Preparation method of cellular three-dimensional graphene

A graphene and honeycomb technology, which is applied in the field of preparation of honeycomb three-dimensional graphene, can solve the problems of difficult mass production, excessive waste liquid, and increase the complexity of the production process, and achieve easy mass production, avoiding the experimental process, and synthesizing The method is simple and efficient

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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] To sum up, most of the existing three-dimensional graphene preparation methods need to use templates for structure building, and then remove the templates, which not only increases the complexity of the production process, but also produces more waste liquid, making it difficult to mass-produce

Method used

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  • Preparation method of cellular three-dimensional graphene
  • Preparation method of cellular three-dimensional graphene
  • Preparation method of cellular three-dimensional graphene

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Step A. Preparation of graphene oxide.

[0025] Step A1. Weigh flake graphite powder, concentrated sulfuric acid, concentrated phosphoric acid, potassium permanganate, deionized water, hydrogen peroxide, and dilute hydrochloric acid as raw materials; wherein, the ratio of flake graphite powder to concentrated sulfuric acid is 1.5 g: 180 mL, The ratio of flake graphite powder to concentrated phosphoric acid is 1.5 g: 20 mL, the ratio of graphite powder to potassium permanganate is 1.5 g: 9 g, and the concentration of hydrogen peroxide is 35%;

[0026] Step A2. In a water bath at room temperature, add concentrated sulfuric acid and concentrated phosphoric acid mixed acid into the three-necked bottle, mechanically stir until the temperature of the mixed acid returns to room temperature, add flake graphite powder, slowly add potassium permanganate in portions, and the temperature of the system rises slowly , control the addition rate of potassium permanganate so that the sy...

Embodiment 2

[0035] Carry out according to the method shown in embodiment 1, difference is only in the add-on of metal-free phthalocyanine in B1 step be 0.5g, the inert gas of step C is nitrogen+hydrogen, and its gas flow is 50 cm 3 min -1 . After solid-phase cleavage and self-assembly, the morphology of the obtained honeycomb three-dimensional graphene is as follows: figure 2 As shown, its specific surface area is 298.2 m 2 g -1 .

Embodiment 3

[0037] Implement according to the method shown in Example 1, the difference is only that the addition of metal-free phthalocyanine is 3g in the B1 step, and the inert gas of step C is nitrogen, and its gas flow is 10 cm 3 min -1 . After self-assembly by solid-phase cleavage, the transmission electron microscope image of the obtained honeycomb three-dimensional graphene is as follows image 3 , with a specific surface area of ​​251.6 m 2 g -1 .

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Abstract

The invention discloses a preparation method of cellular three-dimensional graphene. The preparation method comprises the following steps: performing ultrasonic dispersion and mixing of graphene oxide and phthalocyanine compound to obtain a graphene oxide/phthalocyanine composite precursor; and sintering the graphene oxide/phthalocyanine composite precursor by a temperature programmed sintering method through a solid-phase cracking process under inert gas protection for cracking and self-assembly of the raw materials to finally obtain a cellular three-dimensional graphene material. The preparation method disclosed by the invention has the advantages of simple process, high product purity and industrialization promotion; and the prepared composite material can be applied to the fields such as new energy, radiating materials and catalysts.

Description

technical field [0001] The invention belongs to the field of graphene preparation, in particular to a method for preparing honeycomb three-dimensional graphene. Background technique [0002] Graphene is a two-dimensional planar structure in which carbon atoms are hybridized in the form of sp2. This hybridization method allows carbon atoms to form stable C-C bonds with three adjacent carbon atoms through σ bonds. This bonding method endows graphene with stability. Structure. However, graphene itself is a huge aromatic conjugated molecule, which is easy to stack and agglomerate due to its hydrophobic structure, strong π-π interaction and van der Waals force between sheets, and in most practical applications, It is usually necessary to assemble graphene into macroscopic objects, and the agglomeration and stacking of graphene layers will greatly reduce the effective area of ​​graphene, thereby gradually losing the original excellent physical properties of graphene. In view of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
CPCC01B2204/32C01P2004/03C01P2004/04
Inventor 薛卫东赵睿
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