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A kind of method for preparing high nitrogen-doped nitrogen-doped graphene

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

Active Publication Date: 2016-01-27
FUJIAN XFH NEW ENERGY MATERIALS CO LTD
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  • Summary
  • 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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  • A kind of method for preparing high nitrogen-doped nitrogen-doped graphene

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Effect test

Embodiment 1

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

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

[0024] (3) Microwave heating: move mixture A to a high-pressure reactor with a pressure of 50MPa, then place the reactor in a microwave oven with a power of 2000w, and heat for 600s to obtain mixture B.

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

Embodiment 2

[0027] (1) Dispersion of graphene: Prepare a graphene dispersion liquid with a concentration of 2.0 mg / mL, the dispersant is bilayer graphene, and the dispersant is dehydrated alcohol.

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

[0029] (3) Microwave heating: move mixture A to a high-pressure reactor with a pressure of 1 MPa, then place the reactor in a microwave oven with a power of 1500w, and heat for 10 seconds to obtain mixture B.

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

Embodiment 3

[0032] (1) Dispersion of graphene: Prepare a graphene dispersion liquid 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 nitrogen source were mixed at a certain mass ratio of 1:10, and after ultrasonic treatment for 0.8 h, a mixture A was obtained, and the nitrogen source was melamine and dopamine.

[0034] (3) Microwave heating: move mixture A to a high-pressure reactor with a pressure of 5 MPa, then place the reactor in a microwave oven with a power of 600w, and heat for 600s to obtain mixture B.

[0035] (4) Filtration and drying: The mixture B was filtered through a 0.2 μm PTFE membrane filter, and the obtained filter cake was dried at a temperature of 100°C for 80 minutes to obtain nitrogen-doped graphene, and 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 technology in the field of nitrogen-doped graphene, in particular to a method for preparing nitrogen-doped graphene with a high nitrogen doping amount. 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 had a huge impact on the field of materials, and at the same time it has brought great opportunities and challenges to materials researchers. I believe that in the next few years it will bring a revolution to the field of materials and people's lives Bring many products with excellent performance. Graphene has a theoretical capacity of up to 2630m2 / g due to its single molecular layer. It has broad application prospects in lithium-ion batteries ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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