Preparation method of carbon nano-tube/epoxy resin composite material

A technology of carbon nanotubes and epoxy resin, which is applied in the field of preparation of carbon nanotubes/epoxy resin composite materials, can solve the problems of carbon nanotube surface defects lack of active groups, inability to disperse composite materials, and reduce mechanical properties of materials, etc. , to achieve the effect of improving surface functionalization efficiency, excellent mechanical properties and reducing surface energy

Inactive Publication Date: 2007-10-17
NANCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the few surface defects and the lack of active groups of carbon nanotubes, the solubility in various solvents is very low
In addition, there is a strong van der Waals attraction between carbon nanotubes, coupled with its huge specific surface area and high aspect ratio, making it easy to agglomerate or entangle, which seriously affects its application.
Traditional carbon nanotube / polymer composite materials adopt the method of physical filling or coating, that is, simple physical blending of carbon nanotubes and organic or inorganic materials, which improves the conductivity of the composite material to a certain extent, However, carbon nanotubes are easy to agglomerate and cannot be well dispersed in the composite material, causing defects inside the composite material, and sometimes even reducing the mechanical properties of the material, which seriously affects its application.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Take 5.0g primary carbon nanotubes, and set aside after jet milling;

[0021] (2) Mix the carbon nanotubes in step (1) with the concentrated nitric acid whose mass concentration is 68.0% according to the ratio of mass / volume ratio 1.0g / 50ml, after the mixture is ultrasonicated for 30min, stir and condense at 80°C for reflux for 24h, cool, Dilute with a large amount of deionized water, filter and wash the microporous membrane until neutral, vacuum dry the product at 90°C, and pulverize to obtain carboxylated carbon nanotubes;

[0022] (3) carbon nanotubes in step (2) and N, N '-dicyclohexyl carboximide, dimethylformamide and ethylenediamine are in weight / volume ratio: carbon nanotubes: N, N '-Dicyclohexylcarbodiimide: dimethylformamide: ethylenediamine = 1g: 4g: 20ml: 20g and mixed. Condensed and refluxed at 125°C for 24h. Cool, dilute with absolute ethanol, filter under reduced pressure with a microporous membrane, wash away residual impurities, dry in vacuum at 8...

Embodiment 2

[0032] (1) Take 5.0g primary carbon nanotubes, and set aside after jet milling;

[0033] (2) The carbon nanotubes in step (1) and the concentrated nitric acid whose mass concentration is 68.0% are mixed according to the ratio of mass / volume ratio 1.0g / 50ml, after the mixture is ultrasonicated for 30min, stirred and condensed at 75°C for reflux for 24h, cooled, Dilute with a large amount of deionized water, filter and wash the microporous membrane until neutral, vacuum dry the product at 90°C, and pulverize to obtain carboxylated carbon nanotubes;

[0034] (3) carbon nanotubes in step (2) and N, N'-carbonyldiimidazole, dimethylformamide and hexamethylenediamine in weight / volume ratio: carbon nanotubes: N, N'-carbonyldiimidazole Imidazole: dimethylformamide: hexamethylenediamine = 1g: 4g: 20ml: 30g were mixed. Condensed and refluxed at 125°C for 24h. Cool, dilute with absolute ethanol, filter under reduced pressure with a microporous membrane, wash away residual impurities, vacu...

Embodiment 3

[0040] (1) Take 5.0g primary carbon nanotubes, and set aside after jet milling;

[0041] (2) Mix the carbon nanotubes in step (1) and concentrated nitric acid with a mass concentration of 68.0% according to the ratio of mass / volume ratio 1.0g / 50ml, after the mixture is ultrasonicated for 0.5h, stir, condense and reflux at 75°C for 24h, and cool , diluted with a large amount of deionized water, the microporous membrane was vacuum-filtered and washed until neutral, and the product was vacuum-dried at 90°C and pulverized to obtain carboxylated carbon nanotubes;

[0042] (3) carbon nanotubes in step (2) and 4,5-dicyanoimidazole, dimethylformamide and diethylenetriamine are in weight / volume ratio: carbon nanotubes: 4,5-dicyanoimidazole imidazole: dimethylformamide: m-phenylenediamine = 1g: 4g: 20ml: 20g and mixed. Condensed and refluxed at 125°C for 24h. Cool, dilute with absolute ethanol, filter under reduced pressure with a microporous membrane, wash away residual impurities, d...

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Abstract

The invention discloses a producing method for carbon nano tube/epoxide resin compound material, including steps of: processing the native carbon in the flowing bed jet mill, carboxylation, introducing polyatomic alicyclic amine with a flexibility structure on the carbon nano tube surface. The carbon nano tube/epoxide resin compound material is produced by mixing the epoxide resin and carbon nano tube by hot melt method, high speed stirring, ultrasonic treatment, then adding aromatic amine for solidification moulding. The advantages of the invention is that grafting polyatomic alicyclic amine on the carbon nano tube surface improves the surface function efficiency of the carbon nano tube, reduces the surface energy of the carbon nano tube, decreases the self-aggregation of the carbon nano tube, promotes both affinity and achieves organic connection of the carbon nano tube and epoxide resin by resin chemical reaction. The invention has a simple craft, a qualified mechanical property of obtained compound material, and an ulterior industry application convenient for the carbon nano tube.

Description

technical field [0001] The invention relates to a preparation method of a carbon nanotube / epoxy resin composite material. Background technique [0002] Epoxy resin (EP) has been used abroad since the 1930s. After more than 60 years of development, the variety, quality and application of epoxy resin products have entered a mature stage. Epoxy resin contains a variety of polar groups and highly active epoxy groups, so it has strong adhesion to metals, glass, cement, wood, plastics and other polar materials, especially materials with high surface activity At the same time, the cohesive strength of the epoxy cured product is also very large, so its bonding strength is very high. When the epoxy resin is cured, basically no low-molecular volatiles are produced, and the volume shrinkage of the adhesive layer is small, about 1% to 2%, and can be reduced to less than 0.2% after adding fillers. It has good compatibility and reactivity with various organic sub...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L63/02C08K9/04C08K3/04C08K5/17
Inventor 黄德欢付继伟
Owner NANCHANG UNIV
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