Nitrogen mixed grapheme hydrogel or aerogel and preparation method thereof

A nitrogen-doped graphene and hydrogel technology, which is applied in the field of hydrogel and aerogel, can solve the problems that the research on nitrogen-doped graphene assembly has not been carried out, and the self-assembly process of graphene units is limited, so as to achieve nitrogen-doped Controllable content, low equipment requirements and high production efficiency

Inactive Publication Date: 2013-01-16
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] But so far, the research on the assembly of nitrogen-doped graphene has hardly been carried out, especially the preparation of nitrogen-doped graphene

Method used

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  • Nitrogen mixed grapheme hydrogel or aerogel and preparation method thereof
  • Nitrogen mixed grapheme hydrogel or aerogel and preparation method thereof
  • Nitrogen mixed grapheme hydrogel or aerogel and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0033] (1) Preparation of graphene oxide dispersion:

[0034] Using natural graphite as raw material, graphite oxide was prepared by the Hummers method, and the specific steps were as follows: 5 g graphite powder was added to 1.5 L containing 115 mL 98% H -2 SO 4 In a three-necked flask, stir at room temperature for 24 h; add 2.5 g of NaNO to the three-necked flask 3, continue to stir for 30 min, and place the three-necked flask in an ice bath (4 , control the system temperature to 2 0 2 Reduction of unreacted KMnO 4 and MnO 2 , to terminate the reaction; the mixed system was vacuum filtered while it was hot, and the filter cake was washed with 700 mL of deionized water, and the obtained solid was dried in a vacuum oven at 40 °C for later use. Grind the obtained graphite oxide into a fine powder of 1-100 microns, use water as the solvent, stir magnetically for 24 hours until the dispersion is uniform, and obtain a 2mg / ml graphite oxide dispersion; then perform ultrasonic t...

Embodiment 2

[0040] (1) Preparation of graphene oxide dispersion:

[0041] Using flake graphite as raw material, graphite oxide is prepared by Hummers method; the obtained graphite oxide is ground into a fine powder of 1-100 microns, and water / ethanol (volume ratio 1:1) is used as solvent, and magnetically stirred for 24 hours until the dispersion is uniform. A graphite oxide dispersion of 4 mg / ml was obtained; then ultrasonic treatment was performed at 40KHz / 100W for 1 h, and centrifugation was performed at a centrifugal rate of 4500 rpm for 0.5 h, and the obtained supernatant was the graphene oxide dispersion.

[0042] (2) Preparation of nitrogen-doped graphene hydrogel:

[0043] According to the mass ratio of 80% hydrazine hydrate to graphene oxide of 10:1, add 80% hydrazine hydrate to the above dispersion, mix evenly under magnetic stirring, transfer to a closed container; then react at 35°C for 36h, after the reaction is completed Cool at room temperature to prepare nitrogen-doped gr...

Embodiment 3

[0047] (1) Preparation of graphene oxide dispersion:

[0048] Using artificial graphite as raw material, graphite oxide is prepared by the Staudenmaier method; the obtained graphite oxide is ground into a fine powder of 1-100 microns, and water / methanol (volume ratio 3:1) is used as a solvent, and magnetically stirred for 24 hours until the dispersion is uniform. Obtain 1.5mg / ml graphite oxide dispersion; then perform ultrasonic treatment at 40KHz / 200W for 20min, and centrifuge at 5000rpm for 15min, the obtained supernatant is graphene oxide dispersion.

[0049] (2) Preparation of nitrogen-doped graphene hydrogel:

[0050] According to the mass ratio of urea to graphene oxide is 20:1, add urea to the above dispersion, ultrasonically disperse evenly, transfer to a hydrothermal reaction kettle; then place it in a homogeneous reactor at 200°C, react for 4h, and the reaction is complete After cooling at room temperature, a nitrogen-doped graphene hydrogel was prepared. The prepa...

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Abstract

The invention provides nitrogen mixed grapheme hydrogel of which the water content is 90 to 99.5 percent, the electric conductivity is 10-3-100 S/m, and the molar ratio of N and C is 1 to 25 percent. The invention further provides nitrogen mixed aerogel of which the molar ratio of N and C is 2 to 20 percent, the molar ratio of C and O is 15 to 5, nitrogen atoms existing in the form of amidogen nitrogen accounts for 40 to 70 percent, pyridine type nitrogen accounts for 10 to 40 percent, graphite type nitrogen accounts for 10 to 30 percent, the specific area is 300 to 1500 m<2>/g, the apertures which are micropore account for 10 to 20 percent, the apertures which are mesoporous 20 to 50 percent, the apertures which are macropore 30 to 70 percent, the apparent density is 0.01 to 0.2 g/cm<3>, the pore volume is 5 to 20 cm<3>/g, and the electric conductivity is 1 to 1000 S/m. The nitrogen mixed grapheme hydrogel or aerogel and preparation method thereof provided by the invention has the characteristics that the operation is simple, the equipment requirement is low, the production efficiency is high, the scale-up of the technology is easy, the nitrogen mixed content is controllable and the compounding with other functional substances is simple.

Description

technical field [0001] The invention belongs to a hydrogel and aerogel technology, and more specifically relates to a nitrogen-doped graphene hydrogel or aerogel and a preparation method thereof. Background technique [0002] Graphene is a new type of carbon material following fullerene and carbon nanotubes. Since Geim et al. successfully prepared single-layer graphene by mechanical exfoliation in 2004, it has set off graphite in various fields with its unique properties. The upsurge of ene research. Graphene is SP 2 The hybridized carbon atoms are arranged in a hexagonal lattice to form a sheet-like monolayer, which is a perfect two-dimensional structure material; it has an ultra-high specific surface area (2600 m 2 g -1 ), high thermal conductivity (5000 Wm -1 K -1 ), extremely high carrier mobility (2×10 5 cm 2 V -1 the s -1 ) and strong Young's modulus (1 TPa), so the research of graphene in energy storage, catalysis, sensors, electronic devices, composite mate...

Claims

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Application Information

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IPC IPC(8): C01B31/04C01B32/184
Inventor 孙予罕王刚李德宝贾丽涛
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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