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Functionalized graphene oxide enhanced benzoxazine-based composite resin and preparation method thereof

A technology of benzoxazine and composite resin, which is applied in the field of polymer materials, can solve the problems of small interaction between nanoparticles and resin, low crosslinking density of composite resin, and lower resin curing temperature, so as to improve processing performance and physical properties, Effect of improving heat resistance and increasing glass transition temperature

Inactive Publication Date: 2015-12-02
CHINA UNIV OF GEOSCIENCES (WUHAN)
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Zeng Ming et al. used the in-situ intercalation polymerization method to prepare graphite oxide benzoxazine nanocomposite resin for the first time. The research showed that graphene oxide reduced the curing temperature of the resin and improved the thermal stability of the resin (ZengM., Polymer, 2013, 54, 3107), but there are problems such as small interaction between nanoparticles and resin, low crosslinking density of composite resin, brittleness, poor heat resistance, etc.

Method used

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  • Functionalized graphene oxide enhanced benzoxazine-based composite resin and preparation method thereof
  • Functionalized graphene oxide enhanced benzoxazine-based composite resin and preparation method thereof

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preparation example Construction

[0034] Preparation of carboxylated graphene oxide:

[0035] Using natural flake graphite with a particle size of 50 μm as a raw material, graphite oxide was obtained through an improved Hummers method, wherein the improved Hummers method was to add natural flake graphite to a sulfuric acid / phosphoric acid mixed solution with a volume ratio of 9:1, stir, add Potassium permanganate; specifically: by mass %, natural flake graphite accounts for 3, sulfuric acid / phosphoric acid mixture accounts for 85, and potassium permanganate accounts for 12; control the reaction system temperature below 10°C in an ice-water bath, and heat up after 60 minutes of reaction Reaction at 40°C for 20 hours; the reaction product was washed by centrifugation until there was no sulfate ion, and then dried at 60°C to obtain graphite oxide.

[0036] Then chemically modify graphite oxide by chloroacetic acid method to obtain carboxylated graphene oxide: first add graphite oxide to deionized water and ultras...

Embodiment 1

[0041] Preparation of carboxylated graphene-reinforced benzoxazine / phenolic binary nanocomposite resin:

[0042] According to the mass % ratio, 1% carboxylated graphene oxide and 99% bisphenol A benzoxazine monomer (molecular formula C 22 h 3 0N 2 o 2 , molecular weight 354) / first-stage phenolic resin (phenol source is phenol, cresol, xylenol) prepolymer mixture is blended and intercalated in a high-speed planetary ball mill, wherein the bisphenol A benzoxazine monomer The mass ratio of bisphenol A benzoxazine monomer to the first-stage phenolic resin prepolymer in the first-stage phenolic resin prepolymer is 6:4. The specific process is to first ball mill the mixture at 400rpm for 3 hours, and then at 500rpm for 1 hour. During this process, the high-speed planetary ball mill runs continuously for 20 minutes and stops for 5 minutes.

[0043] The obtained mixed sample was vacuum degassed at 80°C for 2h to remove air bubbles, and then cured at 220°C for 6h to obtain carboxyl...

Embodiment 2

[0046] Preparation of aminated graphene-reinforced benzoxazine / phenolic binary nanocomposite resin:

[0047] According to the mass % ratio, 1% aminated graphene oxide and 97% bisphenol F benzoxazine monomer (molecular formula C 30 h 30 N 2 o 2 , molecular weight 450) / secondary phenolic resin (phenol source is phenol) prepolymer mixture for blending, intercalation, wherein bisphenol F benzoxazine monomer / secondary phenolic resin prepolymer bisphenol F benzene The mass ratio of oxazine monomer to the second-order phenolic resin prepolymer is 7:3. The specific process is to ball mill the mixture at 400rpm for 3 hours, and then at 500rpm for 1 hour. During this process, the high-speed planetary ball mill continues to run for 20 minutes. Turn for 5 minutes.

[0048] The mixed sample was vacuumed and degassed at 100°C for 1 hour to remove air bubbles, and then cured at 200°C for 8 hours to obtain an aminated graphene oxide reinforced benzoxazine / phenolic binary nanocomposite res...

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Abstract

The invention relates to a functionalized graphene oxide enhanced benzoxazine-based composite resin and a preparation method thereof. The resin is prepared by: 1, preparing natural flake graphite into graphene oxide by a modified Hummers method; 2, chemically modifying the graphene oxide to obtain carboxylated graphene oxide or aminated graphene oxide; 3, physically mixing, by weight, 0.1-10% of the carboxylated graphene oxide or aminated graphene oxide with 90-99.9% of benzoxazine binary resin prepolymer or benzoxazine ternary resin prepolymer to obtain a mixed sample; 4, evacuating the mixed sample at 80-100 DEG C for 1-2h, and allowing curing reaction at 100-220 DEG C for 4-24h so as to obtain the functionalized graphene oxide enhanced benzoxazine-based composite resin. The prepared composite resin cures without shrinking and has good heat resistance, moisture resistance, mechanical performances and electrical performances.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a class of functionalized graphene oxide reinforced benzoxazine-based composite resins and a solvent-free in-situ intercalation polymerization method thereof. Background technique [0002] A class of intermediates containing heterocyclic structures—benzoxazines synthesized from phenols, aldehydes, and primary amines, undergo ring-opening polymerization under the action of heating and / or catalysts to produce nitrogen-containing and phenolic resin-like The network structure is called polybenzoxazine or benzoxazine resin (BOZ). As a new type of thermosetting engineering resin, compared with traditional phenolic and epoxy resins, it not only has good flame retardancy and chemical resistance, but also has the advantages of low shrinkage, low dielectric constant and flexible molecular design. , and can be heated and cured without a catalyst, and no small molecules are releas...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/06C08G59/20C08G59/62C08K9/04C08K3/04
Inventor 曾鸣许清强徐庆玉李然然殷蝶曾碧君
Owner CHINA UNIV OF GEOSCIENCES (WUHAN)
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