Preparation method of edge-carboxylated graphene

A technology of carboxylated graphene and edge, which is applied in the field of preparation of carboxylated graphene, can solve the problems of difficult preparation and achieve the effects of good stability, improved efficiency, and long-term stable preparation

Active Publication Date: 2020-02-21
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation of such selectively modified graphene is difficult
At present, there are few application literature reports

Method used

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  • Preparation method of edge-carboxylated graphene
  • Preparation method of edge-carboxylated graphene
  • Preparation method of edge-carboxylated graphene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069] 100g 32 mesh flake graphite powders are ultrasonically cleaned (washed once with water, washed twice with ethanol) to remove impurity substances and impurity elements, then place the graphite flakes in a high-pressure grinding pan kettle, seal the high-pressure grinding pan kettle, and then place the high-pressure The disc kettle was heated to 40°C and pumped in CO 2 Make the pressure in the high-pressure grinding disc kettle rise to 85atm, and the rotating speed is 500r / min. Use the shear force generated by the grinding disc to grind and peel off the graphite. After stirring for 24 hours, reduce the pressure to 1 atm within 10s, and take samples from the high-pressure grinding disc kettle. The edge carboxylated graphene is obtained.

[0070] Scanning electron microscope (SEM) is used to the obtained edge carboxylated graphene (such as figure 1 Shown) analysis, the diameter of graphene sheet is 5-20 μm, elemental analysis (XPS) characterizes, and oxygen content is 5.60...

Embodiment 2

[0072] 40g of expanded graphite is ultrasonically cleaned (washed once with water, washed twice with ethanol) to remove impurities and impurity elements, then place the expanded graphite in a high-pressure grinding still, seal the high-pressure grinding still, then heat the high-pressure grinding still to 40°C by pumping in CO 2 Make the pressure in the high-pressure grinding disc kettle rise to 85atm, and the rotating speed is 500r / min. Use the shear force generated by the grinding disc to grind and peel off the graphite. After stirring for 48 hours, the pressure will be reduced to 1 atm within 10s. Take samples from the high-pressure grinding disc kettle. The edge carboxylated graphene is obtained.

[0073] The prepared edge carboxylated graphene was analyzed by scanning electron microscope (SEM), and the diameter of the graphite flakes was 5-20 μm, characterized by elemental analysis (XPS), and the oxygen content was 7.83%.

Embodiment 3

[0075] 100g 32 mesh flake graphite powders are ultrasonically cleaned (washed once with water, washed twice with ethanol) to remove impurity substances and impurity elements, then place the graphite flakes in a high-pressure grinding pan kettle, seal the high-pressure grinding pan kettle, and then place the high-pressure The disc kettle is heated to 70°C, and CO is pumped in 2 Make the pressure in the high-pressure grinding disc kettle rise to 125atm, and the rotating speed is 1000r / min. Use the shear force generated by the grinding disc to grind and peel off the graphite. After stirring for 24 hours, the pressure will be reduced to 1 atm within 10s. Take samples from the high-pressure grinding disc kettle. The edge carboxylated graphene is obtained.

[0076] The obtained edge carboxylated graphene was analyzed by scanning electron microscope (SEM), and the diameter of the graphene sheet was 5-10 μm, characterized by elemental analysis (XPS), and the oxygen content was 13.40%....

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Abstract

The invention discloses a preparation method of carboxylated graphene. The method comprises the following steps of grinding graphite powder in the presence of supercritical carbon dioxide in a high-pressure millstone kettle. Through the preparation method, carboxyl-modified, especially edge-carboxyl-modified graphene can be directly obtained, the introduced carboxyl content can be controlled in arelatively wide range, and large-area edge-modified graphene can also be prepared.

Description

technical field [0001] The invention relates to a method for preparing carboxylated graphene, in particular to a method for preparing edge carboxylated graphene. Background technique [0002] Functionalized graphene refers to the introduction of functional groups, such as carboxyl, amine, and epoxy groups, on the surface or edge of graphene through chemical reactions. The main purpose of introducing functional groups is to increase the polarity of graphene or provide chemical reaction sites to enhance the interaction between graphene and other materials. However, the introduction of active groups destroys the conjugated system on the surface of graphene, which definitely weakens the excellent performance of graphene. The more modification groups are introduced, the greater the performance of graphene will be reduced. If the functional groups are only introduced at the edge of graphene, the conjugated system on the surface of graphene will not be destroyed, thereby preservin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/19
CPCC01B32/19Y02P20/54
Inventor 王湘乔金樑张晓红戚桂村韩朋曾宪忠陈翔李秉海宋志海蔡传伦高建明赖金梅张江茹茹越蒋海斌张红彬
Owner CHINA PETROLEUM & CHEM CORP
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