Ultralow-oxygen-content three-dimensional nitrogen-doped graphene aerogel and preparation method thereof

A nitrogen-doped graphene, graphene aerogel technology, applied in graphene, chemical instruments and methods, inorganic chemistry, etc. Completely removed, the types of nitrogen-containing functional groups are not adjustable, etc., to achieve the effect of adjustable three-dimensional porous structure, low equipment and raw material requirements, and fewer surface defects

Active Publication Date: 2021-09-14
GRIMAT ENG INST CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN111186832A uses graphene oxide and organic nitrides as precursors to prepare nitrogen-doped graphene aerogels through hydrothermal reaction and heat treatment. The XPS full-spectrum scanning charts have peaks at 285eV, 399eV and 532eV, corresponding to C The characteristic peaks of , N and O elements indicate that nitrogen atoms are introduced into the graphene sheet but oxygen atoms still exist, and the oxygen-containing functional groups at the edge of the graphene sheet have not been completely removed
The main reason is that the oxygen-containing functional groups of graphene oxide and the synergistic effect between the nitrogen dopant and the hydrothermal reducing agent limit the deep extraction of the oxygen-containing functional groups of graphene oxide, and the incomplete removal of the oxygen-containing functional groups leads to high oxygen content, The types of nitrogen-containing functional groups cannot be adjusted, and the degree of sheet structure recovery is low, which affects the performance and application of nitrogen-doped graphene airgel

Method used

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  • Ultralow-oxygen-content three-dimensional nitrogen-doped graphene aerogel and preparation method thereof
  • Ultralow-oxygen-content three-dimensional nitrogen-doped graphene aerogel and preparation method thereof
  • Ultralow-oxygen-content three-dimensional nitrogen-doped graphene aerogel and preparation method thereof

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preparation example Construction

[0080] 3, the third object of the present invention is to provide a kind of preparation method of ultra-low oxygen content three-dimensional nitrogen-doped graphene airgel, the preparation method of graphene airgel comprises the steps:

[0081] Step 1): Graphene oxide is used as a precursor to form an aqueous dispersion, and nitrogen sources, reducing agents, and amine-based small-molecule organic compounds are added in sequence, and a cylindrical low-oxygen three-dimensional nitrogen-doped graphene water is prepared by a one-step hydrothermal reduction method. Gel, after freeze-drying, a three-dimensional nitrogen-doped graphene airgel intermediate with low oxygen content is obtained;

[0082] A lightweight three-dimensional nitrogen-doped graphene hydrogel with high nitrogen-doped content and high proportion of pyrrole-type nitrogen was prepared by hydrothermal reduction method, and then the airgel intermediate was obtained by dialysis to desalt and freeze-dried. The nitrogen...

Embodiment 1

[0097] 1.1 Preparation of low carboxyl group and high hydroxylation few-layer graphene oxide precursor aqueous solution

[0098] Step 1-1): using natural graphite plate as anode, metal titanium mesh as cathode, ammonium sulfate as electrolyte and intercalation agent, sodium dodecylsulfonate as auxiliary additive, and water as solvent to prepare electrolyte;

[0099] Step 1-2): Prepare low-carboxyl and high-hydroxylation few-layer graphene oxide by electrochemical intercalation and stripping the anode method. The specific steps are as follows: cut the thickness to 2mm and the area to 15cm 2 The natural graphite plate as the anode is connected to the positive pole of the 20V DC power supply, and the titanium mesh cathode with more than twice the area of ​​the anode is connected to the negative pole of the 20V DC power supply to form an electrode pair; a 0.1mol / L ammonium sulfate aqueous solution is prepared and added to the electrolytic cell for electrolysis. The liquid volume a...

Embodiment 2

[0111] 2.1 Preparation of low carboxyl group and high hydroxylation few-layer graphene oxide precursor aqueous solution:

[0112] Step 1-1): Using a dense crystalline graphite plate as an anode, a metal titanium mesh as a cathode, ammonium sulfate as an electrolyte and an intercalation agent, sodium dodecylsulfonate as an auxiliary additive, and water as a solvent to prepare an electrolyte;

[0113] Step 1-2): Using electrochemical intercalation exfoliation anodic oxidation to prepare low-carboxyl and high-hydroxylation few-layer graphene oxide, the specific steps are as follows: cut a thickness of 2mm and an area of ​​15cm 2 The scaly graphite plate is used as the anode and connected to the positive pole of the 20V DC power supply, and the titanium mesh cathode with more than twice the area of ​​the anode is connected to the negative pole of the 20V DC power supply to form an electrode pair; a 0.2mol / L ammonium sulfate aqueous solution is prepared and added to the electrolytic...

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Abstract

The invention discloses an ultralow-oxygen-content three-dimensional nitrogen-doped graphene aerogel and a preparation method thereof, belonging to the technical field of graphene aerogel. According to the method, a graphene oxide precursor is adopted for preparation of low-carboxyl highly-hydroxylated graphene oxide through an electrolytic method; and then one-step hydrothermal reduction nitrogen-doped in-situ self-assembling and high-temperature sintering are conducted to obtain the ultralow-oxygen-content three-dimensional nitrogen-doped graphene aerogel with a light three-dimensional grid structure, wherein an oxygen content is less than 0.1 at.%, a nitrogen doping amount is 4-12%, and pyridine type nitrogen accounts for 30-80%.

Description

technical field [0001] The invention belongs to the technical field of graphene airgel, in particular to a three-dimensional nitrogen-doped graphene airgel with ultra-low oxygen content and a preparation method thereof. Background technique [0002] The properties of graphene such as thermal conductivity and electrical conductivity are mainly derived from the single-layer carbon atoms with sp 2 The two-dimensional honeycomb lattice structure formed by hybrid arrangement and close packing and the unbonded π electrons form a large delocalized electronic structure. Heteroatom (such as nitrogen, oxygen, phosphorus, sulfur, boron, etc.) doping and regulated self-assembly constructs a three-dimensional doped graphene airgel, which inherits the excellent electrical and thermal conductivity of graphene, and at the same time has the characteristics of airgel The three-dimensional network cross-linked structural characteristics of ultra-low density, ultra-high specific surface area a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/184C01B32/198
CPCC01B32/184C01B32/198
Inventor 蒋文全罗熳武媛方樊哲吴凡
Owner GRIMAT ENG INST CO LTD
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