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Method for preparing sulfonated graphene material

A technology of sulfonated graphene and graphene, which is applied in chemical instruments and methods, inorganic chemistry, carbon compounds, etc., can solve the constraints of large-scale application of graphene functionalization, high toxicity of reducing agent raw material hydrazine hydrate, and pH value control Higher requirements and other issues, to achieve the effect that is conducive to large-scale production, mild conditions, and low requirements for production equipment

Active Publication Date: 2017-02-08
TAIZHOU CITY GANG YANG RUBBER
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of preparing sulfonated graphene at present, the method adopted has higher requirements on the pH value control of the preparation process, the required reaction time is longer, and the reducing agent raw material hydrazine hydrate used in the reduction reaction process is more toxic. The high temperature reaction stage is required in the preparation process, these factors restrict the large-scale application of graphene functionalization

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  • Method for preparing sulfonated graphene material
  • Method for preparing sulfonated graphene material
  • Method for preparing sulfonated graphene material

Examples

Experimental program
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Effect test

Embodiment 1

[0026] A kind of preparation method of sulfonated graphene material, comprises following process:

[0027] 1. Preparation of rGO (reduced graphene oxide)

[0028] (1) Put 0.15 g of graphene oxide into a 250mL beaker and add 75mL of deionized water for 2 hours, and after 2 hours, use NH 3 •H 2 O adjust the pH to 10.0 and continue sonication for 2 hours.

[0029] (2) Set up the reaction device after the ultrasound, pour the dispersion liquid into a four-necked bottle, and add 2 g (NH 4 ) 2 S 2 o 3 Continue to heat to 70° C. and continue stirring at constant temperature for 10 hours.

[0030] (3) Vacuum filtration and washing, followed by washing with 50 mL methanol and 150 mL water, and drying to obtain the reduced graphene oxide powder.

[0031] 2. Diazonium salt configuration experiment plan

[0032] (1) Weigh 3 mmol of p-aminobenzenesulfonic acid, 0.5195 g;

[0033] (2) Measure 6mL (24 mmol) of 4 mol / L hydrochloric acid to dissolve p-aminobenzenesulfonic acid;

[00...

Embodiment 2

[0045] A kind of preparation method of sulfonated graphene material, comprises following process:

[0046] 1. Preparation of rGO

[0047] (1) Put 0.20 g of graphene oxide into a 250 mL beaker and add 200 mL of deionized water for 3 hours, and after 3 hours, use NH 3 •H 2 O adjust the pH to 10.0 and continue sonication for 3 hours.

[0048] (2) Set up the reaction device after the ultrasound, pour the dispersed liquid into a four-necked bottle, add 2.5 g (NH4)2S2O3 when the oil bath is heated and stirred to 30 °C, continue to heat to 80 °C and continue to react at a constant temperature for 12 Hour.

[0049] (3) Vacuum filtration and washing, washing with 50 mL methanol and 150 mL water, and drying to obtain the reduced graphene oxide powder.

[0050] 2. Diazonium salt configuration experiment plan

[0051] (1) Weigh 6 mmol, 1.039 g of p-aminobenzenesulfonic acid;

[0052] (2) Measure 6mL (24 mmol) of 4 mol / L hydrochloric acid to dissolve p-aminobenzenesulfonic acid;

[00...

Embodiment 3

[0065] A kind of preparation method of sulfonated graphene material, comprises following process:

[0066] 1. Preparation of rGO (reduced graphene oxide)

[0067] (1) Put 0.25 g graphene oxide into a 500 mL beaker and add 250 mL deionized water for 3.5 hours to sonicate. After 3.5 hours, use NH 3 •H 2 O adjusted the pH to 11.0 and continued sonication for 3.5 hours.

[0068] (2) Set up the reaction device after the ultrasound, pour the dispersion liquid into a four-neck bottle, and add 3 g (NH 4 ) 2 S 2 o 3 Continue heating to 90° C. and continue stirring at constant temperature for 14 hours.

[0069] (3) Vacuum filtration and washing, followed by washing with 50 mL methanol and 150 mL water, and drying to obtain the reduced graphene oxide powder.

[0070] 2. Diazonium salt configuration experiment plan

[0071] (1) Weigh 9 mmol of p-aminobenzenesulfonic acid, 1.5585 g;

[0072] (2) Measure 6mL (24 mmol) of 4 mol / L hydrochloric acid to dissolve p-aminobenzenesulfonic ...

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Abstract

The invention discloses a method for preparing a sulfonated graphene material. The method comprises the following steps: taking reduced graphene oxide and sulfanilic acid aryl diazo salt as raw materials, and reacting, thereby obtaining the material. Graphene oxide is prepared by adopting an improved Hummers method, and the reduced graphene oxide is prepared by taking environmental-friendly ammonium thiosulfate as a reducing agent. The diazo salt is prepared from sulfanilic acid and is reacted with the reduced graphene oxide so as to prepare the functionalized sulfonated graphene. Only a low-temperature reaction is carried out in the whole experimental process, and the method adopts mild conditions, is easy to operate and control, high in safety and low in production equipment requirement and contributes to large-scale production.

Description

technical field [0001] The invention relates to a method for preparing sulfonated graphene that can be used for making moisture-sensitive materials. Background technique [0002] Graphene, as a new type of two-dimensional nanomaterial, was prepared for the first time in 2004. With its unique structure and excellent optical, electrical and thermal properties, it has attracted extensive attention from scholars at home and abroad. [0003] Graphene has the characteristics of large specific surface area, high electron mobility, good electrical conductivity, good mechanical properties, and low resistivity. It has a wide range of applications in chemistry, electronics, information, energy, and materials. Due to its high chemical stability and strong van der Waals force between the layers, it is easy to agglomerate and difficult to dissolve in water and common organic solvents. Since the surface of graphene does not have any functional groups, graphene itself has extremely strong ...

Claims

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Application Information

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IPC IPC(8): C01B32/194
CPCC01P2002/72C01P2002/82C01P2004/03
Inventor 张超智陈斌柏源
Owner TAIZHOU CITY GANG YANG RUBBER
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