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Method for preparing nitrogen-doped graphene with high nitrogen doping amount

A nitrogen-doped graphene and graphene technology, applied in the field of nitrogen-doped graphene, can solve the problems of low doping amount, harsh preparation conditions, and high production cost, and achieve low environmental pollution, simple reactant components, and production equipment. less effect

Active Publication Date: 2014-12-24
FUJIAN XFH NEW ENERGY MATERIALS CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In view of this, the present invention aims at the deficiencies in the prior art, and its main purpose is to provide a method for preparing nitrogen-doped graphene with a high nitrogen doping amount, which can effectively solve the problem of existing nitrogen-doped graphene synthesis methods. Harsh conditions, low doping content (not higher than 10%), high production costs, etc.

Method used

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  • Method for preparing nitrogen-doped graphene with high nitrogen doping amount

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Graphene dispersion: A graphene dispersion with a concentration of 1.0 mg / mL is prepared, the dispersant is multilayer graphene, and the dispersant is deionized water.

[0023] (2) Ultrasonic dispersion: The graphene dispersion and the nitrogen source are mixed at a certain mass ratio of 1:0.1, and after ultrasonic treatment for 2 hours, a mixture A is obtained. The nitrogen source is polypyrrole, polyaniline and polypyridine.

[0024] (3) Microwave heating: Move the mixture A into a 50mPa autoclave, then place the reactor in a microwave oven with a power of 2000w and heat it for 600s to obtain a mixture B.

[0025] (4) Filtration and drying: Filter the mixture B in a 0.2μm PTFE membrane filter, and the resulting filter cake is dried at a temperature of 80°C for 200 minutes to obtain nitrogen-doped graphene. The nitrogen doping amount is shown in Table 1. .

Embodiment 2

[0027] (1) Graphene dispersion: prepare a graphene dispersion with a concentration of 2.0 mg / mL, the dispersant is double-layer graphene, and the dispersant is dehydrated ethanol.

[0028] (2) Ultrasonic dispersion: The graphene dispersion and the nitrogen source are mixed at a certain mass ratio of 1:3, and after ultrasonic treatment is 0.5, the mixture A is obtained, and the nitrogen source is triethylenetetramine.

[0029] (3) Microwave heating: Move the mixture A into an autoclave with a pressure of 1 mPa, and then place the reactor in a microwave oven with a power of 1500 W and heat it for 10 seconds to obtain a mixture B.

[0030] (4) Filtration and drying: The mixture B is filtered in a 0.2μm PTFE membrane filter, and the resulting filter cake is dried at a temperature of 150°C for 20 minutes to obtain nitrogen-doped graphene. The nitrogen doping amount is shown in Table 1. .

Embodiment 3

[0032] (1) Graphene dispersion: prepare a graphene dispersion with a concentration of 3.0 mg / mL, the dispersant is multilayer graphene, and the dispersant is acetone.

[0033] (2) Ultrasonic dispersion: The graphene dispersion and the nitrogen source are mixed at a certain mass ratio of 1:10, and after ultrasonic treatment for 0.8 hours, a mixture A is obtained. The nitrogen source is melamine and dopamine.

[0034] (3) Microwave heating: Move the mixture A into an autoclave with a pressure of 5mPa, then place the reactor in a microwave oven with a power of 600w and heat it for 600s to obtain a mixture B.

[0035] (4) Filtration and drying: Filter the mixture B in a 0.2μm PTFE membrane filter, and the resulting filter cake is dried at a temperature of 100°C for 80 minutes to obtain nitrogen-doped graphene. The nitrogen doping amount is shown in Table 1. .

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Abstract

The invention discloses a method for preparing nitrogen-doped graphene with high nitrogen doping amount. The method comprises the following steps: (1) dispersing of graphene; (2) ultrasonic dispersion; (3) microwave heating; and (4) filtering and drying. The nitrogen doping amount of the nitrogen-doped graphene prepared by the method disclosed by the invention is 10%-15.0%, the density of free carriers in graphene is greatly increased by the high nitrogen doping amount, the interaction of graphene and metal is enhanced, no oxidation pretreatment is carried out, no toxic solvent is used in the reaction process, reactants are simple in component, reaction conditions are mild, and the prepared nitrogen-doped graphene has excellent electrochemical property and can be used for preparation of new energy materials such as lithium ion battery, lithium-air battery, super capacitor electrode material and fuel cell oxygen reduction catalysts. According to the method disclosed by the invention, a high-pressure kettle is heated by using microwaves without high temperature; the method is low in energy consumption, is carried out in an airtight environment and therefore hardly causes environment pollution; in addition, the method is simple in process and convenient to operate and needs less production equipment, thus, the cost is further reduced.

Description

Technical field [0001] The invention relates to the field of nitrogen-doped graphene technology, in particular to a method for preparing nitrogen-doped graphene with high nitrogen content. Background technique [0002] Due to its unique two-dimensional monolayer structure and excellent physical properties (high theoretical specific surface area, high electrical conductivity, high mechanical properties, etc.), graphene has received extensive attention from various fields since it was prepared in 2004. Its appearance has a huge impact on the material field, and it also brings great opportunities and challenges to material researchers. I believe that it will bring a revolution in the material field in the next few years, and it will also bring people’s lives. Brings many products with excellent performance. Due to its monolayer, graphene has a theoretical capacity of 2630 m2 / g, which has a wide range of application prospects in lithium ion batteries and supercapacitor electrode mat...

Claims

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Application Information

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IPC IPC(8): C01B31/04
Inventor 宋宏芳赵东辉戴涛周鹏伟
Owner FUJIAN XFH NEW ENERGY MATERIALS CO LTD
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