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Coordination crosslinking type polyimide aerogel and preparation method thereof

A technology of coordination cross-linking and polyimide, which is applied in the field of materials, can solve the problems of large shrinkage, low airgel skeleton strength, and affecting the quality of polyimide airgel products, so as to improve quality and equipment requirements Low, reduced size shrinkage effect

Active Publication Date: 2020-08-25
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the greater flexibility of polyamic acid molecular chains, the strength of its airgel skeleton is low, resulting in a large shrinkage of polyamic acid airgel size, which seriously affects the quality of polyimide airgel products.

Method used

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  • Coordination crosslinking type polyimide aerogel and preparation method thereof
  • Coordination crosslinking type polyimide aerogel and preparation method thereof

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preparation example Construction

[0025] A kind of preparation method of coordination cross-linked polyimide airgel of the present invention, specifically comprises the following steps:

[0026] First, diamine monomers, dianhydride monomers, tertiary amines, and alkyl ammonium halides are reacted in an aqueous solution to prepare polyamic acid hydrogels.

[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 monomer, tertiary amine, and alkyl ammonium halide in a single-necked flask with a magnet, add deionized water, stir at room temperature or in an ice-water bath until a uniform solution is formed, and then add the dianhydride monomer , stirred at room temperature or in an ice-water bath for 24 to 48 hours to form a viscous liquid, that is, polyamic acid hydrogel.

[0028] Secondly, the metal salt compound is added into the polyamic acid hydro...

Embodiment 1

[0040] Preparation of coordination cross-linked polyimide airgel: first, 2.00g 4,4'-diaminodiphenyl ether (ODA), 0.1mL triethylamine, 0.1g dodecyltrimethyl chloride Ammonium chloride was added to 50 mL of deionized water, stirred under ice-water bath conditions until a uniform solution was formed, and 2.18 g of pyromellitic anhydride (PMDA) was added to continue stirring for 24 hours to obtain a viscous liquid, namely polyamic acid hydrogel; Add 0.21g of copper sulfate pentahydrate to the polyamic acid hydrogel to make it all dissolve and disperse evenly, then gradually reduce the stirring rate, then pour the hydrogel into the mold, and vacuum degassing and refrigerating for 48 hours to obtain the coordination Cross-linked polyamic acid hydrogel; finally, the coordination cross-linked polyamic acid hydrogel was freeze-dried to obtain the coordination cross-linked polyamic acid airgel, and the coordination cross-linked polyamic acid airgel was obtained by heat imidization treatm...

Embodiment 2

[0042] Preparation of coordination cross-linked polyimide airgel: first, 1.90g 4,4'-diaminodiphenyl ether (ODA), 0.1mL triethylamine, 0.1g dodecyltrimethyl chloride Ammonium chloride was added to 50 mL of deionized water, stirred under ice-water bath conditions until a uniform solution was formed, and 2.18 g of pyromellitic anhydride (PMDA) was added to continue stirring for 24 hours to obtain a viscous liquid, namely polyamic acid hydrogel; Add 0.21g of copper sulfate pentahydrate to the polyamic acid hydrogel to make it all dissolve and disperse evenly, then gradually reduce the stirring rate, then pour the hydrogel into the mold, and vacuum degassing and refrigerating for 48 hours to obtain the coordination Cross-linked polyamic acid hydrogel; finally, the coordination cross-linked polyamic acid hydrogel was freeze-dried to obtain the coordination cross-linked polyamic acid airgel, and the coordination cross-linked polyamic acid airgel was obtained by heat imidization treatm...

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Abstract

The invention discloses coordination crosslinking type polyimide aerogel and a preparation method thereof, and belongs to the technical field of materials. According to the invention, the polyamide acid hydrogel is prepared under the action of the auxiliary agent and the surfactant in an aqueous solution system; the method then includes introducing metal ions to coordinate and crosslink the polyamic acid hydrogel to prepare coordination crosslinking type polyamic acid hydrogel; then carrying out freeze drying and thermal imidization to obtain coordination cross-linking type polyimide aerogel;the method has the advantages of being simple, efficient, low in equipment requirement, wide in application range and environmentally friendly; the problem that traditional polyimide high-performanceaerogel is difficult to prepare can be effectively avoided, and the obtained aerogel can be used for gas adsorption, organic matter adsorption, heat insulation materials and the like and has high potential application value in the fields of air pollution treatment, water pollution treatment, heat insulation 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 coordination cross-linked polyimide airgel and a preparation method thereof. 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, dielect...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J9/28C08J3/24C08L79/08C08G73/10
CPCC08J9/28C08J3/243C08G73/1071C08G73/1078C08G73/1039C08G73/1028C08G73/1007C08G73/105C08J2201/0484C08J2379/08Y02P20/54
Inventor 卓龙海谢璠蔡亚玲陈珊珊沈东
Owner SHAANXI UNIV OF SCI & TECH
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