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Preparation method of mesoporous nitrogen-doped graphene-loaded molybdenum disulfide synthesized by laser irradiation and application of mesoporous nitrogen-doped graphene-loaded molybdenum disulfide in electrocatalytic hydrogen production

A nitrogen-doped graphene, laser irradiation technology, applied in chemical instruments and methods, physical/chemical process catalysts, electrodes, etc., can solve problems such as the inability to effectively control the content of carbon pyridine nitrogen metal bonds, and achieve easy control and operation. The effect of convenient and efficient catalytic activity

Active Publication Date: 2019-12-20
TIANJIN UNIV
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Problems solved by technology

[0005] The purpose of the present invention is that the existing synthesis process cannot synthesize transition metal oxide / sulfide composite mesoporous nitrogen-doped graphene rich in carbopyridine nitrogen metal bonds at low temperature and low pressure and cannot effectively regulate the carbopyridine in the composite system The problem of the content of nitrogen-metal bonds was found that laser irradiation of graphene oxide in the range of 177-315mJ can increase the content of carbon-pyridine nitrogen-molybdenum bonds in the composite catalyst, and the raw material laser irradiation of graphene oxide and four When the mass ratio of thiomolybdic acid is 1:1 to 1:8, the loading amount of molybdenum disulfide on mesoporous graphene can be optimized, so that while improving the conductivity of molybdenum disulfide, the carbopyridyl nitrogen molybdenum bond at the interface can also be It can synergistically enhance its intrinsic activity and promote the electrocatalytic process of HER

Method used

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  • Preparation method of mesoporous nitrogen-doped graphene-loaded molybdenum disulfide synthesized by laser irradiation and application of mesoporous nitrogen-doped graphene-loaded molybdenum disulfide in electrocatalytic hydrogen production
  • Preparation method of mesoporous nitrogen-doped graphene-loaded molybdenum disulfide synthesized by laser irradiation and application of mesoporous nitrogen-doped graphene-loaded molybdenum disulfide in electrocatalytic hydrogen production
  • Preparation method of mesoporous nitrogen-doped graphene-loaded molybdenum disulfide synthesized by laser irradiation and application of mesoporous nitrogen-doped graphene-loaded molybdenum disulfide in electrocatalytic hydrogen production

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Experimental program
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Effect test

Embodiment 1

[0036] (1) Put 10 mg of graphene oxide in 30 mL of absolute ethanol (purity is analytically pure), ultrasonically crush to obtain a uniformly dispersed suspension, pour the suspension into a 50 mL Erlenmeyer flask, and control the magnetic stirring speed at 400 rpm, and irradiated with 270mJ nanosecond parallel pulsed laser for 25min in an ice-water bath to obtain graphene oxide after laser irradiation.

[0037] (2) After the graphene oxide after the laser irradiation of the step (1) gained is centrifuged (18000 rpm) for 15 minutes, add deionized water to clean the precipitate, centrifuge at a speed of 18000 rpm for 15 minutes, and then Add deionized water and centrifuge at 18,000 rpm for 15 minutes, repeat the operation until the product smells odorless, and then freeze-dry the product with a lyophilizer.

[0038] (3) Graphene oxide and 20 mg ammonium tetrathiomolybdate after freeze-drying obtained in step (2) are dispersed in 10 mL of N,N-dimethylformamide, then 200 mg of ur...

Embodiment 2

[0043] (1) Put 7.5mg of graphene oxide in 30mL of absolute ethanol (purity is analytically pure), ultrasonically crush to obtain a uniformly dispersed suspension, and ultrasonically crush to obtain a uniformly dispersed suspension, pour the suspension into 50mL The Erlenmeyer flask, the magnetic stirring speed is controlled at 300 rpm, and irradiated with 177mJ nanosecond parallel pulsed laser for 30min in an ice-water bath to obtain graphene oxide after laser irradiation.

