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Preparation method of graphene magnetic aerogel with high adsorption performance

A technology of graphene and aerogel, which is applied in the field of preparation of graphene magnetic aerogel with high adsorption performance, can solve the problems of impurity ions, loss of graphene oxide materials, etc., achieve high adsorption capacity, improve microstructure and specificity Surface area, the effect of high surface area

Inactive Publication Date: 2020-04-17
NORTHWESTERN POLYTECHNICAL UNIV
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Problems solved by technology

[0007] Generally speaking, most of the impurity ions in the solution can be removed by centrifugation, suction filtration, cleaning and other processes. However, while removing impurities, a lot of graphene oxide materials are inevitably lost. In addition, the graphene oxide solution after cleaning , some impurity ions still exist
Therefore, how to reduce the loss of graphene oxide during the purification process while completely removing impurity ions as far as possible remains a great challenge for the preparation of graphene magnetic aerogels with high adsorption performance and good mechanical stability.

Method used

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  • Preparation method of graphene magnetic aerogel with high adsorption performance
  • Preparation method of graphene magnetic aerogel with high adsorption performance
  • Preparation method of graphene magnetic aerogel with high adsorption performance

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preparation example Construction

[0039] (2) Preparation and purification of graphene oxide: the pre-oxidized graphite and sodium nitrate obtained in step (1) are fully mixed with concentrated sulfuric acid in a reaction vessel in a mass ratio of (0.1~1):(0.1~1) , and then kept stirring at 0-8°C for 10-60 minutes. After mixing evenly, add potassium permanganate with a mass ratio of (1-6):(0.1-1) to the pre-oxidized graphene to react for 20-100 minutes, then raise the temperature to 30-60°C to continue the reaction for 10-100 minutes, add 50 ~150 mL deionized water. Then continue to heat up to 80-100°C, keep stirring for 10-40min, and when the reaction solution is cooled to room temperature, add 150-300mL deionized water and 1-10ml 30% hydrogen peroxide solution to obtain a golden yellow graphene oxide solution. Filter the obtained graphene oxide solution, and wash with deionized water and 5%-10% hydrochloric acid for 2-7 times. Finally, the washed product was centrifuged 2 to 7 times under the condition of 1...

Embodiment 1

[0050] The graphite powder was pre-oxidized and the resulting graphene oxide solution was purified by dialysis.

[0051] (1) Take respectively graphite powder (particle diameter is 50~150 μm), concentrated nitric acid, concentrated sulfuric acid and potassium permanganate, with mass ratio (0.5~2):(0.5~2):(0.2~1.5):( 0.2 to 1.5) into the reaction vessel, stirred and mixed to obtain a dark brown viscous liquid. Subsequently, wash the viscous liquid with water (to PH = 6.8-7.2) and dry (dry at a temperature of 50-90°C for 10-20h), and then immediately put the dried sample into a crucible with a temperature of 800-1000°C , cover the crucible lid, and obtain the expanded graphite sample when the crucible is cooled to room temperature. Then get expanded graphite, potassium persulfate and phosphorus pentoxide, in the ratio of (1~5):(1~4):(1~4) in mass ratio in the concentrated sulfuric acid of 80 ℃ and insulate and stir for 1~8h, Then the solution is washed with water so that the p...

Embodiment 2

[0063] The graphite powder was pre-oxidized, and the resulting graphene oxide solution was not purified by dialysis.

[0064] (1) Take respectively graphite powder (particle diameter is 50~150 μm), concentrated nitric acid, concentrated sulfuric acid and potassium permanganate, with mass ratio (0.5~2):(0.5~2):(0.2~1.5):( 0.2 to 1.5) into the reaction vessel, stirred and mixed to obtain a dark brown viscous liquid. Subsequently, wash the viscous liquid with water (to PH = 6.8-7.2) and dry (dry at a temperature of 50-90°C for 10-20h), and then immediately put the dried sample into a crucible with a temperature of 800-1000°C , cover the crucible lid, and obtain the expanded graphite sample when the crucible is cooled to room temperature. Then get expanded graphite, potassium persulfate and phosphorus pentoxide, in the ratio of (1~5):(1~4):(1~4) in mass ratio in the concentrated sulfuric acid of 80 ℃ and insulate and stir for 1~8h, Then the solution is washed with water so that th...

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Abstract

The invention relates to a preparation method of graphene magnetic aerogel with high adsorption performance. The preparation method comprises the following steps: preparing Fe3O4 magnetic nanoparticles from anhydrous sodium acetate, polyvinylpyrrolidone, ferric chloride hexahydrate and ethylene glycol; pre-oxidizing crystalline flake graphite by using a pre-oxidation method, and then preparing a graphene oxide solution by using an improved Hummers method; compounding Fe3O4 and graphene through a solvothermal method, and preparing a graphene magnetic hydrogel through reduction; and finally, preparing a graphene magnetic aerogel material through a freeze drying method. Adsorption experiments show that the prepared graphene magnetic aerogel has the advantages of high adsorption capacity, highsurface area and the like, and is greatly improved in adsorption performance on pollutants such as dyes, organic solvents, heavy metal particles and the like, so the graphene magnetic aerogel has good application prospects in the fields of sewage treatment and the like.

Description

technical field [0001] The invention belongs to the field of non-metallic composite materials, and also belongs to the fields of chemistry, chemical industry, agriculture and environmental engineering, and relates to a preparation method of graphene magnetic airgel with high adsorption performance. Background technique [0002] With the deepening of the industrialization process and the rapid development of the economy, people's living standards have been greatly improved, but the resulting pollutants (such as persistent organic pollutants, heavy metals, dyes and pesticides, etc.) inevitably It has a great impact on the environment we live in. Therefore, how to effectively control these pollutants has become a key problem to be solved urgently. [0003] Three-dimensional foam materials, such as sponge, foamed carbon, and aerogel, are of great importance in the fields of heat insulation, sound insulation, energy storage, sensors, catalysis, adsorption, and the environment due...

Claims

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Application Information

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IPC IPC(8): B01J20/20B01J20/28B01J20/06C01B32/19C01G49/08B01D15/08C02F1/28C02F101/20C02F101/30
CPCB01D15/08B01J20/06B01J20/20B01J20/28009B01J20/28047B01J2220/42B01J2220/4806B01J2220/4812C01G49/08C01P2004/03C01P2004/04C01P2004/80C02F1/281C02F1/283C02F2101/20C02F2101/30C02F2101/308C01B32/19
Inventor 党阿磊王羽佳李铁虎赵廷凯李昊艾艳玲
Owner NORTHWESTERN POLYTECHNICAL UNIV
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