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Method of improving dispersity and interface compatibility of graphene in epoxy resin

A technology of interface compatibility and epoxy resin, applied in the field of epoxy resin curing agent and epoxy resin composite material, can solve the problems of poor dispersion, poor interface compatibility between graphene and epoxy resin, etc., and achieve high stability , Improve the interface compatibility, the effect of simple and easy operation

Inactive Publication Date: 2017-05-31
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Technical problem solved: the present invention provides a method for improving the dispersion and interfacial compatibility of graphene in epoxy resin, which solves the problem of poor dispersion of graphene in epoxy resin matrix and the interfacial phase between graphene and epoxy resin. The problem of poor tolerance provides a general and effective method for the preparation of high-performance, multifunctional epoxy resin composites

Method used

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  • Method of improving dispersity and interface compatibility of graphene in epoxy resin
  • Method of improving dispersity and interface compatibility of graphene in epoxy resin
  • Method of improving dispersity and interface compatibility of graphene in epoxy resin

Examples

Experimental program
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Effect test

Embodiment 1

[0028] 0.02g graphene oxide and 3g dehydroabietic acid are dissolved in 200mL ethanol by stirring and ultrasonic dispersion (ultrasonic frequency is 80KHz, ultrasonic power is 300W, ultrasonic time is 0.5h), and then the co-solvent ethanol is removed by rotary evaporation to obtain Graphene oxide / dehydroabietic acid powder. The graphene oxide / dehydroabietic acid powder was placed in 50 mL of hydroiodic acid and reacted at 120°C for 48 hours to obtain graphene / dehydroabietic acid powder. Graphene / dehydroabietic acid powder and tetraethylenepentamine (the molar ratio of dehydroabietic acid and tetraethylenepentamine is 1:2) were reacted at 160°C for 2h and then reacted for 4h at 200°C, then the temperature was lowered to Add a certain amount of acrylonitrile (the molar ratio of dehydroabietic acid to acrylonitrile is 1:3) at 50°C for 2 hours to obtain a stable monolayer or oligolayer liquid graphene / rosin-based polyamine with an amine value of 350mgKOH / g. Such as image 3 show...

Embodiment 2

[0031]0.02g graphene oxide and 3g dehydroabietic acid are dissolved in 100ml acetone by stirring and ultrasonic dispersion (ultrasonic frequency is 80KHz, ultrasonic power is 120W, and ultrasonic time is 1.5h), and then the co-solvent acetone is removed by rotary evaporation to obtain Graphene oxide / dehydroabietic acid powder. The graphene oxide / dehydroabietic acid powder was placed in 100ml of hydroiodic acid and reacted at 100°C for 24 hours to obtain the graphene / dehydroabietic acid powder. Graphene / dehydroabietic acid powder was reacted with triethylenetetramine (the molar ratio of dehydroabietic acid to triethylenetetramine was 1:4) at 160°C for 2h and then at 200°C for 4h to obtain the amine value 850mgKOH / g, stable monolayer or multilayer liquid graphene / rosin-based polyamine.

[0032] Graphene / rosin-based polyamine and E51 type epoxy resin are mixed in a mass ratio of 1:4 and then cured to obtain a uniformly dispersed graphene / epoxy resin composite material, and 0.1wt...

Embodiment 3

[0034] 0.04g graphene oxide and 6g dehydroabietic acid are dissolved in 250ml dimethyl sulfoxide (DMSO) by stirring, ultrasonic dispersion (ultrasonic frequency is 80KHz, ultrasonic power is 150W, ultrasonic time is 1h), then by rotary evaporation The co-solvent DMSO was removed to obtain graphene oxide / dehydroabietic acid powder. The graphene oxide / dehydroabietic acid powder was placed in 100 ml of ascorbic acid aqueous solution at 100° C. for 48 hours to obtain graphene / dehydroabietic acid powder. Graphene / dehydroabietic acid powder was reacted with isophorone diamine (the molar ratio of dehydroabietic acid to isophorone diamine was 1:2) at 160°C for 2h and then at 200°C for 4h, A stable monolayer or multilayer liquid graphene / rosin-based polyamine with an amine value of 248 mgKOH / g was obtained.

[0035] Graphene / rosin-based polyamine and E51 type epoxy resin are mixed in a mass ratio of 1:1 and then cured to obtain a uniformly dispersed graphene / epoxy resin composite mate...

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Abstract

The invention relates to a method of improving dispersity and interface compatibility of graphene in epoxy resin. The method comprises the steps of performing stirring and ultrasonic dispersion on and dissolving graphite oxide and a disproportionated rosin purification product dehydroabietic acid in a cosolvent of graphite oxide and dehydroabietic acid at any ratio, evaporating a graphite oxide / dehydroabietic acid solution to remove the cosolvent to form graphite oxide / dehydroabietic acid powder, putting the graphite oxide / dehydroabietic acid powder in a graphite oxide reducer for reaction to form graphene / dehydroabietic acid powder, allowing the graphene / dehydroabietic acid powder to react with polyamine to form graphene / rosinyl polyamine, and mixing and curing graphene / rosinyl polyamine and the epoxy resin to form a uniform dispersion graphene / epoxy resin composite. The design method is novel; no surfactant is required to be used in a preparation process; the graphene is dispersed in the epoxy resin without a solvent; and the method is easy to operate and suitable for mass production.

Description

technical field [0001] The invention relates to the field of epoxy resin curing agent and epoxy resin composite material, in particular to a method for improving the dispersibility and interfacial compatibility of graphene in epoxy resin. Background technique [0002] With the gradual development of electronic products towards miniaturization, portability, high sensitivity, and high reliability, the traditional Pb / Sn solder can no longer meet the development requirements due to problems such as material deformation, internal stress, and serious environmental pollution caused by high-temperature welding. . Epoxy resin conductive composite materials have the advantages of high resolution, good environmental performance, simple processing procedures, and are suitable for large-scale production. They can meet the development requirements of electronic products and meet the requirements of sustainable development. They are ideal substitutes for highly polluting Pb / Sn solders , h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L63/00C08K9/04C08K3/04C08G59/50
CPCC08G59/502C08G59/5026C08K3/04C08K9/04C08L63/00
Inventor 黄金瑞聂小安胡芳芳王义刚李小英
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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