Nitrogen-rich group functionalized graphene oxide and preparation method and application thereof

A functionalized graphene technology, applied in chemical instruments and methods, inorganic chemistry, carbon compounds, etc., can solve problems such as processing difficulties, dispersion stability effects, etc. The effect of stability

Active Publication Date: 2019-11-29
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Many literatures have revealed the excellent flame retardant efficiency of graphene on polymers, however, due to the strong π-π interaction between each graphene sheet, its dispersion and stability in solution are affected to some extent.
Therefore, graphene is easy to aggregate in the polymer matrix, which brings certain difficulties to the subsequent processing

Method used

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  • Nitrogen-rich group functionalized graphene oxide and preparation method and application thereof
  • Nitrogen-rich group functionalized graphene oxide and preparation method and application thereof
  • Nitrogen-rich group functionalized graphene oxide and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Synthesis of compounds containing phosphorus and nitrogen elements

[0026] In a 150mL three-necked flask, add 1.83g of 3-amino-1,2,4-triazole and 2.66g of p-hydroxybenzaldehyde dissolved in 30mL of absolute ethanol, and stir the reaction at a reaction temperature of 50°C under nitrogen protection. Hour. Then, 30 mL of absolute ethanol containing 4.70 g DOPO was added dropwise with a constant pressure dropping funnel, and the reaction was continued for 12 hours. Finally, it was cooled to room temperature, and the product was purified by vacuum filtration and drying.

[0027] (2) Synthesis of Phosphorus and Nitrogen Functionalized Graphene

[0028] After 50 mg of graphene oxide was sonicated in DMF for 1 hour, 15 mL of DMF dissolved in 25 mg of DMAP, 100 mg of DCC and 0.174 g of a compound containing phosphorus and nitrogen was added, and stirred at room temperature for 36 hours. After the reaction, the product was washed with DMF and deionized water several times...

Embodiment 2

[0031] (1) Synthesis of compounds containing phosphorus and nitrogen elements

[0032] In a 150mL three-necked flask, add 1.83g of 3-amino-1,2,4-triazole and 2.66g of p-hydroxybenzaldehyde dissolved in 30mL of anhydrous methanol, and stir the reaction at a reaction temperature of 50°C under nitrogen protection. Hour. Then, 30 mL of anhydrous methanol containing 4.70 g DOPO was added dropwise with a constant pressure dropping funnel, and the reaction was continued for 12 hours. Finally, it was cooled to room temperature, and the product was purified by vacuum filtration and drying.

[0033] (2) Synthesis of Phosphorus and Nitrogen Functionalized Graphene

[0034] After 50 mg of graphene oxide was sonicated in DMF for 1 hour, 15 mL of absolute ethanol dissolved in 50 mg of DMAP, 200 mg of DCC and 0.18 g of phosphorus and nitrogen-containing compounds were added, and stirred at room temperature for 36 hours. After the reaction, the product was washed with absolute ethanol and ...

Embodiment 3

[0036] (1) Synthesis of compounds containing phosphorus and nitrogen elements

[0037] In a 150mL three-neck flask, add 1.83g of 3-amino-1,2,4-triazole and 3.16g of p-hydroxybenzaldehyde dissolved in 30mL of absolute ethanol, and stir the reaction at a reaction temperature of 50°C under nitrogen protection. Hour. Then, 30 mL of absolute ethanol containing 5.21 g DOPO was added dropwise with a constant pressure dropping funnel, and the reaction was continued for 12 hours. Finally, it was cooled to room temperature, and the product was purified by vacuum filtration and drying.

[0038] (2) Synthesis of Phosphorus and Nitrogen Functionalized Graphene

[0039] After 100 mg of graphene oxide was sonicated in DMF for 1 hour, 15 mL of DMF dissolved in 50 mg of DMAP, 150 mg of EDC and 0.20 g of a compound containing phosphorus and nitrogen was added, and stirred at room temperature for 36 hours. After the reaction, the product was washed with DMF and deionized water several times, ...

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Abstract

The invention discloses a preparation method of nitrogen-rich group functionalized graphene oxide. A phosphorus and nitrogen compound is synthesized by a simple and convenient method. Through esterification reaction between phenolic hydroxyl groups on the compound and carboxyl groups on graphene oxide, an introduced phosphaphenanthrene functional group is expected to improve the dispersibility ofgraphene in an organic solvent, and secondary amine on the compound can also participate in the curing process of epoxy resin to improve the compatibility of the graphene in the epoxy resin. In the invention, phosphorus and nitrogen flame retardant elements are introduced into the graphene oxide to synthesize a flame retardant which can play a flame retardant role in a condensed phase and a gas phase, and is expected to improve the thermal stability of the epoxy resin. The flame retardant has mild reaction conditions, does not contain halogen elements, and is a novel environment-friendly flameretardant.

Description

technical field [0001] The invention belongs to the field of modification of graphene, and in particular relates to a nitrogen-rich group functionalized graphene, a preparation method and an application. Background technique [0002] As a typical thermosetting polymer, epoxy resin has the advantages of good chemical stability, low shrinkage, easy processing and low cost. Therefore, it has been widely used in high-tech fields such as transportation and aerospace. However, the phenomena of flammability, dripping and rapid flame spread in the event of fire greatly limit the application of the material. Therefore, in order to achieve sustainable development, research on green flame-retardant epoxy resins is still in full swing. [0003] Traditional halogen-free flame-retardant epoxy resin materials achieve the purpose of flame retardancy by chemically or physically adding nitrogen, phosphorus, silicon, etc. Nitrogen-containing flame retardants emit inert gases, but they are o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/198C08K9/04C08K3/04C08L63/00
CPCC08K9/04C08K3/042C01B32/198C08L63/00
Inventor 戴李宗吴雯倩许一婷李伟航罗伟昂陈国荣
Owner XIAMEN UNIV
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