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Preparation and application of nitrogen, sulphur or chlorine-doped three-dimensional porous graphene catalyst

A three-dimensional porous and graphene technology, applied in electrical components, battery electrodes, circuits, etc., can solve the problems of rare research reports on doped graphene, achieve the effect of overcoming corrosion problems, simple operation, and improving stability

Inactive Publication Date: 2016-06-15
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the research reports on S and Cl doped graphene are rare

Method used

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  • Preparation and application of nitrogen, sulphur or chlorine-doped three-dimensional porous graphene catalyst
  • Preparation and application of nitrogen, sulphur or chlorine-doped three-dimensional porous graphene catalyst
  • Preparation and application of nitrogen, sulphur or chlorine-doped three-dimensional porous graphene catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] A preparation method of nitrogen-doped three-dimensional porous graphene catalyst, the specific steps are:

[0044] (1) Weigh 100 mg of graphene oxide and dissolve it in 100 mL of absolute ethanol, sonicate for 1 hour to obtain a uniform graphene oxide suspension, add 3 mL of 3-aminopropyltriethoxysilane dropwise while stirring slowly, and then Slowly add 0.5mL of hydrochloric acid with a concentration of 2M, then slowly add 10mL of anhydrous ethanol solution in which 400mg of ferrous chloride tetrahydrate is dissolved, and react the above mixed solution in a water bath for 6 hours (the temperature of the water bath is 60°C). Dry it in an oven at 85°C overnight, and grind it into powder to obtain a catalyst precursor.

[0045] (2) Place the above precursor in a quartz boat, under N 2 Under the protection of the atmosphere, the temperature was raised to 900°C at a rate of 5°C / min and the reduction treatment was carried out for 1 hour to obtain a primary carbonized produ...

Embodiment 2

[0047] A preparation method of a sulfur-doped three-dimensional porous graphene catalyst, the specific steps are:

[0048] (1) Weigh 100mg of graphene oxide (GO) and dissolve it in 100mL of absolute ethanol, sonicate for 1 hour to obtain a uniform graphene oxide suspension, add 3mL of mercaptopropyltrimethoxysilane dropwise while stirring slowly, Then slowly add 0.5mL of hydrochloric acid with a concentration of 2M, and then slowly add 10mL of anhydrous ethanol solution dissolved with 400mg of ferrous chloride tetrahydrate, and react the above mixed solution in a water bath for 6 hours (the temperature of the water bath is 60°C). Dry it overnight in an oven at 85°C, and grind it into powder to obtain a catalyst precursor.

[0049] (2) Place the above precursor in a quartz boat, under N 2 Under the protection of the atmosphere, the temperature was raised to 900°C at a rate of 5°C / min and the reduction treatment was carried out for 1 hour to obtain a primary carbonized product....

Embodiment 3

[0051] A preparation method of chlorine-doped three-dimensional porous graphene catalyst, the specific steps are:

[0052] (1) Weigh 100mg of graphene oxide (GO) and dissolve it in 100mL of absolute ethanol, sonicate for 1 hour to obtain a uniform graphene oxide suspension, add 3mL of 3-chloropropyltrimethoxysilane dropwise while stirring slowly , then slowly drop 0.5mL of hydrochloric acid with a concentration of 2M, then slowly add 10mL of anhydrous ethanol solution that is dissolved with 400mg of ferrous chloride tetrahydrate, and react the above mixed solution in a water bath for 6 hours (the temperature of the water bath is 60°C) Afterwards, it was dried overnight in an oven at 85° C., and ground into powder to obtain a catalyst precursor.

[0053] (2) Place the above precursor in a quartz boat, under N 2 Under the protection of the atmosphere, the temperature was raised to 900°C at a rate of 5°C / min and the reduction treatment was carried out for 1 hour to obtain a prim...

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Abstract

The invention provides a preparation and an application of a nitrogen, sulphur or chlorine-doped three-dimensional porous graphene catalyst. The preparation comprises the following steps: dissolving graphene oxide, an alkyl compound, a transition metal salt containing nitrogen, sulphur or chlorine and hydrochloric acid into a solvent, and carrying out ultrasonic treatment and drying to obtain a precursor; heating the precursor to 600-1,000 DEG C under inert gas protection and carrying out roasting reduction treatment for 1-3 hours to obtain primary carbide; carrying out pickling treatment on the obtained primary carbide with a mixed solution of hydrofluoric acid and hydrochloric acid at a room temperature for 12-24 hours, centrifuging the primary carbide, cleaning the primary carbide with deionized water and then drying the primary carbide to obtain the three-dimensional porous graphene material containing nitrogen, sulphur or chlorine; and heating the three-dimensional porous graphene material to 600-1,000 DEG C under inert gas protection, and carrying out roasting reduction treatment for 1-3 hours to obtain the nitrogen, sulphur or chlorine-doped three-dimensional porous graphene catalyst. The nitrogen, sulphur or chlorine-doped three-dimensional porous graphene catalyst has the characteristics of being high in stability, not easy to poison and the like, and has a good application prospect in the fields of wastewater treatment of a fuel cell, a metal-air cell, a super capacitor, an energy storage battery and a microbial fuel cell and the like.

Description

technical field [0001] The invention belongs to the field of graphene-based catalysts and their preparation and application, in particular to a nitrogen (sulfur, chlorine) doped three-dimensional porous graphene catalyst and a non-template method preparation method and application thereof. Background technique [0002] In recent years, as the consumption of fossil fuels is increasing year by year, the energy crisis and environmental pollution problems are becoming more and more serious, it is particularly urgent to develop efficient, green and environmentally friendly energy storage and conversion technologies. Fuel cell - an electrochemical device that directly and continuously converts the chemical energy in fuel and oxidant into electrical energy. Since it is not limited by the Carnot cycle, the energy conversion rate is two to three times that of the internal combustion engine. Not only that, the fuel cell has the advantages of low maintenance cost, clean working environ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/90H01M4/88H01M4/96
CPCH01M4/88H01M4/90H01M4/9091H01M4/96Y02E60/50
Inventor 乔锦丽唐胜周学俊徐能能
Owner DONGHUA UNIV
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