A kind of modified graphene/thermosetting resin composite material and preparation method thereof

Abstract

The invention discloses a modified grapheme / thermosetting resin composite material and a preparation method thereof. The preparation method comprises the following steps: adding a hydrochloric acid doped polyaniline modified carbon nano tube to oxidized grapheme aqueous dispersion, filtering, washing and drying the reactant to obtain the modified grapheme, uniformly mixing the modified grapheme with molten resin capable of thermosetting, and solidifying the mixture, so as to obtain the modified grapheme / thermosetting resin composite material. The modified grapheme provided has a micro capacitance structure; the hydrochloric acid doped polyaniline modified carbon nano tube is loaded on the surface of the grapheme through Pi to Pi conjugation; the excellent electrical property of the grapheme is maintained; the lamellas of the grapheme are prevented from mutually contacting; the obtained modified grapheme / thermosetting resin composite material has the advantages of high dielectric constant, low dielectric loss, and low percolation threshold, and can realize control on the dielectric property of the composite material by adjusting the variation of the content of the hydrochloric acid doped polyaniline modified carbon nano tube coated on the surface of the grapheme.

Description

technical field

[0001] The invention relates to a composite material and a preparation method thereof, in particular to a modified graphene / thermosetting resin composite material and a preparation method thereof. Background technique

[0002] High dielectric constant and low dielectric loss composite materials are important functional materials at present, and have great application value in electronics, aerospace, biomedicine and other fields. Graphene as a two-dimensional structure has huge electron mobility and large specific surface area, and is often used as a reinforcement for high-performance polymer-based composites. Graphene / polymer-based composite materials are an important type of high dielectric constant materials. In recent years, scholars at home and abroad have conducted a lot of research on graphene / polymer-based composite materials. Modification of graphene can effectively solve its agglomeration problem and improve the dielectric properties of composite ma...

Examples

Embodiment 1

[0028] 1. Preparation of hydrochloric acid-doped polyaniline-modified carbon nanotubes

[0029] in N 2 Under protection, at 0-5°C, disperse 1g of multi-walled carbon nanotubes into 500mL of deionized water, add 0.99g of sodium dodecyl sulfate, and mix for 0.5h under stirring; then add 0.4g of aniline, and Add 100mL hydrochloric acid solution (0.043mol / L), and mix well under stirring conditions for 1h; slowly add 100mL ammonium persulfate solution (0.043mol / L) dropwise, after the dropwise addition, react for 6h, after the reaction, filter and wash , and dry to obtain polyaniline-modified carbon nanotubes. The infrared spectrogram, Raman spectrogram, X-ray diffraction pattern, scanning electron microscope pattern and electrical conductivity at 1 Hz of the prepared hydrochloric acid-doped polyaniline-modified carbon nanotubes are shown in the appendix respectively. figure 1 , 2 , 3, 4 and 5.

[0030] 2. Preparation of graphite oxide

[0031] Take 2g of graphite, 1g of sodium...

Embodiment 2

[0041] 1. Preparation of modified graphene

[0042] Weigh 1 g of graphite oxide (provided in Example 1) and disperse it in 500 mL of deionized water, stir and sonicate for 1 hour to obtain a graphene oxide dispersion, add 0.50 g of hydrochloric acid doped polyaniline-modified carbon nanotubes (provided in Example 1) Put it into the graphene oxide dispersion, stir it ultrasonically, react at 60°C for 12h, then add 10g of L-ascorbic acid, raise the temperature of the reaction liquid to 80°C and react for 24h, soak in 500mL of 1mol / L ammonia water for 1h, After suction filtration, washing, and drying, a graphene-hydrochloric acid-doped polyaniline-modified carbon nanotube composite is obtained, wherein the mass of the hydrochloric acid-doped polyaniline-modified carbon nanotube is twice the mass of graphene. The X-ray diffraction figure of prepared graphene-modified graphene, the electrical conductivity under the scanning electron microscope picture, 1Hz are shown in the attached...

