Sulfur and nitrogen codoped graphene-based aerogel and preparation method thereof

An alkene-based aerogel, graphene-based technology, applied in graphene, chemical instruments and methods, other chemical processes, etc., can solve the problem of graphene aerogel with large pore size, secondary heavy metal pollution in water, small specific surface area, etc. problems, to achieve the effect of good recycling performance, avoiding metal pollution in water, and high adsorption capacity

Active Publication Date: 2018-08-24
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The graphene airgel prepared by this method has large pore size, small specific surface area, and low adsorption efficiency; in addition, the raw material contains metal iron ions, which will cause secondary heavy metal pollution to the water body

Method used

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  • Sulfur and nitrogen codoped graphene-based aerogel and preparation method thereof
  • Sulfur and nitrogen codoped graphene-based aerogel and preparation method thereof
  • Sulfur and nitrogen codoped graphene-based aerogel and preparation method thereof

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preparation example Construction

[0041] Graphene oxide in the present application can be commercially available graphene oxide, and can also be prepared according to the preparation method of other documents, and the application provides a kind of preparation method of graphene oxide, and its steps are:

[0042]Slowly add 18g of potassium permanganate and 3g of sodium nitrate into 138mL of concentrated sulfuric acid in an ice bath at 0°C, while mechanically stirring at a speed of 200-500rpm. After the potassium permanganate and sodium nitrate are completely dissolved, slowly Add 3g of expanded graphite, after the expanded graphite is completely stirred evenly, seal it and place it in the refrigerator, and keep it warm at 0°C for 24h; then transfer the reaction system to a constant temperature oil bath at 35°C and stir for 30min, then slowly add deionization dropwise while heating up Water, add a total of 300mL of deionized water dropwise, at this time the temperature just rises to 98°C, keep stirring at 98°C f...

Embodiment 1

[0044] A preparation method of sulfur and nitrogen co-doped graphene-based airgel,

[0045] (1) 80 mg of graphene oxide was added to 40 mL of deionized water, and dispersed by ultrasonic for 1 h until uniformly mixed to obtain a 2 mg / mL graphene oxide aqueous solution.

[0046] (2) Weigh 1.6 g of thiourea as a source of sulfur and nitrogen, mix it with the graphene oxide aqueous solution obtained in step (1), and ultrasonically dissolve it completely for 15 minutes to obtain a mixed aqueous solution of graphene oxide and thiourea.

[0047] (3) Transfer the mixed aqueous solution obtained in step (2) to a high-pressure reactor with a volume of 50 mL, and conduct a hydrothermal reaction at a constant temperature of 160 ° C for 12 hours. After natural cooling, a sulfur-nitrogen co-doped graphene hydrogel precursor is obtained. body.

[0048] (4) Soak the sulfur-nitrogen co-doped graphene hydrogel precursor prepared in step (3) in deionized water for 48 hours, and change the deio...

Embodiment 2

[0063] A preparation method of sulfur and nitrogen co-doped graphene-based airgel,

[0064] (1) Add 120 mg of graphene oxide into 40 mL of deionized water, and ultrasonically disperse for 2 hours until uniformly mixed to obtain a 3 mg / mL graphene oxide aqueous solution.

[0065] (2) Weigh 3.6g of thiourea as a source of sulfur and nitrogen, mix it with the graphene oxide aqueous solution obtained in step (1), and ultrasonically dissolve it completely for 20 minutes to obtain a mixed aqueous solution of graphene oxide and thiourea.

[0066] (3) Transfer the mixed aqueous solution obtained in step (2) to a high-pressure reactor with a volume of 50 mL, and conduct a hydrothermal reaction at a constant temperature of 200 ° C for 8 hours. After natural cooling, a sulfur-nitrogen co-doped graphene hydrogel precursor is obtained. body.

[0067] (4) Soak the sulfur-nitrogen co-doped graphene hydrogel precursor prepared in step (3) in deionized water for 72 hours, during which time th...

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Abstract

The invention discloses a sulfur and nitrogen codoped graphene-based aerogel and a preparation method thereof. The preparation method comprise the following steps: preparing a sulfur and nitrogen codoped graphene hydrogel precursor from graphene oxide and thiourea by a hydrothermal synthesis technology, performing vacuum freeze drying on the precursor, and carbonizing the dried precursor to obtainthe sulfur and nitrogen codoped graphene-based aerogel. The sulfur and nitrogen codoped graphene-based aerogel prepared by the method has the advantages of super hydrophobic property, lipophilic property, good mechanical property, and high oil and organic solvent absorption rate. Additionally, the preparation method has the advantages of simplicity, wide sources of raw materials, greenness and environmental protection.

Description

technical field [0001] The invention belongs to the field of carbon nanomaterials and oil-water separation, and relates to a sulfur-nitrogen co-doped graphene-based airgel with superhydrophobic high oil absorption performance and a preparation method thereof. Background technique [0002] Marine oil spills, industrial oily wastewater, and leaks of organic solvents pose serious hazards to aquatic ecosystems and human health, and there is an urgent need to develop new materials and technologies that can efficiently clean such pollution from the water surface. At present, commonly used materials and technologies mainly include four types: chemical solidification, in-situ combustion, bioremediation, and mechanical repair (adsorbent and oil skimmer), among which the adsorbent adsorption method has in-situ complete removal The potential for oil slicks, while having no adverse impact on the ecosystem, has attracted much attention. [0003] As a good oil slick adsorption material, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/184B01J20/20B01J20/28B01J20/30C02F1/28
CPCB01J20/20B01J20/28047C01B32/184C01B2204/20C01B2204/32C01P2002/80C01P2002/85C01P2004/03C02F1/283B01J20/02B01J20/205B01J20/28011B01J20/28061B01J20/3078B01J20/3085C02F1/281C02F1/40C02F2101/32C02F2305/08
Inventor 慈立杰任小花郭焕焕
Owner SHANDONG UNIV
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