Method for preparing graphene simultaneously doped with nitrogen and sulfur through biological reduction

A graphene and biological technology, which is applied in the field of graphene reduction based on sulfate-reducing bacteria, and achieves the effects of wide distribution, broad application prospects and low cost.

Active Publication Date: 2013-08-21
HUAZHONG UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, since the organism itself has various trace elements such as nitrogen and phosphorus, there may be more surprises in the element doping of graphene

Method used

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  • Method for preparing graphene simultaneously doped with nitrogen and sulfur through biological reduction
  • Method for preparing graphene simultaneously doped with nitrogen and sulfur through biological reduction
  • Method for preparing graphene simultaneously doped with nitrogen and sulfur through biological reduction

Examples

Experimental program
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Effect test

Embodiment 1

[0027] The preparation of embodiment 1 graphene oxide

[0028] Mix 1.5g of natural flake graphite powder with 1.5g of sodium nitrate and 69ml of concentrated sulfuric acid in an ice bath. Slowly add 9g of potassium permanganate, and stir the reaction for 1h in a normal temperature water bath. Gradually add 100ml of deionized water, the temperature is gradually increased, stirring at 90 ° C to continue the reaction for 30min, the mixture turns from brown to bright yellow, add 10ml, 30% hydrogen peroxide solution, the mixture turns from brown to bright yellow. Filtrate while hot, and fully wash with hydrochloric acid solution and deionized water until the filtrate is pH=6. The graphene oxide filter cake was fully dried in a vacuum oven at 80°C and stored for future use.

Embodiment 2

[0029] The activation of embodiment 2 SRB bacterial classification

[0030] Take out the SRB strains stored in the refrigerator, place them in a constant temperature incubator at a suitable temperature and incubate them for 2 to 3 hours, pipette an appropriate amount of strains into a sterilized bottle, and fill the entire bottle with the sterilized medium. Close the stopper to ensure that there is no air in the bottle. Place the culture solution inoculated with SRB in a constant temperature incubator and cultivate it for 24 hours. If the solution in the bottle turns black, it means that the cultured SRB has considerable activity. If it does not turn black, follow the above steps to re-inoculate until the solution in the bottle turns black. If the solution in the bottle does not turn black after three inoculations, it means that the strain has been inactivated and needs to be replaced.

Embodiment 3

[0031] Example 3 Graphene modified electrode detects heavy metal ions

[0032] (1) Graphene oxide is prepared by the Hummers method. Graphene oxide was dispersed in water and ultrasonically dispersed to prepare a 0.1 mg / ml dispersion.

[0033] (2) The composition of SRB medium is as follows: sodium lactate 4.0ml; yeast infusion 1.0g; magnesium sulfate heptahydrate 0.2g; dipotassium hydrogen phosphate 0.01g; sodium chloride 10g; distilled water 1000ml. Use sodium hydroxide to adjust the pH to 7.0-7.2, at 0.12×10 5 Under high-pressure steam of Pa, sterilize for 20 minutes, rapidly cool to about 37°C, and store at a constant temperature for later use.

[0034] (3) The SRB strain came from the sewage of Shengli Oilfield in my country. After activation according to the method of Application Example 2, it is ready for use.

[0035] (4) Get 100ml of graphene oxide solution with a concentration of 0.1mg / ml, 20ml of diluted cultured SRB bacterial solution with considerable activity...

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Abstract

The invention provides a method for preparing graphene simultaneously doped with nitrogen and sulfur through biological reduction, and belongs to the technical fields of graphene synthesis and a nano material. The method is characterized in that oxidized graphene dispersion solution is used as a raw material, sulfate-containing reduction bacteria suspension is used as a biological reduction agent, the raw material is reacted with the biological reduction agent for 5 to 10 days in a control reaction system under an air insulation condition to obtain a graphene solution, and the graphene solution is centrifugally filtered and repeatedly washed to obtain graphene doped with nitrogen and sulfur. According to the method, no stabilizer or dispersing agent is added, and oxidized graphene is reduced by utilizing the metabolic activity of the microorganisms to obtain graphene doped with nitrogen and sulfur, so that the method has the advantages of safety, no toxicity, simplicity in operation, environmental friendliness and the like, the difficulty that nitrogen and sulfur cannot be simultaneously doped in the existing graphene preparation method can be solved, when graphene simultaneously doped with the nitrogen and sulfur is applied to the fields such as electrochemical sensors, electric catalysis and the like, the detection limit and the detection sensitivity can be remarkably improved, and the application prospect is promising.

Description

technical field [0001] The invention relates to a method for preparing graphene simultaneously doped with nitrogen and sulfur, and belongs to the technical field of graphene synthesis and nanomaterials, in particular to a method for preparing graphene based on sulfate-reducing bacteria (SRB) reduction. Background technique [0002] Graphene is a unique two-dimensional planar structure single-layer carbon nanomaterial, and the carbon atoms are connected by covalent bonds to form a hexagonal honeycomb structure. This unique structural feature of graphene makes it have good electrical, mechanical and thermal properties. In recent years, it has broad application prospects in microelectronics, new superconducting materials, energy storage, sensors and electrocatalysis. At the same time, basic and applied research on graphene is also in full swing around the world. [0003] The research on the preparation method of graphene is the premise of its basic and applied research. The c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C12P3/00
Inventor 刘宏芳郭佩佩秦双王帅
Owner HUAZHONG UNIV OF SCI & TECH
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