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Boron-nitrogen co-doped porous graphene as well as preparation method and application thereof

A porous graphene, co-doping technology, applied in the preparation/separation of ammonia, chemical instruments and methods, inorganic chemistry, etc., can solve problems such as low preparation efficiency, harsh pore-making conditions, and environmental pollution

Inactive Publication Date: 2019-12-06
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Conventional graphene pore-forming conditions are harsh (high temperature, high pressure, catalyst) and often involve strong oxidants (HNO 3 and KMnO 4 ), the subsequent treatment is still high temperature annealing or reducing agent (N 2 h 4 、H 2 , NH 3 , NaBH 4 etc.), the preparation efficiency is low, and it causes serious pollution to the environment

Method used

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  • Boron-nitrogen co-doped porous graphene as well as preparation method and application thereof
  • Boron-nitrogen co-doped porous graphene as well as preparation method and application thereof
  • Boron-nitrogen co-doped porous graphene as well as preparation method and application thereof

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Embodiment 1

[0057] A preparation method of boron-nitrogen co-doped porous graphene catalyst, comprising the steps of:

[0058] (1) Place the quartz boat with 100 mg of graphene in the heating zone of the tube furnace, heat the steam generator to 150°C, turn on the pure water peristaltic pump, and feed water vapor and argon, the flow rate of water vapor is 0.05 mL / min, the flow rate of argon gas is 50mL / min, heat treatment is carried out by raising the temperature, the heating rate is 20 ℃ / min, the temperature of heat treatment is 800 ℃, and the time of heat treatment is 1 h. During this process, water vapor Accompanied by the Ar atmosphere entering the heating zone of the tube furnace, it reacts with graphene to produce in-plane nanopores. At the same time, water vapor has weak oxidizing properties, and can functionalize the edges of the pores to obtain porous graphene. The porous graphene The pore size is 8.9 nm;

[0059] (2) in NH 3 In a mixed atmosphere with Ar, the porous graphene (...

Embodiment 2

[0071] A preparation method of boron-nitrogen co-doped porous graphene catalyst, comprising the steps of:

[0072] (1) Place the quartz boat with 100 mg of graphene in the heating zone of the tube furnace, heat the steam generator to 150°C, turn on the pure water peristaltic pump, and feed water vapor and argon, the flow rate of water vapor is 0.015 mL / min, the flow rate of argon gas is 50 mL / min, heat treatment is carried out by raising the temperature, the heating rate is 5 ℃ / min, the temperature of heat treatment is 800 ℃, and the time of heat treatment is 1 h. Steam enters the heating zone of the tube furnace with the Ar atmosphere to react with graphene to generate in-plane nanopores. At the same time, water vapor has weak oxidizing properties and can functionalize the edges of the pores to obtain porous graphene. The porous graphene The average pore diameter is 8.1 nm;

[0073] (2) in NH 3 In a mixed atmosphere with Ar, the porous graphene (50 mg) described in step (1)...

Embodiment 3

[0085] A preparation method of boron-nitrogen co-doped porous graphene, comprising the steps of:

[0086] (1) Place the quartz boat with 100 mg of graphene in the heating zone of the tube furnace, heat the steam generator to 150°C, turn on the pure water peristaltic pump, and feed water vapor and argon, the flow rate of water vapor is 0.05 mL / min, the flow rate of argon gas is 50 mL / min, heat treatment is carried out by raising the temperature, the heating rate is 5 ℃ / min, the temperature of heat treatment is 800 ℃, and the time of heat treatment is 1 h. During this process, water vapor Accompanied by the Ar atmosphere entering the heating zone of the tube furnace, it reacts with graphene to produce in-plane nanopores. At the same time, water vapor has weak oxidizing properties, and can functionalize the edges of the pores to obtain porous graphene. The porous graphene The average pore size is 9.3 nm;

[0087] (2) in NH 3 In a mixed atmosphere with Ar, the porous graphene (5...

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Abstract

The invention discloses boron-nitrogen co-doped porous graphene as well as a preparation method and an application thereof. The method comprises the following steps of placing graphene in a reaction container, introducing water vapor and argon, and carrying out heating to perform heating treatment to obtain porous graphene; heating the porous graphene in a mixed atmosphere of NH3 and Ar to carry out nitrogen doping treatment to obtain nitrogen-doped porous graphene; and putting the nitrogen-doped porous graphene and boric acid into the reaction container, and heating in a protective atmospherefor boron doping treatment to obtain a boron-nitrogen co-doped porous graphene catalyst. According to the method, water vapor is used as a weak oxidizing agent, so that pore size regulation and large-scale preparation of the porous graphene are realized. The boron-nitrogen co-doped porous graphene catalyst provided by the invention shows excellent catalytic efficiency and catalytic stability, andhas a wide application prospect in the field of nitrogen catalytic reduction.

Description

technical field [0001] The invention belongs to the technical field of ammonia synthesis by electrochemical catalytic nitrogen reduction, and in particular relates to a boron-nitrogen co-doped porous graphene and its preparation method and application. Background technique [0002] Ammonia is not only a necessary chemical raw material for the synthesis of explosives, fertilizers, resins and other chemicals, but also an efficient and clean non-carbon energy carrier. At present, the industry mainly uses hydrogen and nitrogen as raw materials, and uses the Hubble method to synthesize ammonia under the conditions of high temperature (400-500 ℃), high pressure (150-300 atm), and catalyst (Ru or Fe). The process conditions are harsh and the yield Less than 20%, about 1% of the world's energy is used for ammonia production every year. The latest research shows that nitrogen (photo) electrochemical reduction ammonia has the advantages of mild reaction conditions (normal temperature...

Claims

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Application Information

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IPC IPC(8): C01B32/194C01C1/04B01J27/24
CPCC01B32/194C01C1/0411B01J27/24B01J35/33Y02P20/52
Inventor 徐建铁张加奎肖峰陈香宏胡彤谢佩燃
Owner SOUTH CHINA UNIV OF TECH
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