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Preparation method of graphene modified epoxy resin

A graphene modification and epoxy resin technology, applied in the field of resin materials, can solve the problems of graphene being difficult to disperse, poor dispersibility, and prone to agglomeration of graphene, so as to reduce solvent adsorption, improve tensile strength, and avoid the effect of reunion

Active Publication Date: 2016-08-10
SHANDONG OBO NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still many problems in the composite process in the existing actual production process. In the prior art, graphene and epoxy resin are usually composited by a blending method, and graphene has poor dispersion in the epoxy resin matrix by direct blending. Good, and graphene is prone to agglomeration
The solution blending method of graphene is also difficult to fully and uniformly disperse, and the solvent is difficult to remove due to the strong adsorption of graphene.
Both methods will introduce defects after the epoxy resin is cured, which will affect the strengthening effect of graphene, and then lead to the performance of the graphene epoxy resin composite material is not ideal enough to meet the application requirements in various fields, which limits the promotion and application of composite materials. develop

Method used

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preparation example Construction

[0031] The invention provides a kind of preparation method of graphene modified epoxy resin, comprises the following steps:

[0032] A) After mixing the graphene aqueous solution, bisphenol A and epichlorohydrin, a mixed solution is obtained;

[0033] B) After adding an initiator to the mixed solution obtained in the above steps for reaction, a graphene-modified epoxy resin is obtained.

[0034] In the present invention, firstly, the graphene aqueous solution, bisphenol A and epichlorohydrin are mixed to obtain a mixed solution. In the present invention, the source of the graphene aqueous solution is not particularly limited, it can be prepared by a method well known to those skilled in the art or purchased from the market, and the present invention is preferably prepared by a conventional method. The present invention has no special limitation to the concentration of described graphene aqueous solution, those skilled in the art can select and adjust according to actual produ...

Embodiment 1

[0048] Add bisphenol A and epichlorohydrin into the four-necked flask at a molar ratio of 1:10, and set up the device. Heat the reactant in a water bath to 75°C and stir. After the bisphenol A is completely dissolved, add a graphene aqueous solution with a concentration of 5‰ (the mass ratio of bisphenol A to graphene is 100:1), and stir and reflux for 30 minutes.

[0049] Then prepare a NaOH solution with a mass concentration of 28.6%, and the molar ratio of NaOH to epichlorohydrin is 1.1:1.

[0050] Then lower the temperature to 70°C, slowly add one-tenth of the NaOH solution dropwise, and strictly control the rate of addition.

[0051] Then stop dropping the lye, raise the temperature of the water bath to 80°C, and continue the reaction for 1.5 hours, then add the remaining lye dropwise, about 2.5 hours after the drop, and continue the reaction for 1.5 hours after the drop.

[0052] After the reaction is complete, add distilled water at 65°C in an amount of about 1 / 3 of th...

Embodiment 2

[0056] Add bisphenol A and epichlorohydrin into the four-necked flask at a molar ratio of 1:10, and set up the device. Heat the reactant in a water bath to 75°C and stir. After the bisphenol A is completely dissolved, add a graphene aqueous solution with a concentration of 5‰ (the mass ratio of bisphenol A to graphene is 50:1), and stir and reflux for 30 minutes.

[0057] Then prepare a NaOH solution with a mass concentration of 28.6%, and the molar ratio of NaOH to epichlorohydrin is 1.1:1.

[0058] Then lower the temperature to 70°C, slowly add one-tenth of the NaOH solution dropwise, and strictly control the rate of addition.

[0059] Then stop dropping the lye, raise the temperature of the water bath to 80°C, and continue the reaction for 1.5 hours, then add the remaining lye dropwise, about 2.5 hours after the drop, and continue the reaction for 1.5 hours after the drop.

[0060] After the reaction is complete, add distilled water at 65°C in an amount of about 1 / 3 of the...

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Abstract

The invention provides a preparation method of graphene modified epoxy resin. The preparation method comprises the following steps: first mixing a graphene aqueous solution, bisphenol A and epichlorohydrin to obtain a mixed solution; adding an initiator into the mixed solution obtained in the step, and performing the reaction to obtain the graphene modified epoxy resin. By utilizing an in-situ polymerization method, graphene is added at an initial synthetic phase, the surface of the graphene adsorbs epoxy resin molecules, sufficient and uniform dispersion can be realized in an epoxy resin matrix, the agglomeration phenomenon is avoided, and hole and solvent adsorption are reduced, so that the defects after the solidification are reduced, the reinforcing effect of the graphene is maximally realized, and the defects in the prior art that the graphene is easy to agglomerate and poor in compatibility when a graphene / epoxy resin composite material is prepared through a way of directly blending or solution blending graphene and epoxy resin can be effectively overcome.

Description

technical field [0001] The invention belongs to the technical field of resin materials, in particular to a preparation method of graphene-modified epoxy resin. Background technique [0002] Epoxy resin generally refers to organic compounds containing two or more epoxy groups in the molecule. Due to the active epoxy groups in the molecular structure, it can be cross-linked with various types of curing agents to form an insoluble three-dimensional network. structure. The cured epoxy resin has good physical and chemical properties, it has excellent bonding strength to the surface of metal and non-metal materials, good dielectric properties, small deformation shrinkage, good dimensional stability of products, high hardness, flexibility It has good resistance and is stable to alkali and most solvents, so it is widely used in various sectors of national defense and national economy for pouring, impregnation, lamination, adhesives and coatings. However, pure epoxy resin is relati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/06C08K3/04
CPCC08G59/063C08K3/04C08K2201/011
Inventor 刘海波张在忠赵新新
Owner SHANDONG OBO NEW MATERIAL CO LTD
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