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Polyimide aerogel and preparation method thereof

A technology of polyimide and airgel, which is applied in the field of airgel, and can solve the problems of cumbersome organic solvent replacement steps and high gel density in the system

Active Publication Date: 2021-04-20
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It mainly solves the shortcomings of high gel density and cumbersome organic solvent replacement steps in the existing polyimide airgel preparation process

Method used

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  • Polyimide aerogel and preparation method thereof
  • Polyimide aerogel and preparation method thereof
  • Polyimide aerogel and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] 1. Dissolve 7.89g of pyromellitic anhydride (PMDA) and 7.11g of 4,4`-diaminodiphenyl ether (ODA) (the molar ratio of dianhydride and diamine is 1.02:1) in 85.0g of N , in N-dimethylformamide (DMF) (the mass ratio of solute to solvent is 15:85), in N 2 Mix under the protection of an inert gas, stir and react at 25°C for 6 hours, and obtain a polyamic acid (PAA) solution after the reaction; then add the PAA solution dropwise to water to precipitate, filter, wash, and dry to obtain PAA powder.

[0055] 2. Add 5.0g of PAA (0.024mol of carboxyl moles) powder into 95.0g of water to disperse, then add 1.21g (0.012mol) triethylamine and stir for a while, then add 0.56g (0.0048mol) tetramethylethylamine The diamine continued to stir, and after the polyamic acid was completely dissolved and the solution was clear and transparent, it was left to stand for 2 hours to make the solution produce sol-gel.

[0056] 3. Before freezing, place the gelled sample in a refrigerator at 4°C to...

Embodiment 2

[0059] 1. Dissolve 3.58g of PMDA, 4.83g of biphenyltetracarboxylic dianhydride (BPDA) and 6.58g of ODA (the molar ratio of dianhydride and diamine is 1.02:1, wherein the molar ratio of PMDA to BPDA is 1:1) In 85.0g of N,N-dimethylformamide (DMF) (the mass ratio of solute to solvent is 15:85), in N 2 Mix under the protection of an inert gas, stir and react at 25°C for 6 hours, and obtain a polyamic acid (PAA) solution after the reaction; then add the PAA solution dropwise to water to precipitate, filter, wash, and dry to obtain PAA powder.

[0060] 2. Add 5.0 g of PAA (0.022 mol of carboxyl moles) powder into 95.0 g of water to disperse, then add 1.11 g (0.011 mol) triethylamine and stir for a while, then add 0.51 g (0.0044 mol) tetramethylethylamine The diamine continued to stir, and after the polyamic acid was completely dissolved and the solution was clear and transparent, it was left to stand for 4 hours to make the solution produce sol-gel.

[0061] 3. Before freezing, pl...

Embodiment 3

[0064] 1. Mix 4.61g of 3,3',4,4'-benzophenone tetracarboxylic dianhydride (BTDA), 6.37g of 4,4'-(hexafluoroisopropylene) diphthalic anhydride (6FDA), 2.60g ODA and 1.41g of terephthalic anhydride (PDA) (the molar ratio of dianhydride and diamine is 1.10:1, wherein the molar ratio of BTDA to 6FDA is 1:1, and the molar ratio of ODA to PDA is 1:1) is dissolved in 85.0 g of N,N-dimethylacetamide (DMAc) (the mass ratio of solute to solvent is 15:85), in N 2 Mix under the protection of an inert gas, stir and react at 25°C for 6 hours, and obtain a polyamic acid (PAA) solution after the reaction; then add the PAA solution dropwise to water to precipitate, filter, wash, and dry to obtain PAA powder.

[0065] 2. Add 15.0 g of PAA (0.057 mol of carboxyl moles) powder into 85.0 g of water for dispersion, then add 4.04 g (0.040 mol) of triethylamine and stir for a while, then add 1.32 g (0.011 mol) of tetramethylethane The diamine continued to stir, and after the polyamic acid was comple...

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Abstract

The invention relates to a green and environment-friendly preparation method of low-density polyimide aerogel. The method comprises the following steps: dispersing polyamic acid in water, and respectively and sequentially adding monobasic tertiary amine and polybasic tertiary amine to form a hydrogel; after the hydrogel is aged, carrying out freeze drying to obtain aerogel, and then carrying out thermal imidization to obtain the polyimide aerogel. According to the method, the organic gel aerogel conversion process needed in a traditional polyimide aerogel preparation method is well solved, the tedious replacement steps of an organic solvent are reduced, the tolerance requirement of solvent replacement equipment is reduced, and large-scale green production can be achieved; in addition, by regulating and controlling the dosage of a cross-linking agent, the control of the cross-linking density can be effectively realized, the intrinsic density of the gel material is reduced on the premise of ensuring certain strength, and the polyimide aerogel with good barrier property is obtained.

Description

technical field [0001] The present invention relates to the field of aerogels, in particular to a method for preparing a low-density polyimide airgel with a certain strength and imide aerogels, and the selection of a green and environment-friendly solvent system can realize industrial application expand. Background technique [0002] Polyimide (PI) is a high-performance engineering plastic with excellent temperature resistance and good molding processability. It has been widely used in aerospace, environmental industry, medical and health and other harsh fields. Polyimide airgel is a typical application of the organic combination of various properties of polyimide. Through the method of sol-gel and solvent replacement, the three-dimensional network of polyimide is filled with air to form a porous material. This kind of material While obtaining the intrinsic heat resistance of polyimide, the introduction of the air medium also increases the specific surface area and porosity...

Claims

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Application Information

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IPC IPC(8): C08J9/28C08J3/075C08G73/10C08L79/08
CPCY02P20/54
Inventor 张培斌李应成崔晶孙旭阳
Owner CHINA PETROLEUM & CHEM CORP
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