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Preparation method of in situ intercalated solution of carboxyl graphene oxide benzoxazine nano-composite resin

An alkenyl benzoxazine and in-situ intercalation technology, applied in the field of polymer material science and engineering, can solve the problem of reducing the curing temperature of benzoxazine resin without nanocomposite resin, achieve fast curing rate, and easy to obtain raw materials , the effect of high glass transition temperature

Active Publication Date: 2015-01-07
淮北绿洲新材料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The carboxyl functional group can promote the curing of benzoxazine resin and reduce the curing temperature, but so far there is no nanocomposite resin prepared by blending carboxylated graphene oxide and benzoxazine resin to reduce the curing temperature of benzoxazine resin report

Method used

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Embodiment 1

[0034] A kind of preparation method of the in-situ intercalation solution of carboxylated graphene oxide benzoxazine nanocomposite resin, concrete steps are as follows:

[0035]Using natural flake graphite with a particle size of 20 μm as raw material, graphite oxide was prepared by the improved Hummers method, specifically adding natural flake graphite to a 9:1 sulfuric acid / phosphoric acid mixture, stirring, adding potassium permanganate, and , natural flake graphite accounts for 2%, sulfuric acid / phosphoric acid mixture accounts for 86%, potassium permanganate accounts for 12%, control the temperature of concentrated sulfuric acid at 4°C, react for 45min, raise the temperature to 50°C, react for 14h, and the reaction product is washed by centrifugation to no After sulfate ions, dry at 55°C to obtain graphite oxide; chemically modify the obtained graphite oxide through the chloroacetic acid method, specifically, prepare the obtained graphite oxide into a 2 mg / mL solution, and...

Embodiment 2

[0038] A kind of preparation method of the in-situ intercalation solution of carboxylated graphene oxide benzoxazine nanocomposite resin, concrete steps are as follows:

[0039] Using natural flake graphite with a particle size of 24 μm as raw material, graphite oxide was prepared by the improved Hummers method, specifically adding natural flake graphite to a 9:1 sulfuric acid / phosphoric acid mixture, stirring, adding potassium permanganate, and , natural flake graphite accounts for 1%, sulfuric acid / phosphoric acid mixture accounts for 93%, potassium permanganate accounts for 6%, control the temperature of concentrated sulfuric acid at 6°C, react for 50min, raise the temperature to 55°C, react for 24h, and the reaction product is washed by centrifugation to no After sulfate ions were dried at 50°C, graphite oxide was obtained; the obtained graphite oxide was chemically modified by the chloroacetic acid method, specifically, the graphite oxide was formulated into a 2 mg / mL solu...

Embodiment 3

[0042] A kind of preparation method of the in-situ intercalation solution of carboxylated graphene oxide benzoxazine nanocomposite resin, concrete steps are as follows:

[0043] Using natural flake graphite with a particle size of 30 μm as raw material, graphite oxide was prepared by the improved Hummers method, specifically adding natural flake graphite to a 9:1 sulfuric acid / phosphoric acid mixture, stirring, adding potassium permanganate, and , natural flake graphite accounted for 3%, sulfuric acid / phosphoric acid mixture accounted for 79%, potassium permanganate accounted for 18%, controlled the temperature of concentrated sulfuric acid at 5°C, reacted for 60min, raised the temperature to 55°C, reacted for 24h, and the reaction product was washed by centrifugation to no After sulfate ions, dry at 60°C to obtain graphite oxide; chemically modify the obtained graphite oxide through the chloroacetic acid method, specifically prepare graphite oxide into a 2 mg / mL solution, then...

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Abstract

The invention discloses a preparation method of in situ intercalated solutionof carboxyl graphene oxide benzoxazine nano-composite resin. The method comprises the following steps of: preparing graphene oxide by using natural crystalline flake graphite as raw materials by utilizing an improved Hummers method; chemically modifying the graphene oxide by utilizing a chloroacetic acid method to obtain carboxyl graphene oxide; ultrasonically dispersing carboxyl graphene oxide into an organic solvent to obtain carboxyl graphene oxide solution; dissolving benzoxazine prepolymer into the organic solvent to obtain benzoxazine prepolymer solution; blending the carboxyl graphene oxide solution with the benzoxazine prepolymer solution to obtain the in situ intercalated solution by utilizing an in situ intercalated solution polymerization method. The preparation method is simple in process, and the raw materials are easily obtained. By adding carboxyl graphene oxide, the curing temperature of the composite resin is reduced, the processibility and glass-transition temperature are improved, and the heat resistance of resin is increased. Moreover, the preparation method has wide application prospect in the fields of copper-cladding boards, laminated boards, spacecrafts and the like.

Description

technical field [0001] The invention belongs to the technical field of polymer material science and engineering, and in particular relates to a method for preparing an in-situ intercalation solution of carboxylated graphene oxide benzoxazine nanocomposite resin. Background technique [0002] Benzoxazine is a class of benzo six-membered heterocyclic intermediates synthesized from phenols, aldehydes and primary amines. It undergoes ring-opening polymerization under the action of heating or a catalyst to form nitrogen-containing and similar phenolic resins. The network structure of polybenzoxazine or benzoxazine resin (BOZ) (Yagci Y, et al. Journal of Polymer Science: Part A, 2009, 47, 5565; Wu Y, Zeng M, et al . Tribology International, 2012, 54, 51). Benzoxazine resin has good heat resistance, moisture resistance, mechanical properties and electrical properties. The essential difference between it and ordinary phenolic resin is that no small molecules are released during the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/06C08K9/04C08K3/04B82Y40/00
Inventor 曾鸣郁燕李然然刘建新许清强
Owner 淮北绿洲新材料有限责任公司
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