment 3

[0048] Add 10 mg of melamine-doped three-dimensional graphene airgel loaded nano-zero-valent iron into a 40 mL EPA bottle, add an appropriate amount of distilled water, adjust the pH to 1.0, 3.0, 5.0, 7.0, and 9.0 with 1M sulfuric acid or sodium hydroxide, and then add 200 μL of concentration 2000ppm of β-666, and finally add 100 μL of 1M sodium persulfate solution to make the molar ratio of the iron content in the three-dimensional graphene airgel-loaded iron to 1:1, and immediately put it in a shaker for reaction, the oscillation frequency 150rpm / min, after the reaction starts, take 0.5mL samples at 0, 1, 2, 5, 7, 10, 20, and 30min respectively into a 2mL centrifuge tube, immediately add 1mL n-hexane for extraction (shake table for 30min), and then take 0.7mL It was determined by gas chromatography-mass spectrometry in the injection vial. Experimental results such as image 3 shown. The results show that when the reaction time is 5 min, the nitrogen-doped three-dimensional...

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Abstract

The invention discloses a method for preparing a three-dimensional graphene aerogel loaded nano zero-valent iron material by using a calcining-liquid-phase reduction manner. The method comprises the following steps: (1) synthesizing nitrogen-doped graphene oxide; (2) synthesizing nitrogen-doped three-dimensional graphene aerogel; and (3) synthesizing the nitrogen-doped three-dimensional graphene aerogel loaded nano zero-valent iron material. According to the material disclosed by the invention, zero-valent iron particles in the obtained composite material are nano-scale, are uniformly distributed, have high catalytic activity, and interact with persulfate to generate sulfate free radicals and hydroxyl free radicals with strong oxidizing property, so as to degrade organic pollutants. Compared with conventional methods for synthesizing melamine-doped three-dimensional graphene aerogel, the method disclosed by the invention has the characteristics of higher nitrogen content, high reactionrate, high efficiency, easiness in recovery after use, no secondary pollution, simplicity, economy and high operability.

Description

technical field [0001] The invention belongs to the field of composite materials, and in particular relates to a method for preparing nitrogen-doped three-dimensional graphene airgel loaded with nanometer zero-valent iron and its application Background technique [0002] Organochlorine pesticides (organ chlorine pesticides, OCPs) generally have the characteristics of strong toxicity, refractory degradation, and easy enrichment, and some OCPs still have endocrine disruptor properties under low-dose long-term exposure conditions, bringing huge impacts on the ecological environment and human health. potential threats. With the rapid development of my country's industrialization and urbanization and the implementation of the "Stockholm Convention", a large number of OCPs production enterprises have been closed, leaving more than 1200 polluted sites. These polluted sites often have the characteristics of high pollution concentration and deep distribution, and have become importa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J37/16B01J37/08C02F1/72C02F101/30C02F101/36
CPCB01J27/24B01J37/16B01J37/082C02F1/722C02F1/725C02F2101/306C02F2101/36C02F2305/02C02F2305/023B01J35/23B01J35/33B01J35/40
Inventor 张鹏范明毅孙红文
Owner NANKAI UNIV
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