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Preparation method of two-dimension nitrogen- and phosphorus-doped graphene

A technology of graphene and nitrogen and phosphorus, which is applied in the field of preparation of two-dimensional nitrogen and phosphorus doped graphene, can solve the problems of complex preparation process and high price, and achieve the effect of simple process and 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

[0009] The purpose of the present invention is to provide a method for preparing two-dimensional nitrogen-phosphorus-doped graphene 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

[0023] According to the amount of 0.5 mmol sodium butyrate per gram of hydrotalcite, commercially available magnesium aluminum hydrotalcite passing through a 20-mesh sieve was added to a sodium butyrate solution with a concentration of 0.1% by mass, and stirred in a constant temperature water bath at 60°C for 5 hours. Aged for 12h to obtain the hydrotalcite suspension modified by butyric acid; then according to the corresponding amount per gram of hydrotalcite being 0.5mmol of 4-dimethylaminopyridine and 1.5mmol of n-butyl phosphate, 4-dimethylaminopyridine and Add n-butyl phosphate to the hydrotalcite suspension modified by butyric acid, stir in a constant temperature water bath at 60°C for 6 hours, separate the precipitate from the liquid, wash the precipitate twice with deionized water, dry it, and grind it. Pass through a 20-mesh sieve to obtain modified hydrotalcite powder; put the obtained modified hydrotalcite powder into a vacuum tube furnace, heat to 400°C under vacuum...

Embodiment 2

[0025] According to the amount of 1 mmol sodium butyrate per gram of hydrotalcite, commercially available nickel-aluminum hydrotalcite passed through a 50-mesh sieve was added to a sodium butyrate solution with a mass percent concentration of 1%, stirred in a constant temperature water bath at 70°C for 6 hours, and aged 24h, obtain butyric acid-modified hydrotalcite suspension; then according to the 4-dimethylaminopyridine of 1.5mmol and the n-butyl phosphate of 0.5mmol according to every gram of hydrotalcite, 4-dimethylaminopyridine and phosphoric acid Add n-butyl ester to the hydrotalcite suspension modified by butyric acid, 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, dry, grind, and pass 40-mesh sieve to obtain modified hydrotalcite powder; put the obtained modified hydrotalcite powder into a vacuum tube furnace, heat to 600°C under vacuum conditions, vacuum calcin...

Embodiment 3

[0027] Firstly, the magnesium-aluminum hydrotalcite was synthesized according to the literature (hydrothermal synthesis of magnesium-aluminum hydrotalcite, Applied Chemistry, 2001, 18, 70-72); the hydrotalcite was passed through a 40-mesh sieve for later use.

[0028]According to the amount of 0.8 mmol sodium butyrate per gram of hydrotalcite, the hydrotalcite passed through a 20-mesh sieve was added to a sodium butyrate solution with a mass percent concentration of 0.5%, stirred in a constant temperature water bath at 60°C for 6 hours, and aged for 24 hours to obtain Butyric acid modified hydrotalcite suspension; then according to the 4-dimethylaminopyridine and the n-butyl phosphate of 0.75mmol in the corresponding amount per gram of hydrotalcite, the 4-dimethylaminopyridine and n-butyl phosphate Add it to the hydrotalcite suspension modified by butyric acid, stir in a constant temperature water bath at 70°C for 8 hours, separate the precipitate from the liquid, wash the prec...

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Abstract

The invention discloses a preparation method of two-dimension nitrogen- and phosphorus-doped graphene. The preparation method particularly includes following steps: adding hydrotalcite to a proper amount of a sodium butyrate solution, stirring the mixture, aging the mixture, adding 4-dimethyl aminopyridine 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 hydrotalcite powder, heating the modified hydrotalcite 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 to a hydrochloric 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 two-dimension nitrogen- and phosphorus-doped graphene. 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 two-dimensional nitrogen and phosphorus doped graphene. 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 monochromat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/00
Inventor 黄文艳黄勇
Owner JINING XINRUIDA INFORMATION TECH CO LTD
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