Embodiment 3

[0046] 1. Preparation of modified graphene

[0047] Weigh 1 g of graphite oxide (provided in Example 1) and disperse it in 500 mL of deionized water, stir and sonicate for 1 h to obtain a graphene oxide dispersion, add 1.0 g of hydrochloric acid-doped polyaniline-modified carbon nanotubes (Example 1) to In the graphene oxide dispersion, ultrasonically stirred, reacted at 60°C for 12h, then added 10g of L-ascorbic acid, raised the temperature of the reaction liquid to 80°C and reacted for 24h, soaked in 500mL of 1mol / L ammonia water for 1h, pumped After filtering, washing and drying, the modified graphene is obtained, wherein the quality of the hydrochloric acid-doped polyaniline-modified carbon nanotubes is twice that of the graphene. The X-ray diffraction pattern of prepared modified graphene, the scanning electron microscope pattern, the electrical conductivity under 1Hz are respectively shown in the appendix image 3 , 4 and 5.

[0048] 2. Preparation of modified graphen...

technical field

[0001] The invention relates to a composite material and a preparation method thereof, in particular to a modified graphene / thermosetting resin composite material and a preparation method thereof. Background technique

[0002] High dielectric constant and low dielectric loss composite materials are important functional materials at present, and have great application value in electronics, aerospace, biomedicine and other fields. Graphene as a two-dimensional structure has huge electron mobility and large specific surface area, and is often used as a reinforcement for high-performance polymer-based composites. Graphene / polymer-based composite materials are an important type of high dielectric constant materials. In recent years, scholars at home and abroad have conducted a lot of research on graphene / polymer-based composite materials. Modification of graphene can effectively solve its agglomeration problem and improve the dielectric properties of composite ma...

Examples

Embodiment 1

[0028] 1. Preparation of hydrochloric acid-doped polyaniline-modified carbon nanotubes

[0029] in N 2 Under protection, at 0-5°C, disperse 1g of multi-walled carbon nanotubes into 500mL of deionized water, add 0.99g of sodium dodecyl sulfate, and mix for 0.5h under stirring; then add 0.4g of aniline, and Add 100mL hydrochloric acid solution (0.043mol / L), and mix well under stirring conditions for 1h; slowly add 100mL ammonium persulfate solution (0.043mol / L) dropwise, after the dropwise addition, react for 6h, after the reaction, filter and wash , and dry to obtain polyaniline-modified carbon nanotubes. The infrared spectrogram, Raman spectrogram, X-ray diffraction pattern, scanning electron microscope pattern and electrical conductivity at 1 Hz of the prepared hydrochloric acid-doped polyaniline-modified carbon nanotubes are shown in the appendix respectively. figure 1 , 2 , 3, 4 and 5.

[0030] 2. Preparation of graphite oxide

[0031] Take 2g of graphite, 1g of sodium...

Embodiment 2

[0041] 1. Preparation of modified graphene

[0042] Weigh 1 g of graphite oxide (provided in Example 1) and disperse it in 500 mL of deionized water, stir and sonicate for 1 hour to obtain a graphene oxide dispersion, add 0.50 g of hydrochloric acid doped polyaniline-modified carbon nanotubes (provided in Example 1) Put it into the graphene oxide dispersion, stir it ultrasonically, react at 60°C for 12h, then add 10g of L-ascorbic acid, raise the temperature of the reaction liquid to 80°C and react for 24h, soak in 500mL of 1mol / L ammonia water for 1h, After suction filtration, washing, and drying, a graphene-hydrochloric acid-doped polyaniline-modified carbon nanotube composite is obtained, wherein the mass of the hydrochloric acid-doped polyaniline-modified carbon nanotube is twice the mass of graphene. The X-ray diffraction figure of prepared graphene-modified graphene, the electrical conductivity under the scanning electron microscope picture, 1Hz are shown in the attached...

Embodiment 3

[0046] 1. Preparation of modified graphene

[0047] Weigh 1 g of graphite oxide (provided in Example 1) and disperse it in 500 mL of deionized water, stir and sonicate for 1 h to obtain a graphene oxide dispersion, add 1.0 g of hydrochloric acid-doped polyaniline-modified carbon nanotubes (Example 1) to In the graphene oxide dispersion, ultrasonically stirred, reacted at 60°C for 12h, then added 10g of L-ascorbic acid, raised the temperature of the reaction liquid to 80°C and reacted for 24h, soaked in 500mL of 1mol / L ammonia water for 1h, pumped After filtering, washing and drying, the modified graphene is obtained, wherein the quality of the hydrochloric acid-doped polyaniline-modified carbon nanotubes is twice that of the graphene. The X-ray diffraction pattern of prepared modified graphene, the scanning electron microscope pattern, the electrical conductivity under 1Hz are respectively shown in the appendix image 3 , 4 and 5.

[0048] 2. Preparation of modified graphen...

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