Method for preparing graphene/polyimide composite aerogel

A composite aerogel and polyimide technology, applied in the field of materials, can solve the problems of complex preparation of graphene/polyimide aerogel, not meeting the requirements of green preparation, etc., and achieves a range of applications that are environmentally friendly and have low equipment requirements. , a wide range of effects

Pending Publication Date: 2019-12-20
SHAANXI UNIV OF SCI & TECH
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Problems solved by technology

[0004] In order to solve the problem that the preparation of graphene / polyimide airgel in the prior art is complicated and does not meet the requirements of green preparation, the present invention provides a graphene / polyimide airgel that is simple, efficient, low in equipment requirements, and widely applicable. The preparation method of imine composite airgel is to prepare polyamic acid aqueous solution mainly through quaternary ammonium salt cationic surfactant and tertiary amine, and then uniformly disperse graphene in polyamic acid aqueous solution to obtain graphene / polyamic acid The mixed solution was aged, freeze-dried, and thermally imidized to obtain graphene / polyimide composite airgel

Method used

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  • Method for preparing graphene/polyimide composite aerogel
  • Method for preparing graphene/polyimide composite aerogel

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preparation example Construction

[0025] A kind of preparation method of graphene / polyimide composite airgel of the present invention specifically comprises the following steps:

[0026] First, the diamine monomer is dissolved in deionized water under the action of tertiary amine and quaternary ammonium salt cationic surfactant to prepare diamine monomer aqueous solution; the addition mole of quaternary ammonium salt cationic surfactant and diamine monomer The ratio is (0.03~0.04):1, and the molar ratio of tertiary amine and diamine monomer is (0.05~0.08):1

[0027] The specific means are as follows: ultrasonically treat single-necked flasks, beakers, molds, magnets, etc. with absolute ethanol to remove surface impurities, and dry them for later use. Put the weighed diamine, tertiary amine, and quaternary ammonium salt cationic surfactant into a single-necked flask with a magnet, add deionized water, and stir until the diamine is completely dissolved to obtain an aqueous solution of diamine monomer;

[0028] ...

Embodiment 1

[0040] Preparation of graphene / polyamic acid composite airgel: First, 2.00g 4,4'-diaminodiphenyl ether (ODA), 0.08g dodecyltrimethylammonium chloride, 0.07mL triethylamine Dissolve in 50mL of deionized water, then add 2.18g of pyromellitic anhydride (PMDA) and stir to obtain an aqueous solution of polyamic acid; secondly, add 0.10g of graphene oxide to the aqueous solution of polyamic acid, and stir until a uniform solution is formed, that is, graphite alkene / polyamic acid aqueous solution; again, the graphene / polyamic acid aqueous solution is poured into the mold and then degassed, aged, frozen, and freeze-dried to obtain a graphene / polyamic acid composite airgel; finally, the thermal imidization The graphene / polyimide composite airgel is processed, and the thermal imidization process is: 120°C (0.5h) + 150°C (0.5h) + 200°C (1h) + 250°C (4h).

Embodiment 2

[0042] Preparation of graphene / polyamic acid composite airgel: First, 2.00g 4,4'-diaminodiphenyl ether (ODA), 0.08g dodecyltrimethylammonium chloride, 0.07mL triethylamine Dissolve in 50mL of deionized water, then add 2.18g of pyromellitic anhydride (PMDA) and stir to obtain an aqueous solution of polyamic acid; secondly, add 0.50g of graphene oxide to the aqueous solution of polyamic acid, and stir until a uniform solution is formed, that is, graphite alkene / polyamic acid aqueous solution; again, the graphene / polyamic acid aqueous solution is poured into the mold and then degassed, aged, frozen, and freeze-dried to obtain a graphene / polyamic acid composite airgel; finally, the thermal imidization The graphene / polyimide composite airgel is processed, and the thermal imidization process is: 120°C (0.5h) + 150°C (0.5h) + 200°C (1h) + 250°C (4h).

[0043] from figure 1 It can be seen that the graphene-enhanced polyimide airgel has good dimensional stability and is light in weigh...

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Abstract

The invention discloses a method for preparing graphene / polyimide composite aerogel and belongs to the technical field of materials. The method mainly comprises the steps of supplementarily preparinga polyamic acid aqueous solution through the assistance of a quaternary ammonium salt cationic surfactant and tertiary amine, then, uniformly dispersing graphene in the polyamic acid aqueous solutionso as to obtain a graphene / polyamic acid mixed solution, and carrying out aging, freeze drying and thermal imidization, thereby obtaining the graphene / polyimide composite aerogel. The method has the advantages of simplicity, high efficiency, low equipment requirements, wide applicable range, environment-friendliness and low cost, the problem that the traditional polyimide high-performance aerogelis difficult to prepare can be effectively avoided, and the obtained aerogel can be applied to gas adsorption, organic matter adsorption, heat-insulating materials and the like and has a very high potential application value in the fields of atmospheric pollution abatement, water pollution abatement, heat-insulating structural materials and the like.

Description

technical field [0001] The invention belongs to the technical field of materials, and relates to the preparation of polymer airgel, in particular to a preparation method of graphene / polyimide composite airgel. Background technique [0002] Airgel is a highly dispersed solid material, mainly composed of a nanoporous network structure filled with a gaseous dispersion medium in the pores obtained by the aggregation of colloidal particles (or polymer molecules). Three-dimensional porous nanomaterials in which the liquid component is replaced by a gas while still maintaining its gel network. The special continuous three-dimensional network structure makes airgel show unique properties in thermal, mechanical, acoustic, optical, electrical, etc. and other fields have received much attention. [0003] Polyimide refers to a class of polymers containing imide rings in the molecular main chain structural unit, which has outstanding thermo-oxidative stability, dielectric properties, e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J9/28C08L79/08C08K3/04C08G73/10
CPCC08G73/1071C08J9/28C08J2201/0484C08J2205/026C08J2379/08C08K3/042
Inventor 卓龙海谢璠蔡亚玲陈珊珊
Owner SHAANXI UNIV OF SCI & TECH
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