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Preparation method of synthesizing multiple-active site nitrogen-doped graphene with laser irradiation

A technology of nitrogen-doped graphene and laser irradiation, applied in chemical instruments and methods, carbon compounds, inorganic chemistry, etc., can solve the problem of inability to synthesize nitrogen-doped graphene with high catalytic activity and effectively control nitrogen-doped graphite Improve catalytic activity, convenient operation, and easy control

Inactive Publication Date: 2017-07-14
TIANJIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to solve the problems existing in the prior art, the present invention provides a preparation method for synthesizing multi-active-site nitrogen-doped graphene by laser irradiation, which overcomes the fact that the synthesis process in the prior art cannot synthesize graphene with high-efficiency catalytic activity at low temperature and low pressure. Nitrogen-doped graphene and the problem of ineffective control of pyridinic nitrogen content in nitrogen-doped graphene

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  • Preparation method of synthesizing multiple-active site nitrogen-doped graphene with laser irradiation
  • Preparation method of synthesizing multiple-active site nitrogen-doped graphene with laser irradiation
  • Preparation method of synthesizing multiple-active site nitrogen-doped graphene with laser irradiation

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Embodiment 1

[0023] A preparation method for synthesizing multi-active-site nitrogen-doped graphene by laser irradiation, comprising the following steps:

[0024] (1) Using graphene oxide prepared by the improved Hummers method as a raw material, 10 mg of graphene oxide was dissolved in 20 ml of ethanol solution (analytically pure), crushed under the condition of 400w power crushing for five minutes, and then ultrasonically oscillated for 10 minutes.

[0025] (2) Put 20 ml of the sample obtained in step (1) into a conical flask, and irradiate the solution with a nanosecond parallel pulse laser for 10 minutes.

[0026] (3) The sample obtained in step (2) was centrifuged at high speed (16000 rpm) for 25 min to obtain a precipitate and freeze-dried.

[0027] (4) Dissolve 10 mg of the sample obtained in step (3) in 30 ml of water and add 100 mg of ammonium bicarbonate, pour the mixed solution into a 40 ml reaction kettle, and react at a temperature of 90° C. for 12 hours.

[0028] (5) The sam...

Embodiment 2

[0030] A preparation method for synthesizing multi-active-site nitrogen-doped graphene by laser irradiation, comprising the following steps:

[0031] (1) Using graphene oxide prepared by the improved Hummers method as a raw material, 60 mg of graphene oxide was dissolved in 180 ml of ethanol solution (analytical pure), crushed for 40 minutes under the condition of 300w power crushing, and then ultrasonically oscillated for 20 minutes .

[0032] (2) Put 30 ml of the sample obtained in step (1) into a conical flask, and irradiate the solution with a nanosecond parallel pulse laser for 30 minutes.

[0033] (3) The sample obtained in step (2) was centrifuged at high speed (20,000 rpm) for 30 min to obtain a precipitate and freeze-dried.

[0034] (4) 15 mg of the sample obtained in step (3) was dissolved in 30 ml of water and 75 mg of ammonium bicarbonate was added, the mixed solution was poured into a 40 ml reactor, and reacted at a temperature of 150° C. for 12 hours.

[0035] ...

Embodiment 3

[0037] A preparation method for synthesizing multi-active-site nitrogen-doped graphene by laser irradiation, comprising the following steps:

[0038] (1) Using graphene oxide prepared by the improved Hummers method as a raw material, dissolve 30 mg of graphene oxide in 300 ml of ethanol solution (analytically pure), crush it for 20 minutes under the condition of 450w power crushing, and then ultrasonically shake for 40 minutes .

[0039] (2) Put 40 ml of the sample obtained in step (1) into a conical flask, and irradiate the solution with nanosecond parallel pulse laser for 40 min.

[0040] (3) The sample obtained in step (2) was centrifuged at high speed (18000 rpm) for 35 min to obtain a precipitate and freeze-dried.

[0041] (4) Dissolve 20 mg of the sample obtained in step (3) in 80 ml of water and add 1 g of ammonium bicarbonate, pour the mixed solution into a 100 ml reaction kettle, and react at a temperature of 200° C. for 16 hours.

[0042] (5) The sample obtained in s...

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Abstract

The invention discloses a preparation method of synthesizing multiple-active site nitrogen-doped graphene with laser irradiation. Through nano-second laser for irradiating a solution, a graphene oxide raw material with more edge active sites exposed can be produced, wherein the exposed edge active sites on the raw material can be regulated by means of laser energy and irradiation time, so that in the later period of hydrothermally synthesizing the nitrogen-doped graphene, more controllable pyridine nitrogen can be formed, thus improving catalytic activity of the nitrogen-doped graphene. In the invention, for the first time, a method of controllably increasing the content of pyridine nitrogen in the nitrogen-doped graphene is disclosed, wherein high-active nitrogen-doped graphene is synthesized in a water phase under a gentle environment. In addition, the preparation method is simple, is convenient to operate and is easy to control, is free of toxic reaction raw materials and is an environment-friendly green synthesis technology.

Description

technical field [0001] The invention relates to a method for preparing nitrogen-doped graphene, in particular to a method for preparing nitrogen-doped graphene with multiple active sites synthesized by laser irradiation. Background technique [0002] At present, the energy crisis and environmental problems caused by fossil fuels are becoming more and more serious, and people are paying more and more attention to the development and utilization of renewable energy. The key technologies for the conversion and storage of renewable energy include fuel cells, rechargeable metal-air batteries, photolysis of water, etc., and the core issue is to find efficient and cheap catalysts for oxygen reduction reaction (ORR) and oxygen evolution reaction (OER). , to replace expensive and scarce precious metals (Pt, Pt alloys) and their oxides (IrO 2 , RuO 2 ), which is of great significance to promote the commercialization process of renewable energy utilization technology. Based on earth...

Claims

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Application Information

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IPC IPC(8): C01B32/194C01B32/198B01J27/24
CPCB01J27/24C01P2002/72C01P2002/82C01P2004/04C01P2006/40
Inventor 杨静王学瑞杜希文毛晶
Owner TIANJIN UNIV
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