A kind of preparation method of reduced graphene and polyimide nanocomposite material

A nanocomposite material and polyimide technology, which is applied in the field of preparation of reduced graphene and polyimide nanocomposite materials, can solve the problems of low temperature resistance, poor dispersion stability, and graphene oxide re-agglomeration, etc. The process is simple and reliable, the effect of improving dispersion stability and overcoming adverse effects

Active Publication Date: 2016-01-27
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Abstract
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  • Application Information

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Problems solved by technology

However, the dispersion stability of graphene oxide in polar organic solvents is poor, and graphene oxide re-agglomeration occurs during the polymerization process, which limits the degree of dispersion of graphene in the polyimide matrix.
In addition, the method of chemically modifying graphene oxide (such as: CN20110100930) can significantly increase the dispersion stability of graphene oxide in polar solvents, but the temperature resistance of various modifying agents used is significantly lower than that of polyimide oxide. The amine itself has an adverse effect on the temperature resistance of the composite material

Method used

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  • A kind of preparation method of reduced graphene and polyimide nanocomposite material
  • A kind of preparation method of reduced graphene and polyimide nanocomposite material

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Effect test

Embodiment 1

[0025] Add 5.0 g of graphene oxide into 1 L of deionized water, and use an ultrasonic generator to ultrasonically disperse for 180 min at an ultrasonic power of 150 W and room temperature to prepare an aqueous graphene oxide dispersion with a concentration of 5 mg / ml for future use.

[0026] Weigh 200.24g of 4,4'-diaminodiphenyl ether and 218.12g of pyromellitic dianhydride, add it to 1.77L of N,N'-dimethylformamide, and place it at 25°C under nitrogen protection The reaction was stirred for 24 hours under the conditions to obtain a polyamic acid solution. 306.64 ml of triethylamine was added to the solution, and the reaction was continued for 1 h to obtain a hydrophilic polyamic acid solution. Next, under the condition of stirring, 1L of the prepared aqueous graphene oxide dispersion was added to the hydrophilic solution, and stirred for 60 minutes to realize the uniform dispersion of graphene oxide in the polyamic acid. The above solution was filmed by a spin coating mechan...

Embodiment 2

[0028] Add 0.52 g of graphene oxide into 260 ml of deionized water, and use an ultrasonic generator to ultrasonically disperse for 60 min at an ultrasonic power of 100 W and room temperature to prepare an aqueous graphene oxide dispersion with a concentration of 2 mg / ml for future use.

[0029] Weigh 32.22g of 3,3',4,4'-benzophenonetetracarboxylic dianhydride and 20.02g of 3,3'-diaminodiphenyl ether, add to 300ml of N,N' - In dimethylformamide, stirring and reacting for 2 hours at 0° C. under the protection of argon to synthesize a polyamic acid solution. 30.67ml of triethylamine was added to the solution, and the reaction was continued for 0.5h to obtain a hydrophilic polyamic acid solution. Then, under the condition of stirring, the aqueous graphene oxide dispersion liquid prepared above was added to the hydrophilic solution, and stirred for 30 minutes to realize the uniform dispersion of graphene oxide in the polyamic acid. Take 100ml of the above solution to coat a film o...

Embodiment 3

[0031] Add 0.03 g of graphene oxide into 60 ml of deionized water, and use an ultrasonic generator to ultrasonically disperse for 120 min at an ultrasonic power of 120 W and room temperature to prepare an aqueous graphene oxide dispersion with a concentration of 0.5 mg / ml for future use.

[0032] Weigh 5.02g of bisphenol A dianhydride and 1.08g of m-phenylenediamine, and add them to 50ml of N,N'-dimethylformamide under stirring conditions. The reaction was stirred for 6 hours to synthesize a polyamic acid solution. 1.15 ml of tributylamine was added to the solution, and the reaction was continued for 1 h to obtain a hydrophilic polyamic acid solution. Then, under the condition of stirring, the above-mentioned aqueous graphene oxide dispersion liquid was added to the hydrophilic solution, and stirred for 45 minutes to realize the uniform dispersion of graphene oxide in the polyamic acid. The above solution was coated on a film, and dried under vacuum at 70° C. to obtain a grap...

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Abstract

The invention relates to a preparation method of a reduced graphene and polyimide nano composite material. The preparation method comprises the following steps: firstly performing ultrasonic dispersion on oxidized graphene in deionized water by adopting a solution mixing method to prepare an oxidized graphene waterborne suspension with high dispersion and stability; then directly mixing a polyamic acid solution subjected to neutralization with the oxidized graphene waterborne suspension to realize the high dispersion of the oxidized graphene in polyamic acid; and finally performing and synchronous thermal reduction on the oxidized graphene through thermal imidization to prepare the reduced graphene and polyimide nano composite material. The preparation method provided by the invention has the advantages of good reduced graphene dispersion and good thermal stability.

Description

technical field [0001] The invention belongs to a nanocomposite material, in particular to a preparation method of a reduced graphene and polyimide nanocomposite material. Background technique [0002] Polyimide has high temperature resistance, high mechanical properties and excellent chemical stability, and is widely used in aerospace, electronic devices and automotive industries. However, with the continuous development of modern civilization, the performance requirements of polyimide in various industries are constantly increasing, and pure polyimide resin can no longer meet people's application needs. In this context, the polyimide resin modified by nanomaterials, that is, polyimide nanocomposites, has gradually come into people's sight and has become a reliable method to improve and expand the performance of polyimide. [0003] Graphene, a novel monoatomic layer-thick carbon material, has become one of the most attractive reinforcement materials in nanocomposites due t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L79/08C08K9/00C08K3/04C08G73/10C08J5/18
CPCC08G73/1007C08J5/18C08J2379/08C08K3/04C08K9/00C08L2203/16C08L79/08
Inventor 吕春祥张寿春原浩杰安锋
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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