Preparation method of nitrogen-doped graphene material

A nitrogen-doped graphene and graphite technology, applied in graphene, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of harsh operating conditions, high alkalinity, and single nitrogen species in nitrogen-doped graphene , to achieve the effect of low cost and high nitrogen content

Active Publication Date: 2014-04-02
NANKAI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This type of method has many reaction processes and harsh operating conditions
In addition, the nitrogen species of nitrogen-doped graphene prepared by many preparation methods is relatively single and the basicity is generally low, so the application range is narrow
Therefore, how to prepare nitrogen-doped graphene with a wide variety of nitrogen species and high basicity on a large scale with a simple and cheap method remains a great challenge.

Method used

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  • Preparation method of nitrogen-doped graphene material
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  • Preparation method of nitrogen-doped graphene material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Preparation of graphite oxide: Add 240mL of concentrated sulfuric acid and 30mL of concentrated phosphoric acid into a three-neck flask, add 6g of graphite powder, then slowly add 18g of potassium permanganate, stir at 50°C for 6-24h, then add 400mL of water . At this point the temperature rose sharply to 98°C and was maintained for 30 minutes. Add 3 mL of 30% hydrogen peroxide.

[0028] (2) Purification of graphite oxide: the turbid liquid obtained in (1) was left to stand, and then decanted. Decant four times with deionized water, then six times with ethanol. Graphite oxide can be obtained by vacuum drying at 80°C for 24 hours.

[0029] (3) Preparation of graphene oxide: 10 g of graphite oxide was weighed and added to 1 L of deionized water and stirred slowly. After stirring for 30 minutes, ultrasonically disperse for 30 minutes. The obtained aqueous solution is the aqueous solution of graphene oxide. The pH value of the aqueous solution is between 4 and 5. ...

Embodiment 2

[0036] The difference between this example and example 1 is that the amine used is 70% ethylamine, the amount added is 26g, and the obtained sample is recorded as EAGO.

[0037] All the other contents are the same as those described in Example 1.

[0038] The Raman spectrum and XPS spectrogram of gained nitrogen-doped graphene are as figure 2 shown.

[0039] The high-resolution C 1s XPS spectrum of gained nitrogen-doped graphene and the high-resolution N 1s XPS spectrum are as follows image 3 shown.

Embodiment 3

[0041] The difference between this example and Example 1 is that the amine used is 30% methylamine, the amount added is 40 g, and the obtained sample is marked as MAGO.

[0042] All the other contents are the same as those described in Example 1.

[0043] The Raman spectrum and XPS spectrogram of gained nitrogen-doped graphene are as figure 2 shown.

[0044]The high-resolution C 1s XPS spectrum of gained nitrogen-doped graphene and the high-resolution N 1s XPS spectrum are as follows image 3 shown.

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Abstract

The invention relates to a preparation method of a nitrogen-doped graphene material. The preparation method comprises the following steps: adding a micro-molecule fatty amine water solution into a water solution of graphite oxide dispersed by ultrasound, performing hydrothermal reaction for 36-72 hours, separating out precipitate, washing and drying to obtain the nitrogen-doped graphene material. The material containing nitrogen and carbon prepared by the preparation method is high in nitrogen content, and contains different nitrogen species such as secondary amine and pyridine nitrogen, so that the surface of the prepared material has alkali centers with different intensities, wherein the secondary amine is super base. In addition, the proportion and content of nitrogen species can be controlled by changing the species of micro-molecule amine, so that the effect of controlling the alkalinity and the alkali amount of a catalyst is achieved. The actual operation of the method is simple and feasible, and the preparation material does not contain any metal element, so the nitrogen-doped graphene material is a green environment-friendly catalyst. Good catalytic activity is shown in Michael addition reaction and ester exchange reaction, and the catalyst is in favor of separation and purification of products, so the catalyst has a potential industrial application value.

Description

technical field [0001] The invention relates to the preparation of a nitrogen-containing carbon material, in particular to a preparation method of a nitrogen-doped graphene material. Background technique [0002] Metal-free catalysts are emerging green catalysts that are more efficient, environmentally friendly and economical in many industrial catalysis fields. Carbon materials are an important class of non-metallic catalysts developed in recent years. They do not add or support any metal elements but directly use carbon materials themselves as catalysts. Carbon material catalysts have shown superior performance to traditional metal catalysts in reactions such as alkylation reactions, carbonylation reactions, rearrangement reactions, and cycloaddition reactions, and have great potential, so they have gradually become the frontier in the field of non-metallic catalysis. [0003] Graphene is an important class of carbon materials developed in recent years. It is a two-dimens...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24C01B31/04C01B32/184
Inventor 关乃佳张义成李兰冬武光军
Owner NANKAI UNIV
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