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Preparation method of graphene/polymer nano composite material

A nanocomposite material and graphene technology, which is applied in the field of preparation of graphene/polymer nanocomposite materials, can solve problems such as unfavorable graphene dispersion, and achieve the effects of low cost, simple preparation process and excellent electrical conductivity

Active Publication Date: 2011-08-24
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in this traditional emulsion blending method, graphene oxide will inevitably re-agglomerate after being reduced to graphene, which is not conducive to the dispersion of graphene.

Method used

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  • Preparation method of graphene/polymer nano composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Disperse 0.1g of graphite oxide in 100g of water with a power of 50W and a frequency of 10Hz for 5 hours at a temperature of 10°C to obtain an aqueous solution of graphene oxide, and then add the aqueous solution of graphene oxide to natural latex containing 100g of natural rubber. After mixing evenly, add 5g of sodium sulfate solution with a concentration of 5% to break the emulsion to obtain a graphene oxide / natural rubber particle suspension, add 0.1g of hydrazine hydrate to reduce the graphene oxide, and reduce at a temperature of 100°C for 2 hours. After filtering, the product was dried in an oven at a temperature of 60° C. for 48 hours to obtain a graphene / natural rubber nanocomposite material. The composite material is formed by traditional rubber vulcanization method, and the gas permeability of the obtained sheet is reduced by 46%.

Embodiment 2

[0031] 0.5g of graphite oxide is mechanically ground in 200g of water for 1 hour to obtain an aqueous solution of graphene oxide, and the aqueous solution of graphene oxide is added to the natural rubber latex containing 100g of natural rubber. After mixing evenly, add sodium chloride and chlorine with a concentration of 25%. 10g of potassium chloride mixed solution was demulsified to obtain a suspension of graphene oxide / natural rubber particles, and 1g of sodium borohydride was added to pre-reduce graphene oxide, and the temperature was reduced at 20°C for 2 hours, then 3g of hydrazine hydrate was added, and at a temperature of 100°C, After reduction for 24 hours, the product was filtered and dried in a vacuum oven with a vacuum degree of 0.01 MPa and a temperature of 60° C. for 48 hours to obtain a graphene / natural rubber nanocomposite material. The composite material is molded by a traditional rubber vulcanization method, and the tensile strength of the prepared sheet is 24...

Embodiment 3

[0033]Disperse 7g of graphite oxide in 400g of water, using ultrasound with a power of 100W and a frequency of 10000Hz, at a temperature of 80°C for 15 minutes to obtain an aqueous solution of graphene oxide. Add the aqueous solution of graphene oxide to the latex containing 100g of styrene-butadiene rubber, and mix well Finally, add 100 g of magnesium chloride solution with a concentration of 15% to break the emulsion, obtain a suspension of graphene oxide / styrene-butadiene rubber particles, add 10 g of dimethylhydrazine to reduce graphene oxide, and reduce it for 24 hours at a temperature of 90 ° C. After filtering, the product is in The degree of vacuum is 0.1 MPa, and the temperature is 70° C. in a vacuum oven for 24 hours to obtain a graphene / styrene-butadiene rubber nanocomposite material. The composite is molded using conventional rubber vulcanization methods.

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Abstract

The invention discloses a preparation method of a graphene / polymer nano composite material, which is characterized by comprising the following steps: adding 0.1-30 parts by weight of graphite oxide into 10-3000 parts by weight of water, and dispersing and exfoliating by carrying out ultrasonic dispersion (the power is 50-500W, and the frequency is 10-100000Hz) at 10-100 DEG C for 15 minutes-5 hours or mechanical lapping for 15 minutes-5 hours or mechanical stirring for 1-48 hours to obtain a graphene oxide water solution; adding the graphene oxide water solution into 100 parts by weight of polymer emulsion of which the solid content is 10-70%; continuing the ultrasonic or mechanical stirring to carry out uniform mixing; demulsifying by adding 1-100 parts by weight of 5-100% demulsifier toobtain a graphene oxide / polymer granular suspension; adding 0.1-100 parts by weight of reducer into the graphene oxide / polymer granular suspension, reducing at 20-100 DEG C for 1-72 hours, filtering,and drying in a drying oven at 20-100 DEG C for 2-72 hours or drying in a vacuum drying oven at 20-120 DEG C under a vacuum degree of 0.1-0.01 MPa for 2-48 hours, thereby obtaining the graphene / polymer nano composite material.

Description

Technical field [0001] The invention relates to a preparation method of graphene / polymer nanocomposite materials and belongs to the field of preparation of polymer nanocomposite materials. Background technique [0002] In 2004, British scientists Novoselov and Geim discovered the 2 Two-dimensional honeycomb single-atom layer crystal connected by hybrid carbon atoms - graphene (K.S. Novoselov, A.K. Geim, S.V. Morozov, et al. Science, 2004, 306, 666-669). Graphene has a large specific surface area, excellent mechanical properties, conductive properties and barrier properties, and is an ideal nanofiller for polymers. At present, the main methods for preparing graphene / polymer nanocomposites are: solution blending method, mechanical blending method and in-situ polymerization method. Stankovich et al. used a solution blending method to prepare graphene / styrene nanocomposites with low conductive percolation value and high conductivity (S. Stankovich, D.A. Dikin, G.H.B. Dommett, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L7/00C08L9/06C08L55/02C08L53/02C08L9/02C08L31/04C08L75/04C08L33/08C08L33/10C08L25/06C08L25/08C08K3/04H01B1/24C09K5/14H05K9/00C09K3/00
Inventor 吴锦荣黄光速李辉翁更生吴思多刘玉峰
Owner SICHUAN UNIV
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