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Preparation method of nitrogen- and phosphorus-doped graphene sheet

A graphene sheet, nitrogen and phosphorus technology, applied in nanotechnology and other directions, can solve the problems of high price and complex preparation process, and achieve the effect of simple source

Active Publication Date: 2015-08-05
JINING XINRUIDA INFORMATION TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to provide a method for preparing nitrogen-phosphorus-doped graphene sheets in order to overcome the deficiencies in the prior art such as complex preparation process and high price

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] According to the amount of 2 mmol of tetramethylammonium bromide per gram of bentonite, add commercially available bentonite that has passed through a 20-mesh sieve into a tetramethylammonium bromide solution with a concentration of 0.1% by mass, and stir in a constant temperature water bath at 60°C for 5 hours , aging for 12h to obtain the bentonite suspension modified by tetramethylammonium bromide; then according to the corresponding amount of 0.5mmol of 4-dimethylaminopyridine and 1.5mmol of n-butyl phosphate per gram of bentonite, the 4-dimethyl Add aminopyridine and n-butyl phosphate to tetramethylammonium bromide-modified bentonite suspension, stir in a constant temperature water bath at 60°C for 6 hours, separate the precipitate from the liquid, and wash the precipitate twice with deionized water , dried, ground, and passed through a 20-mesh sieve to obtain modified bentonite powder; put the obtained modified bentonite powder into a vacuum tube furnace, heat to 4...

Embodiment 2

[0024] According to the amount of 3 mmol of tetramethylammonium bromide per gram of bentonite, add commercially available bentonite through a 50-mesh sieve to a tetramethylammonium bromide solution with a concentration of 1% by mass, and stir in a constant temperature water bath at 70°C for 6 hours , aging for 24h to obtain the bentonite suspension modified by tetramethylammonium bromide; then according to the corresponding amount of 1.5mmol of 4-dimethylaminopyridine and 0.5mmol of n-butyl phosphate per gram of bentonite, the 4-dimethyl Add aminopyridine and n-butyl phosphate to tetramethylammonium bromide-modified bentonite suspension, stir in a constant temperature water bath at 70°C for 8 hours, separate the precipitate from the liquid, and wash the precipitate 3 times with deionized water , dried, ground, and passed through a 40-mesh sieve to obtain modified bentonite powder; put the obtained modified bentonite powder into a vacuum tube furnace, heat to 600 ° C under vacuu...

Embodiment 3

[0026] According to the amount of 2 mmol of tetramethylammonium bromide per gram of bentonite, add bentonite that has passed through a 20-mesh sieve into a tetramethylammonium bromide solution with a concentration of 0.5% by mass, stir in a constant temperature water bath at 60°C for 6 hours, and age 24h, obtain the bentonite suspension liquid modified by tetramethylammonium bromide; Then according to the 4-dimethylaminopyridine of 0.75mmol and the n-butyl phosphate of 0.75mmol according to every gram of bentonite, the 4-dimethylaminopyridine Add n-butyl phosphate and tetramethylammonium bromide modified bentonite suspension, stir in a constant temperature water bath at 70°C for 8 hours, separate the precipitate from the liquid, wash the precipitate 3 times with deionized water, and dry Dry, grind, and pass through a 40-mesh sieve to obtain modified bentonite powder; put the obtained modified bentonite powder into a vacuum tube furnace, heat to 500°C under vacuum conditions, va...

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Abstract

The invention discloses a preparation method of a nitrogen- and phosphorus-doped graphene sheet. The preparation method particularly includes following steps: adding bentonite to a proper amount of a tetramethyl ammonium bromide solution, stirring the mixture, aging the mixture, adding 4-dimethylamino pyridine and n-butyl phosphate, stirring the mixture in a constant-temperature water bath at 60-70 DEG C for 6-8 h, separating a precipitation from liquid, washing the precipitation with deionized water for 2-3 times, drying and grinding the precipitation, sieving the precipitation through a sieve being 20-40 in meshes to obtain modified bentonite powder, heating the modified bentonite powder in a vacuum tubular furnace to 400-600 DEG C under a vacuum condition for calcining the powder for 2-4 h, adding the calcined powder in a hydrofluoric acid solution, separating the precipitation and finally heating the precipitation to 2000-2500 DEG C under the vacuum condition to perform heat treatment for 3-6 h, and cooling a product to obtain the nitrogen- and phosphorus-doped graphene sheet. The preparation method is simple in raw materials and is mild in conditions.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation, and in particular relates to a preparation method of nitrogen and phosphorus doped graphene sheets. Background technique [0002] In the research and development of new materials, dimensionality has become an important parameter for modulating the structure and properties of matter. When the material changes from three-dimensional structure to two-dimensional, one-dimensional and zero-dimensional, its geometric structure and physical and chemical properties will change significantly. Two-dimensional nanomaterials have been widely used in many fields such as solid-state nanodevices, sensing and functional thin films due to their anisotropy and unique optoelectronic properties. In particular, highly oriented graphitic carbon 001 has a unique resistance to radiation, which is expected to be used in medical low-energy neutron radiation-resistant materials, X-Ray monochromator radiat...

Claims

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Application Information

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IPC IPC(8): C01B31/04B82Y40/00
Inventor 黄文艳黄勇
Owner JINING XINRUIDA INFORMATION TECH CO LTD
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