A kind of graphene oxide-containing multifunctional epoxy resin-based water-soluble sizing agent and preparation method thereof

A technology of epoxy resin and epoxy resin, which is applied in the field of graphene nanocomposite materials and carbon fiber composite materials, can solve the problems of low glass transition temperature, low crosslinking density of cured products, and affecting the use of composite materials, and achieve high Effects of glass transition temperature, overcoming heat resistance deficiency, and ease of handling

Active Publication Date: 2020-04-07
北京石墨烯技术研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this type of glycidyl ether type epoxy resin is mostly a two-functional epoxy resin, and its cured product has a low crosslinking density, a low glass transition temperature, and poor heat resistance, which affects the application of composite materials in some special fields. Therefore, it is very urgent to develop high-temperature-resistant carbon fiber sizing agents based on multi-functional epoxy resins such as three-functional groups and four-functional groups.
[0004] At present, the sizing agent is mostly prepared by two methods. The solvent-based sizing agent is made by dissolving the main resin with an organic solvent to make a sizing agent with a certain solid content. However, most organic solvents are volatile and pollute the environment, so there are few practical applications; emulsion Type sizing agent is made of polymer film former, surfactant and water as the main materials, assisted by high-shear emulsifier, and prepared by inverse emulsification method
Emulsion-type sizing agents hardly use organic solvents in the preparation process, so they can effectively avoid the shortcomings of solvent-type sizing agents. However, the emulsion particle size of emulsion-type sizing agents is affected by the type of emulsifier, the amount of emulsifier, emulsification temperature, emulsification time, Influenced by many factors such as mechanical stirring speed, a large number of formulation tests are required to prepare emulsions with excellent performance, and there are many parameters to be considered in the preparation process, which are difficult to control

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0026] 1) Weigh 1g of graphene oxide, 1g of dopamine and 1000mL of deionized water and stir for 40min under ultrasonic conditions, then centrifuge at a speed of 6000r / min for 30min, and finally take the upper liquid to obtain a graphene oxide aqueous solution.

[0027] 2) Weigh 118g (1mol) N,N,N',N'-tetraglycidyl-4,4'-diaminodiphenylmethane (AG-80), 32g (0.3mol) diethanolamine and 17g propylene glycol methyl Ether, the reactant was reacted at 80°C for 90min, then lowered the reaction temperature to 60°C, added 18g (0.3mol) acetic acid and continued to react for 30min, after the reaction was completed, cooled to room temperature and added 300g of graphene oxide aqueous solution, stirred evenly to obtain A multifunctional epoxy-based water-soluble sizing agent for graphene oxide.

example 2

[0029] 1) Weigh 1 g of graphene oxide, 1 g of sodium alginate and 2000 mL of deionized water and stir for 30 min under ultrasonic conditions, then centrifuge at a speed of 5000 r / min for 40 min, and take the upper liquid to obtain a graphene oxide aqueous solution.

[0030] 2) Weigh 146g (1mol) of N,N,N',N'-tetraglycidyl-3,3'-diethyl-4,4'-diaminodiphenylmethane, 58g (0.5mol) of 6- Amino-1-hexanol and 50g propylene glycol methyl ether, the reactant reacted at 70°C for 120min, then added 30g (0.5mol) acetic acid, and reacted at a constant temperature of 50°C for 30min, after the reaction was completed, cooled to room temperature and added 267g graphene oxide aqueous solution, stirred The multifunctional epoxy resin-based water-soluble sizing agent containing graphene oxide can be obtained evenly.

example 3

[0032] 1) Weigh 1g of graphene oxide, 1g of tea polyphenols and 1000mL of deionized water and stir for 60min under ultrasonic conditions, then centrifuge at a speed of 9000r / min for 30min, and then take the upper liquid to obtain a graphene oxide aqueous solution.

[0033] 2) Weigh 104g (1mol) triglycidyl p-aminophenol and 33g (0.25mol) diisopropanolamine, react the reactant at 75°C for 100min, then add 12g (0.25mol) formic acid, and react at 55°C for 30min After the reaction is completed, cool to room temperature, and add 317g of graphene oxide aqueous solution dropwise under stirring conditions to obtain a multifunctional epoxy resin-based water-soluble sizing agent containing graphene oxide.

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PUM

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Abstract

The invention relates to a graphene oxide-containing poly-functional group epoxy resin-based water-soluble sizing agent and a preparation method thereof. The method comprises the following steps: 1) preparing a water-soluble poly-functional group epoxy resin and 2) preparing the poly-functional group epoxy resin-based water-soluble sizing agent. The graphene oxide-containing poly-functional group epoxy resin-based water-soluble sizing agent and the preparation method thereof disclosed by the invention have the advantages that a poly-functional group resin is used as a main resin adopted by the sizing agent; the sizing agent has high cross-linking density, high glass-transition temperature, excellent heat resistance and high thermal stability, is beneficial to the forming of a resin film with high thermal stability on the carbon fiber surface and is capable of improving the bonding strength between the carbon fiber and the substrate base; the preparation process is simple and the sizing agent is convenient for the large-scale production and is beneficial to the industrial application of the graphene and the derivative thereof; the production manufacturability, such as, collection property and abrasion resistance, of the carbon fiber subjected to the sizing treatment with the prepared sizing agent is improved; the monofilament breaking strength of the carbon fiber and the thermal properties and mechanical properties of the compound material thereof are all promoted.

Description

technical field [0001] The invention belongs to the fields of graphene nanocomposite materials and carbon fiber composite materials, and relates to a multifunctional epoxy resin-based water-soluble sizing agent for carbon fibers and a preparation method thereof, in particular to the preparation of a high-temperature-resistant water-soluble sizing agent modified by graphene oxide method. Background technique [0002] Carbon fiber has many outstanding properties, such as high specific strength, high specific modulus, light weight, high temperature resistance, corrosion resistance, fatigue resistance, wear resistance, etc. It is used in the form of main load-bearing structural parts and secondary load-bearing structural parts. Widely used in aerospace, transportation, construction, energy, medical, sports and other fields. However, carbon fiber is brittle and has a small elongation at break. It is also prone to single-filament breakage and fluffing due to mechanical friction d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D06M15/55D06M15/03D06M13/368D06M13/152D06M11/74C08G59/32C08G59/50D06M101/40
CPCC08G59/3218C08G59/3227C08G59/5006D06M11/74D06M13/152D06M13/368D06M15/03D06M15/55D06M2101/40
Inventor 杨程任志东邢悦郝思嘉戴圣龙
Owner 北京石墨烯技术研究院有限公司
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