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Reduction and modification method of graphite oxide and application of graphite oxide in modified epoxy resin

A technology of epoxy resin and modification method, which is applied in the field of preparation of nanocomposite materials, can solve the problem of inability to realize long-term stable storage of graphene/epoxy resin, weak interfacial bonding force between graphene and epoxy resin composite materials, and unfavorable graphene Composite with epoxy resin and other issues to achieve the effect of convenient and fast transportation and storage, uniform and controllable content, and effective dispersion

Active Publication Date: 2019-03-08
QUANGANG PETROCHEM RES INST OF FUJIAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above process has the following deficiencies: 1) It is not conducive to the compounding of higher concentration graphene and epoxy resin, 2) The added dispersion liquid may cause adverse effects on the epoxy resin matrix, 3) It does not effectively treat the graphene surface. The surface modification of the surface does not solve the problem of weak interfacial bonding between graphene and epoxy resin composites
However, due to the modification of the amine group on the surface of graphene oxide, the long-term stable storage of the modified graphene / epoxy resin cannot be achieved.

Method used

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  • Reduction and modification method of graphite oxide and application of graphite oxide in modified epoxy resin
  • Reduction and modification method of graphite oxide and application of graphite oxide in modified epoxy resin
  • Reduction and modification method of graphite oxide and application of graphite oxide in modified epoxy resin

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Experimental program
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Effect test

Embodiment 1

[0025] Dissolve the acetylation reagent composed of 6.12 g of acetic anhydride and 14.2 g of pyridine, and 18.8 g of urushiol in 30 mL of xylene, heat up to 80-100 ° C for 4 hours, cool to room temperature, add 0.1 mol / L NaOH aqueous solution to wash, To pH = 7, liquid separation, removal of the water layer, to obtain the product acetylated urushiol. Dissolve 17.8g of acetylated urushiol, 23g of E44 epoxy resin and 0.2g of N,N-dimethylbenzylamine in 30mL of xylene, heat up to 50°C, stir, react for 6h, add 1mol / L NaOH ethanol solution, react at 50°C for 3h, and cool to room temperature to obtain the crude product. Wash with aqueous solution until pH = 7, remove the water layer, take the organic phase and rotary evaporate, remove excess epoxy resin, and obtain the product urushiol epoxy resin. The obtained urushiol epoxy resin and the graphene oxide prepared by the Hummer method were respectively dissolved and dispersed in N,N-dimethylformamide (DMF) solvent to prepare urushio...

Embodiment 2

[0030]Dissolve the acetylation reagent composed of 6.12 g of acetic anhydride and 14.2 g of pyridine, and 18.8 g of urushiol in 30 mL of toluene, heat up to 80-100 ° C for 4 h, cool to room temperature, add 0.1 mol / L NaOH aqueous solution to wash, until pH=7, liquid separation, removal of the water layer to obtain the product acetylated urushiol. Dissolve the obtained 17.8g of acetylated urushiol, 23g of ethylene glycol diglycidyl ether and 0.2g of benzyltriethylammonium chloride in 30mL of toluene, raise the temperature to 50°C, stir, react for 6h, and add 1M NaOH ethanol solution , 50 ° C reaction for 3h, cooled to room temperature to obtain a crude product. Wash with aqueous solution until pH = 7, remove the water layer, take the organic phase and rotary evaporate, remove excess epoxy resin, and obtain the product urushiol epoxy resin. The obtained urushiol epoxy resin and the graphene oxide prepared by the Hummer method were respectively dissolved and dispersed in N,N-dim...

Embodiment 3

[0032] Dissolve the acetylation reagent composed of 6.12 g of acetic anhydride and 14.2 g of pyridine, and 18.8 g of urushiol in 30 mL of toluene, heat up to 80-100 ° C for 4 h, cool to room temperature, add 0.1 mol / L NaOH aqueous solution to wash, until pH=7, liquid separation, removal of the water layer to obtain the product acetylated urushiol. Dissolve 17.8g of acetylated urushiol, 23g of E51 epoxy resin and 0.2g of benzyltriethylammonium chloride in 30mL of toluene, heat up to 50°C, stir, react for 6h, add 1M NaOH ethanol solution , 50 ° C reaction for 3h, cooled to room temperature to obtain a crude product. Wash with aqueous solution until pH = 7, remove the water layer, take the organic phase and rotary evaporate, remove excess epoxy resin, and obtain the product urushiol epoxy resin. The obtained urushiol epoxy resin and the graphene oxide prepared by the Hummer method were respectively dissolved and dispersed in N,N-dimethylformamide (DMF) solvent to prepare urushio...

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Abstract

The invention discloses a reduction and modification method of graphite oxide and an application of graphite oxide in modified epoxy resin. The method comprises the steps of allowing a Chinese lacquertree extract urushiol and an epoxy compound to give a ring-opening reaction in an organic solvent to form a urushiol glycidyl ether reaction intermediate with a phenolic hydroxyl group, reducing thegraphite oxide by taking the urushiol glycidyl ether reaction intermediate as a reducer to form graphene that has many long carbon chains, carbon-carbon double bonds and epoxy groups on the surface and shows good dispersity in the organic solvent, and mixing the prepared graphene and epoxy resin according to a certain proportion to form the graphene modified epoxy resin. The graphene prepared by the method can be quickly and uniformly dispersed in various epoxy resins; compatibility and an interface binding force between the graphene and the epoxy resin are effectively improved; long-term andstable storage of the modified graphene / epoxy resin can be achieved; and the convenience is provided for subsequent preparation of a graphene-based epoxy resin composite.

Description

technical field [0001] The invention belongs to the field of preparation of nanocomposite materials, and in particular relates to a reduction and modification method of graphene oxide and its application in modified epoxy resin. Background technique [0002] Epoxy resin generally refers to organic polymer compounds containing two or more epoxy groups in the molecule, and is an important class of thermosetting plastics. The cured epoxy resin has good physical and chemical properties, and can be used as adhesives, coatings, and composite materials in various fields of national economy such as electronics, chemical anticorrosion, automobiles, construction, and aerospace. However, pure epoxy resin has a large degree of crosslinking, poor impact damage resistance, poor toughness, and brittle quality. Especially when used as a coating, the solvent volatilizes during the curing process to form many micropores inside the coating, which reduces the corrosion resistance of the coatin...

Claims

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Application Information

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IPC IPC(8): C08K9/04C08K3/04C08L63/00
CPCC08K9/08C08L63/00C08K3/042
Inventor 郑雪琳杨俊威朱虎陈登龙刘成峰
Owner QUANGANG PETROCHEM RES INST OF FUJIAN NORMAL UNIV
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