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Preparation method of graphene sulfide

A technology of sulfided graphene and graphene, applied in chemical instruments and methods, inorganic chemistry, carbon compounds, etc., can solve the problems of harsh equipment requirements, unfavorable large-scale production, long reaction time, etc., and achieve excellent anti-wear reduction. The effect of friction

Active Publication Date: 2019-03-19
中国人民解放军空军勤务学院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, MUllen et al. reported a method for preparing graphene sulfide and graphene nitride on a porous plate, specifically using hydrogen sulfide gas as a reducing agent and a sulfur source to reduce graphene oxide at high temperature, but this method requires the use of hydrogen sulfide gas It is toxic and corrosive, takes a long time to react, and requires harsh equipment, so it is not conducive to large-scale production

Method used

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  • Preparation method of graphene sulfide
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  • Preparation method of graphene sulfide

Examples

Experimental program
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Effect test

Embodiment 1

[0025] 1. Oxidation of graphene

[0026] (1) Take 1 g of 50-mesh graphene powder in a flask, add 46 ml of concentrated sulfuric acid (98%H 2 SO 4 ) and 0.5 g sodium nitrate (NaNO 3 ), at 35 o Stir for 2min under heating condition in C water bath;

[0027] (2) Stir the mixture in an ice bath for 15 min to lower the temperature to 0 o C;

[0028] (3) Add 3 g potassium permanganate (KMnO 4 ), the temperature is controlled at 20 o React in C for 5 minutes, after the reaction is stable, at 35 o C water bath heating condition was stirred for 24 h, and the graphene oxide product was obtained after centrifugation and filtration.

[0029] 2. Vulcanization of graphene oxide

[0030] (1) Take 100 mg of graphene oxide and graphene in 100 ml DMF, and ultrasonically treat it for 1 h to make it uniformly dispersed;

[0031] (2) Centrifuge at 1000 rpm for 10 min to remove precipitated impurities;

[0032] (3) Put it in the flask again, add 300 mg of P with a mass fraction of 99% 4...

Embodiment 2

[0037] 1. Oxidation of graphene

[0038] (1) Take 1 g of 50-mesh graphene powder in a flask, add 46 ml of concentrated sulfuric acid (98%H 2 SO 4 ) and 0.5 g sodium nitrate (NaNO 3 ), at 35 o Stir for 2min under heating condition in C water bath;

[0039] (2) Stir the mixture in an ice bath for 15 min to lower the temperature to 0 o C;

[0040] (3) Add 3 g potassium permanganate (KMnO 4 ), the temperature is controlled at 20 o React in C for 5 minutes, after the reaction is stable, at 35 o C water bath heating condition was stirred for 24 h, and the graphene oxide product was obtained after centrifugation and filtration.

[0041] 2. Vulcanization of graphene oxide

[0042] (1) Take 100 mg of graphene oxide and graphene in 100 ml DMF, and ultrasonically treat it for 1 h to make it uniformly dispersed;

[0043] (2) Centrifuge at 1000 rpm for 10 min to remove precipitated impurities;

[0044] (3) Put it in the flask again, add 300 mg of P with a mass fraction of 99% 4...

Embodiment 3

[0048] 1. Oxidation of graphene

[0049] (1) Take 1 g of 325-mesh graphene powder in a flask, add 46 ml of concentrated sulfuric acid (98%H 2 SO4 ) and 0.5 g sodium nitrate (NaNO 3 ), at 35 o Stir for 2min under heating condition in C water bath;

[0050] (2) Stir the mixture in an ice bath for 15 min to lower the temperature to 0 o C;

[0051] (3) Add 3 g potassium permanganate (KMnO 4 ), the temperature is controlled at 20 o React in C for 5 minutes, after the reaction is stable, at 35 o C water bath heating condition was stirred for 24 h, and the graphene oxide product was obtained after centrifugation and filtration.

[0052] 2. Vulcanization of graphene oxide

[0053] (1) Take 100 mg of graphene oxide and graphene in 100 ml DMF, and ultrasonically treat it for 1 h to make it uniformly dispersed;

[0054] (2) Centrifuge at 1000 rpm for 10 min to remove precipitated impurities;

[0055] (3) Put it in the flask again, add 300 mg of P with a mass fraction of 99% 4 ...

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Abstract

The invention relates to graphene sulfide as well as a preparation method and application thereof. The preparation method comprises the following steps: oxidizing graphene by using potassium permanganate and concentrated sulfuric acid, and then vulcanizing the oxidized graphene by using P4S10, thereby preparing the graphene sulfide. In addition, the dispersion performance and absorption performance of the graphene sulfide in lubricating oil basic oil are also researched, the tribological performance of a graphene reaction lubricating membrane is tested, and the lubricating mechanism is researched. The result shows that the dispersion performance of the graphene can be improved by virtue of vulcanization, and the wear-resisting and friction reducing effect of the graphene can be improved.

Description

technical field [0001] The invention relates to a preparation method of sulfide graphene, belonging to the field of sulfide graphene preparation. Background technique [0002] Graphene is a two-dimensional crystalline material in which carbon atoms form a hexagonal network structure with sp2 hybrid orbitals. Basic research on tribological properties has confirmed that graphene has excellent lubricating properties. Utilizing the interaction between the active sulfur in graphene sulfide and the surface of the iron-based friction pair, the graphene sulfide generates a strong interfacial force through chemical adsorption or reaction with the surface of the iron-based friction pair, so that the graphene is anchored on the surface of the friction pair , In theory, good anti-wear and anti-friction effects can be obtained. At present, there are many reports on graphene sulfide, but few studies on its tribological properties. The reported preparation methods include the use of dibe...

Claims

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Application Information

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IPC IPC(8): C10M125/02C10N60/04C10N60/10C10N60/12C01B32/194
CPCC10M125/02C10N2060/04C10N2060/10C10N2060/12C01B32/194
Inventor 马军姜旭峰胡建强胡役琴费逸伟董仕宝陈利安翟新业
Owner 中国人民解放军空军勤务学院
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