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Preparation method and product of in-situ reduced graphene oxide/benzoxazine composite material

A technology of benzoxazine and composite materials, which is applied in the field of composite materials, can solve problems such as poor heat resistance, low crosslinking density of composite resins, and small interaction between nanoparticles and resins, so as to improve compatibility, improve dispersion, Ease of chemical and physical interaction effects

Active Publication Date: 2019-04-16
成都科宜高分子科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are problems such as small interaction between nanoparticles and resin, low crosslinking density of composite resin, brittleness, and poor heat resistance.

Method used

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  • Preparation method and product of in-situ reduced graphene oxide/benzoxazine composite material
  • Preparation method and product of in-situ reduced graphene oxide/benzoxazine composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Add 0.2g (0.1wt%) graphene oxide in a three-necked flask of 250mL, and disperse it in a mixed solvent of 20g ethanol and water (wherein the volume ratio of ethanol and water is 8: 2) in, and adjust PH with triethylamine to be 8, obtain graphene oxide dispersion liquid;

[0030] (2) Add 8.66g (0.092mol) of phenol to the graphene oxide dispersion, ultrasonically treat it with a power of 300w for 60min, add triethylamine to adjust the pH to 8, and then mechanically stir at 70°C for 2h to obtain phenol / graphene oxide Dispersions;

[0031] (3) Add 2.77g (0.092mol) of paraformaldehyde to the prepared phenol / graphene oxide dispersion, then mechanically stir at 70°C for 1h, perform in-situ reduction reaction and phenol methylolation reaction, and obtain phenol / formaldehyde / graphene oxide mixture;

[0032] (4) Reduce the temperature of the phenol / formaldehyde / graphene oxide mixture system to 50°C, add 50g DMF until the system is not viscous, add 4.14g (0.138mol) formaldeh...

Embodiment 2

[0034] (1) Add 0.2g (0.1wt%) graphene oxide to a 250mL three-necked flask, and ultrasonically treat it with a power of 500w for 30 minutes to disperse it in 20g of methanol solvent, and adjust the pH to 8.5 with NaOH solution to obtain graphite oxide olefin dispersion;

[0035] (2) Add 8.66g (0.092mol) phenol to the graphene oxide dispersion, ultrasonically treat it with a power of 500w for 30min, add NaOH solution to adjust the pH to 8.5, and then mechanically stir at 70°C for 2h to obtain a phenol / graphene oxide dispersion liquid;

[0036] (3) Add 4.15 g (0.138 mol) of paraformaldehyde to the prepared phenol / graphene oxide dispersion, then mechanically stir at 70°C for 1 h, perform in situ reduction reaction and phenol hydroxymethylation reaction, and obtain phenol / formaldehyde / graphene oxide mixture;

[0037] (4) Reduce the temperature of the phenol / formaldehyde / graphene oxide mixture system to 60°C, add 50g DMF until the system is not viscous, add 6.9g (0.23mol) formald...

Embodiment 3

[0039](1) Add 0.6g (0.3wt%) graphene oxide to a 500mL three-necked flask, disperse it in 50g of DMF by ultrasonic treatment with 600w power for 60min, and adjust the pH to 8 with KOH solution to obtain graphite oxide olefin dispersion;

[0040] (2) Add 8.66g (0.092mol) of phenol to the graphene oxide dispersion, ultrasonically treat it with a power of 600w for 60min, add KOH solution to adjust the pH to 9, and then mechanically stir at 70°C for 2h to obtain a phenol / graphene oxide dispersion liquid;

[0041] (3) Add 3.04g (0.101mol) trioxane to the prepared phenol / graphene oxide dispersion, then mechanically stir at 70°C for 1h, carry out in situ reduction reaction and phenol hydroxymethylation reaction, and obtain phenol / formaldehyde / graphene oxide mixture;

[0042] (4) Reduce the temperature of the phenol / formaldehyde / graphene oxide mixture system to 60°C, add 50g DMF until the system is not viscous, add 6.08g (0.203mol) trioxane, stir to disperse evenly, and at the same ...

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Abstract

The invention discloses a preparation method and a product of an in-situ reduced graphene oxide / benzoxazine composite material. According to the method, a phenolic compound and formaldehyde are firstly used as reducing agents, and graphene oxide is reduced 'in situ'; then, an 'in-situ' reduced graphite oxide / phenolic compound system is used as a phenol source, and a formaldehyde source is added tomake the 'in-situ' reduction reaction continue. The method adopts the 'in-situ' reduction method, so that on one hand, a graphite structure is more perfect after the graphite oxide is reduced; on theother hand, a chemical bond is formed between the graphene oxide and the phenolic compound through the reduction reaction, uniform dispersion of graphene oxide in benzoxazine is facilitated, and meanwhile the mutual effects of a benzoxazine polymer network and the graphene oxide are strengthened. Therefore, the graphene oxide / benzoxazine composite material prepared by the method has excellent heat resistance, thermal stability and mechanical properties and is suitable for preparation of high-performance high-temperature-resistant materials or high-temperature anti-corrosion materials.

Description

technical field [0001] The invention relates to the technical field of composite materials, in particular to a preparation method of an in-situ reduced graphene oxide / benzoxazine composite material and a product thereof. Background technique [0002] Polybenzoxazine resin is a new type of thermosetting resin developed on the basis of traditional phenolic resin. It has flexible molecular design. Its monomer benzoxazine is formed by Mannich condensation reaction of phenols, primary amines and formaldehyde. The obtained six-membered heterocyclic compound can be synthesized to meet different needs of intermediate resins by selecting different types of phenolic and amine monomers. Heating can be cured by ring-opening polymerization to form a polybenzoxazine resin with a cross-linked structure similar to phenolic resin. In addition to the advantages of traditional phenolic resins (such as high temperature resistance, flame retardancy, good dielectric properties and mechanical pro...

Claims

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Application Information

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IPC IPC(8): C08G14/073C08K3/04
CPCC08G14/06C08K3/042
Inventor 盛玉萍夏益青高晨廖彬李新跃张雪梅侯真良李晓莲唐利平杜若佳
Owner 成都科宜高分子科技有限公司