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Graphene oxide-based curing agent as well as preparation and use thereof

A graphene-based, curing agent technology, applied in the field of material science, can solve the problems of harsh reaction conditions, low efficiency of the main chain grafting method and the grafting main chain method, limiting the application of graphene, etc., and achieves the effect of good electrical conductivity.

Inactive Publication Date: 2015-01-07
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these graphene and its derivatives in the above studies cannot act as curing agents and epoxy groups to achieve covalent bond connection, and the efficiency of the main chain grafting method and the grafting main chain method used in these studies is relatively low, Moreover, the reaction conditions are relatively harsh, which limits the application of graphene in epoxy resins.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] In 100 parts of graphene oxide, add 20 parts of thionyl chloride (SOCl 2 ) and 0.5 parts of anhydrous N,N-dimethylformamide (DMF), reflux at 70°C for 24h, and keep the reaction system in an anhydrous environment. Unreacted SOCl in the above product 2 Pump under reduced pressure to constant weight, then add 20 parts of DMF to the product, after ultrasonication for 10 minutes, slowly add the mixed solution to 20 parts of polyetheramine in an ice bath, continue ultrasonication for 10 minutes to mix the solution evenly, and then react at 120°C After 12 hours, the reaction product was washed with 900 parts of absolute ethanol for 6 times and then dried under vacuum at 60° C. to obtain polyetheramine-GN.

Embodiment 2

[0026] In 100 parts of graphene oxide, add 25 parts of thionyl chloride (SOCl 2 ) and 1.0 parts of anhydrous N,N-dimethylformamide (DMF), reflux at 70°C for 24 hours, and keep the reaction system in an anhydrous environment. Unreacted SOCl in the above product 2 Pump under reduced pressure to constant weight, then add 20 parts of DMF to the product, after ultrasonication for 10 minutes, slowly add the mixed solution to 25 parts of polyamide in an ice bath, continue ultrasonication for 10 minutes, mix the solution evenly, and react at 120°C for 12 hours , The reaction product was washed 6 times with 1000 parts of absolute ethanol and then dried in vacuum at 60°C to obtain polyamide-GN.

Embodiment 3

[0028] In 120 parts of graphene oxide, add 25 parts of thionyl chloride (SOCl 2 ) and 1.5 parts of anhydrous N,N-dimethylformamide (DMF), reflux at 70°C for 24 hours, and keep the reaction system in an anhydrous environment. Unreacted SOCl in the above product 2 Pump under reduced pressure to constant weight, then add 30 parts of DMF to the product, and after ultrasonication for 10 minutes, slowly add the mixed solution to 30 parts of aromatic amines in an ice bath, continue ultrasonication for 10 minutes to mix the solution evenly, and then store at 120°C After reacting for 12 hours, the reaction product was washed 6 times with 1000 parts of absolute ethanol and then dried in vacuum at 60°C to obtain aromatic amine-GN.

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Abstract

The invention discloses a preparation method of a graphene oxide-based curing agent and application of the graphene oxide-based curing agent in epoxy resin conductive glue. The conductive glue consists of the following components in parts by weight: 1-2 parts of a graphene oxide-based curing agent, 3-10 parts of a conventional curing agent, 10-20 parts of E-51 epoxy resin, 10-20 parts of AG-80 epoxy resin, 15-25 parts of carbon black, 15-25 parts of silver precipitate powder, 1-8 parts of amine accelerants, 1-5 parts of a liquid imidazole defoaming agent and 1-20 parts of glycidyl ether diluents. The preparation method of the graphene oxide-based curing agent comprises the following steps: firstly, preparing graphene oxide and then modifying the graphene oxide to obtain a graphene oxide-based curing agent capable of conducting and toughening; and then, blending according to a formula of the conductive glue and curing to obtain a graphene oxide-based epoxy resin composite material. The graphene oxide-based curing agent with capacity of conducting and toughening is obtained by the preparation method; and an epoxy-based composite adhesive material prepared by taking the graphene oxide as the curing agent has good conducting capacity, acid and alkaline resistance, thermal stability and mechanical performance; and the adhesive is suitable for adhering electronic elements.

Description

technical field [0001] The invention relates to a graphene oxide-based curing agent and its preparation method and application, belonging to the field of material science and technology. Background technique [0002] Curing agent is a kind of substance or mixture that promotes or controls the curing reaction. Resin curing is an irreversible change process of thermosetting resin through chemical reactions such as condensation, ring closure, addition or catalysis. The epoxy resin curing agent reacts chemically with the epoxy resin to form a network-like three-dimensional polymer, enveloping the composite material in the network. The existing epoxy resin curing agents are mainly divided into basic, acidic, addition type, catalytic type, apparent type, latent type, amine curing agent, acid anhydride curing agent, synthetic resin curing agent and so on. Epoxy resin is widely used in coatings, composite materials, adhesives, and aviation and aerospace fields because of its excel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/50C08G59/44C09J163/02C09J163/00C09J11/00C09J11/06C09J11/04C09J9/02C01B31/04
Inventor 郭坤琨刘凤丹宋艳杰郭荣中李柱
Owner HUNAN UNIV
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