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Polyimide aerogel with crosslinked surface functionalized nanoparticles and preparation method thereof

A nanoparticle, surface functional technology, applied in the field of airgel and its preparation, to achieve the effects of good heat resistance, stable physical and chemical properties, and high specific surface area

Active Publication Date: 2017-07-28
BEIHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, in terms of the use of nanoparticles, these documents mentioned that the oxygen-containing functional groups such as carboxyl, carbonyl, epoxy, and hydroxyl groups present on the nanoparticles were used to cross-link polyamides, but did not apply to the nanoparticles. for efficient surface modification

Method used

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  • Polyimide aerogel with crosslinked surface functionalized nanoparticles and preparation method thereof
  • Polyimide aerogel with crosslinked surface functionalized nanoparticles and preparation method thereof
  • Polyimide aerogel with crosslinked surface functionalized nanoparticles and preparation method thereof

Examples

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Embodiment 1

[0044] The preparation of polyimide airgel cross-linked by aminated silver nanowires: disperse the silver nanowires in absolute ethanol solvent, add p-mercaptoaniline with a molar ratio of 4:1 to the silver in the silver wires, Carry out amination modification in ethanol solvent for 6h, then centrifuge, wash 5 times with absolute ethanol and dry for later use; dissolve 15mmol of diamine monomer 4,4-diaminodiphenyl ether in solvent N,N-dimethyl Add 15.3 mmol of dianhydride monomer 3,3',4,4'-biphenyltetracarboxylic dianhydride slowly to acetamide, fully dissolve and react at room temperature for 4 hours to obtain an anhydride-terminated polyamide with a degree of polymerization of about 50 acid, and adjust the solid content to 12% by changing the quality of the solvent. A certain amount of modified silver nanowires is added to the polyamic acid solution. Crosslink for 40 min at room temperature with mechanical stirring. Then add triethylamine and acetic anhydride with a molar ...

Embodiment 2

[0052] Preparation of functionalized mesoporous silica cross-linked polyimide airgel: prepare mesoporous silica microspheres by template method, under rapid magnetic stirring, mix 2.31ml dodecylamine, 0.1822g hexadecane Trimethylammonium bromide was added to the mixed solution of ethanol, isopropanol, deionized water and a small amount of ammonia water (ethanol: 131.01ml, ammonia water: 0.11ml, isopropanol 47.74ml, deionized water 67.5ml), and then Add tetraethyl orthosilicate quickly, keeping stirring slowly. 10 hours after the addition, the reaction solution was centrifuged and ultrasonically dispersed, washed with deionized water, and repeated 5 times to obtain a wet powder of silica microspheres, and then the powder was freeze-dried for 3 hours. Finally, the dried powder was calcined in a high-temperature furnace at 700K for 10 h to obtain mesoporous silica microspheres. Subsequently, the microspheres and aminopropyltriethoxysilane were refluxed at 110° C. for 5 h in a to...

Embodiment 3

[0054] Preparation of isocyanate-modified graphene oxide cross-linked polyimide airgel: ultrasonically disperse graphene oxide in N-methylpyrrolidone, and add it in a ratio of 6:1 to graphene oxide mass ratio Diphenylmethane diisocyanate. React at 40°C for 24 hours under a nitrogen atmosphere, replace the hydroxyl and carboxyl groups on the graphene oxide with isocyanate groups, and purify by centrifugation, washing and dialysis to obtain isocyanate group-modified graphene oxide. According to the same procedure as in Example 1, the graphene oxide modified by the isocyanate group was added to the same polyamic acid solution as in Example 1 at a mass fraction of 5% based on the polyamic acid precursor, according to Example 1 The procedure in is carried out cross-linking reaction, gelation and chemical imidization reaction, and finally polyimide airgel is obtained by supercritical drying. The compressive modulus of the obtained product airgel is 40% higher than that of the sampl...

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Abstract

The invention relates to polyimide aerogel and a preparation method thereof, and in particular relates to polyimide aerogel with crosslinked surface functionalized nanoparticles and a preparation method thereof. The preparation method of the aerogel comprises the following steps: functionalizing surfaces of the nanoparticles; synthesizing a polyamide acid precursor; preparing polyimide wet gel by adopting functionalized nanoparticles as a crosslinking agent; and carrying out supercritical drying, so that the crosslinked polyimide aerogel is obtained. The polyimide aerogel provided by the invention has a stable and narrowly distributed mesoporous structure and is large in specific surface area, good in heat resistance and stable in physicochemical properties, and different performance characteristics, including better toughness, rigidity, heat insulation property, dielectric property, conductivity, electromagnetic shielding property and the like, can be given to the aerogel, so that the polyimide aerogel can further serve as a polymer electrode material, an adsorption catalysis carrier, a porous thermal insulation material, an electromagnetic shielding material and the like.

Description

technical field [0001] The invention relates to an airgel and a preparation method thereof, in particular to a polyimide airgel crosslinked by surface functionalized nanoparticles and a preparation method thereof. Background technique [0002] Airgel is a lightweight porous solid material with the advantages of large specific surface area and high porosity. It can be used as heat insulation material, catalyst carrier, hydrogen storage material, adsorption material, etc. in many fields such as energy, aerospace, and environmental protection. Traditional silicon aerogels are relatively brittle, so their applicable fields are relatively limited. Organoaerogels represented by polyimide have been valued by researchers because of their excellent mechanical properties and good processing properties. [0003] Polyimide is a special engineering plastic with good thermal stability and high mechanical strength. The polyimide airgel prepared by condensation polymerization and imidizati...

Claims

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Application Information

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IPC IPC(8): C08J9/28C08J3/24C08L79/08C08K9/04C08K7/00C08K3/08C08K9/06C08K7/26C08K3/04C08K7/08C08G73/10
CPCC08G73/1071C08J3/24C08J9/28C08J2379/08C08K3/04C08K3/08C08K7/00C08K7/08C08K7/26C08K9/04C08K9/06C08K2003/0806C08K2201/011C08L79/08
Inventor 王凯张天翼李永武
Owner BEIHANG UNIV
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