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Three-dimensional graphene-based nano zero-valent iron material as well as preparation method and application thereof

A nano-zero-valent iron, graphene-based technology, applied in chemical instruments and methods, catalyst activation/preparation, water/sludge/sewage treatment, etc., can solve the application of three-dimensional graphene/iron-based composite materials. The application of graphene/zero-valent iron composite materials, etc., to achieve the effect of improving the transfer effect of electrons, strong stability and strong magnetism, and mild reaction conditions

Inactive Publication Date: 2020-02-28
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] However, the graphene-based composite material prepared by the above-mentioned patents has a maximum load of iron-based materials of only 30wt%-40wt%, and there is still a lot of room for improvement.
Meanwhile, the application of 3D graphene / iron-based composites in advanced oxidation technology has not been reported yet
The above defects and deficiencies have seriously hindered the application of graphene / zero-valent iron composites in advanced oxidation and need to be solved urgently

Method used

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  • Three-dimensional graphene-based nano zero-valent iron material as well as preparation method and application thereof
  • Three-dimensional graphene-based nano zero-valent iron material as well as preparation method and application thereof
  • Three-dimensional graphene-based nano zero-valent iron material as well as preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Weigh 2g graphite powder and 1g NaNO 3 To mix, add 46 mL concentrated H 2 SO 4 Place in an ice bath and add 6 g of KMnO with rapid stirring 4 , to obtain mixture C. KMnO 4 It must be added slowly to the reaction solution to prevent the temperature of the reaction system from increasing sharply, and the temperature of the reaction solution should be controlled below 20°C. After reacting for 2 h, the mixture C was transferred to a warm water bath at 35° C. to continue the reaction for 40 min. After the reaction, add 92mL deionized water while stirring, control the temperature of the reaction solution at about 98°C, continue stirring for 30min, add 440mL deionized water to dilute, and slowly add a certain amount of H 2 o 2 Carry out high-temperature reaction, at this time the reaction solution turns golden yellow (generally hydrogen peroxide 10-50mL), and mixture D is obtained. The two additions of deionized water must be added slowly, because unreacted concentrated...

Embodiment 2

[0062] Weigh 2g graphite powder and 1g NaNO 3 To mix, add 46 mL concentrated H 2 SO 4 Place in an ice bath and add 8 g of KMnO with rapid stirring 4 , to obtain mixture C. KMnO 4 It must be added slowly to the reaction solution to prevent the temperature of the reaction system from increasing sharply, and the temperature of the reaction solution should be controlled below 20°C. After reacting for 2 h, the mixture C was transferred to a warm water bath at 35° C. to continue the reaction for 45 min. After the reaction, add 100mL deionized water while stirring, control the temperature of the reaction solution at about 98°C, continue stirring for 35 minutes, add 500mL deionized water to dilute, and slowly add a certain amount of H 2 o 2 A high-temperature reaction was carried out, and the reaction solution turned golden yellow at this time, and a mixture D was obtained. The two additions of deionized water must be added slowly, because unreacted concentrated sulfuric acid w...

Embodiment 3

[0066] Add 6 mg of three-dimensional graphene-based nano-zero-valent iron material into a 40 mL EPA bottle (the mass ratio of three-dimensional graphene to iron element is 1:3, and the same mass of nano-zero-valent iron is used as a control), add an appropriate amount of distilled water, and then add 40 μL concentration For phorate of 10000ppm, finally add 62 μL of 800mM sodium persulfate solution to make the molar ratio of iron content in the three-dimensional graphene-based nano-zero-valent iron material to 1:1, and immediately put it in a shaker for reaction, and the oscillation frequency 150rpm / min, after the reaction started, 0.5mL samples were taken at 0, 0.5, 1, 1.5, 2, 3, 4, 5, 7, and 10min respectively in a 2mL centrifuge tube, and 1mL n-hexane was added immediately for extraction (shaking table for 30min). Then take 0.7mL and measure it by gas chromatography-mass spectrometry in the injection vial.

[0067] The experimental results are shown in Table 1 and image 3A...

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Abstract

The invention discloses a preparation method of a three-dimensional graphene-based nano zero-valent iron material. The preparation method comprises the following steps: step 1, preparing a three-dimensional graphene aerogel; step 2, loading nano zero-valent iron, wherein 2.1, mixing the three-dimensional graphene aerogel with a ferrous or ferric iron solution under nitrogen gas condition to obtaina mixed solution A, controlling the mass ratio of three-dimensional graphene to iron to be 1: 1-1: 10; 2.2, adding sodium borohydride into the mixed solution A, reacting for 20-40 min, and carrying out suction filtration to obtain a product B, and controlling the molar ratio of iron to sodium borohydride to be 1: 1-1: 10; 2.3, subjecting the product B to washing with absolute ethyl alcohol and freeze drying for 12-36h to obtain the three-dimensional graphene-based nano zero-valent iron material. Compared with a previous one-step hydrothermal synthesis method, the method has the advantages that the reaction conditions are milder, and the prepared three-dimensional graphene-based nano zero-valent iron material is controllable in morphology, high in iron loading capacity, easy to recycle after being used, free of secondary pollution, simple, economical and high in operability.

Description

technical field [0001] The invention relates to the field of functional composite materials, in particular to a three-dimensional graphene-based nanometer zero-valent iron material and its preparation method and application. Background technique [0002] Advanced oxidation technology uses a series of physical and chemical interactions (including the synergistic effect of oxidants and catalysts) to generate highly active free radicals in the system to oxidize and decompose refractory organic pollutants into small molecular substances. Compared with the incompleteness of reduction technology, advanced oxidation technology is to convert organic pollutants into carbon dioxide, water and inorganic substances, or convert them into biodegradable or harmless products. Commonly used oxidizing agents mainly include Fenton’s reagent , potassium permanganate, hydrogen peroxide, persulfate, percarbonate and ozone. Compared with other oxidants, persulfate is relatively stable at room tem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/745B01J21/18B01J37/16B01J37/32B01J35/10C02F1/72C02F101/30
CPCB01J23/745B01J21/18B01J37/16B01J37/32C02F1/725C02F2101/30B01J35/394B01J35/61
Inventor 张鹏范明毅孙红文
Owner NANKAI UNIV
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