[0044] (2) After the graphene oxide after the laser irradiation of the step (1) gained is centrifuged (15000 rpm) for 20 minutes, add deionized water to clean the precipitate, centrifuge at a speed of 15000 rpm for 20 minutes, and then Add deionized water and centrifuge at 15,000 rpm for 20 minutes, repeat the operation until the product smells odorless, and then freeze the product with a lyophilizer.

[0045] (3) Graphene oxide and 15 mg ammonium tetrathiomolybdate after the lyophilized laser irradiation ...

Embodiment 3

[0050] (1) Put 9.5 mg of graphene oxide in 30 mL of absolute ethanol (purity is analytically pure), ultrasonically crush to obtain a uniformly dispersed suspension, ultrasonically to obtain a uniformly dispersed suspension, and ultrasonically to obtain a uniformly dispersed suspension For turbid liquid, pour the suspension into a 50mL Erlenmeyer flask, control the magnetic stirring speed at 400 rpm, and irradiate with 220mJ nanosecond parallel pulsed laser in an ice-water bath for 28min to obtain graphene oxide after laser irradiation.

[0051] (2) After the graphene oxide after the laser irradiation of the step (1) gained is centrifuged (16000 rpm) for 20 minutes, add deionized water to clean the precipitate, centrifuge at a speed of 16000 rpm for 20 minutes, and then Add deionized water and centrifuge at 16,000 rpm for 20 minutes, repeat the operation until the product smells odorless, and then freeze-dry the product with a lyophilizer.

[0052] (3) Graphene oxide and 19 mg ...

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Abstract

The invention relates to a preparation method of mesoporous nitrogen-doped graphene-loaded molybdenum disulfide synthesized by laser irradiation and application of the mesoporous nitrogen-doped graphene-loaded molybdenum disulfide in electrocatalytic hydrogen production. In order to solve the problems that by an existing synthesis process, transition metal oxide / sulfide composite mesoporous nitrogen-doped graphene rich in carbon-pyridine nitrogen metal bonds cannot be synthesized at low temperature and under low pressure, and the content of the carbon-pyridine nitrogen metal bonds in the composite system cannot be regulated and controlled effectively, it is found that the content of the carbon-pyridine nitrogen-molybdenum bonds in the composite catalyst can be improved by irradiating graphene oxide with laser in a range of 177-315 mJ, and in a hydrothermal process, the mass ratio of laser irradiation graphene oxide to tetrathiomolybdic acid as raw materials is 1: 1-1: 8, the loading amount of the molybdenum disulfide on mesoporous graphene can be optimized, thus, while the conductivity of the molybdenum disulfide is improved, the intrinsic activity of the molybdenum disulfide can also be improved synergistically by the carbon-pyridine nitrogen molybdenum bonds at an interface, and the electrocatalysis process of HER is promoted. The preparation method is simple in process, ingenious in design and low in cost, and is safe and environmentally friendly.

Description

technical field [0001] The present invention relates to the hydrothermal synthesis of molybdenum disulfide / mesoporous nitrogen-doped graphene composites using laser-irradiated graphene oxide as a substrate, taking advantage of the increased electrical conductivity and exposed edge sites and interfacially formed carbon-pyridine nitrogen -Mo bonds serve as highly active sites to enhance the performance of electrocatalytic hydrogen production. In particular, it relates to the preparation method of mesoporous nitrogen-doped graphene supported molybdenum disulfide by laser irradiation and its application in electrocatalytic hydrogen production. Background technique [0002] With the increasing consumption of traditional fossil fuels and the severity of environmental degradation, such as: CO 2 Induced greenhouse effect, SO 2 Acid rain pollution and smog caused by excessive PM2.5 have made it imperative for people to develop and utilize new clean energy. Among many clean energy ...

Claims

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Application Information

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IPC IPC(8): B01J27/24C25B1/04C25B11/06
CPCB01J27/24C25B1/04C25B11/091B01J35/33Y02E60/36
Inventor 杨静覃佳艺杜希文
Owner TIANJIN UNIV
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