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Nitrogen-doped graphene, Pd-loaded nitrogen-doped graphene catalyst and preparation method and application thereof

A graphene and catalyst technology, applied in aza-graphene catalyst and preparation thereof, in the field of aza-graphene, can solve problems such as expensive price, restricting large-scale practical application, harsh preparation conditions, etc., achieving easy content, mild conditions, Easy to wash effect

Inactive Publication Date: 2015-10-28
HUBEI UNIV
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  • Description
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Problems solved by technology

[0004] In recent years, a variety of methods can be used to prepare various new nitrogen-doped graphene, such as organic pyrolysis, high-voltage arc method, laser lift-off method or chemical vapor deposition method, etc., but harsh preparation conditions and expensive prices restrict its Large-scale practical application

Method used

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  • Nitrogen-doped graphene, Pd-loaded nitrogen-doped graphene catalyst and preparation method and application thereof
  • Nitrogen-doped graphene, Pd-loaded nitrogen-doped graphene catalyst and preparation method and application thereof
  • Nitrogen-doped graphene, Pd-loaded nitrogen-doped graphene catalyst and preparation method and application thereof

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preparation example Construction

[0022] The present invention provides a kind of preparation method of azagraphene, comprises the following steps;

[0023] (1), GO is added to a certain amount of water, and treated in an ultrasonic generator for 1-3h; the mass volume ratio of the GO to water is (10-90)mg:(10-80)mL;

[0024] (2), then transferred to the reaction kettle, stirred and reacted at 150-200°C for 5-24h;

[0025] (3) Vacuum drying at 30-60° C. for 12-24 hours after suction filtration and washing to obtain sample RGO.

[0026] Further, the preparation method of azagraphene as described above also needs to add urea in step 1, specifically:

[0027] Treat GO with a certain amount of urea and water in an ultrasonic generator for 1-3 hours, and finally get the sample NRGO -x , the mass volume ratio of GO, urea, and water is: A mg:B g:C mL, wherein, 10≤A≤90, 0<B≤27, 10≤C≤80, and x represents urea and oxidation Graphene mass ratio, 0<X<300.

[0028] Further, the preparation method of azagraphene as descr...

Embodiment 1

[0035] Preparation of Graphene Oxide (GO)

[0036] 1) Add an appropriate amount of 98% concentrated sulfuric acid into a 500mL beaker, and control the temperature to 0°C.

[0037] 2) Add 10g of graphite powder and 5g of sodium nitrate, and stir for 1h.

[0038] 3) Add 30 g of potassium permanganate powder under vigorous stirring (the addition speed should be well controlled, and it is best not to make the temperature exceed 20° C.).

[0039] 4) Remove the low-temperature ice bath, and stir in a water bath at 35°C for 30 min.

[0040] 5) Add 460mL of deionized water under stirring, raise the temperature of the reaction solution to about 98°C, and continue stirring for 1h.

[0041] 6) Dilute the reaction solution with 1.4L deionized warm water, and then add a certain amount of 3% hydrogen peroxide solution.

[0042] 7) Filtrate while it is hot, and fully wash the filter cake with a pre-prepared 5% hydrochloric acid aqueous solution (warm) until there is no sulfate ion in the ...

Embodiment 2

[0045] Preparation process of nitrogen-doped graphene

[0046] (1) GO (containing about 81 mg C) and a certain amount of urea were added to 70 mL of water, and treated in an ultrasonic generator (200 W) for 3 h.

[0047] (2) Then transfer to a 100mL reactor and stir the reaction at 180°C for 10h.

[0048] (3) Vacuum-dry at 30° C. for 12 hours after suction filtration and washing. Label this sample as NRGO -x(x represents the weight ratio of urea and GO = 10, 75, 150, 300, etc.), adjusting the value of x can produce azagraphene with different nitrogen contents.

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Abstract

The invention provides nitrogen-doped graphene, a Pd-loaded nitrogen-doped graphene catalyst and its preparation method and application. The preparation method of the Pd-loaded nitrogen-doped graphene catalyst comprises the following steps: mixing graphene oxide, urea and water, and conducting ultrasonic treatment for 3h; transferring the mixture into a reaction vessel and stirring at 180 DEG C to react for 10 h; conducting suction filtration, washing and drying to obtain NRGO-x; mixing NRGO-x, a palladium chloride solution and water, and conducting ultrasonic treatment for 1 h; pouring the mixture into a reaction vessel, heating to 40 DEG C, and stirring at 2MPaH2 to react for 8 h; and conducting suction filtration after the reaction, washing, and conducting vacuum drying at 60 DEG C for 12 h, so as to obtain Pd / NRGO-x. In comparison with a traditional carbon material-loaded Pd catalyst, the nitrogen-doped graphene-loaded Pd catalyst has higher catalytic activity and stability. High temperature and high pressure are avoided by a method for preparing the nitrogen-doped graphene, and content of nitrogen is easy to adjust.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to azagraphene, a Pd-loaded azagraphene catalyst, a preparation method and an application thereof. Background technique [0002] Recently, a new type of single-atom-thick carbon nanosheets—graphene—has been the focus of intense research. From the current research, it is found that graphene not only has a larger theoretical specific surface area than activated carbon and carbon nanotubes (up to 2630m 2 / g), and has better electrical and thermal conductivity properties. At the same time, since the upper and lower layers of the graphene nanosheet are easily exposed, it has a high specific surface area utilization efficiency. In addition, there are many oxygen-containing groups and defects such as carbon or oxygen on the surface of graphene. This will bring many chemically active sites, or serve as anchor sites for metal particles. However, compared with carbon nanotubes, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/18B01J23/44B01J27/24B01J35/10C07B37/00C07C15/14C07C1/32
Inventor 聂仁峰江和展鲁新环周丹夏清华
Owner HUBEI UNIV
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