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Flexible polyimide aerogel and preparation method thereof

A technology of polyimide and airgel, which is applied in the field of flexible polyimide airgel and its preparation, can solve the problems of polyimide lack of toughness, ineffective performance, and unobtainable, etc., to achieve excellent flexibility The effects of outstanding stability, thermodynamic and mechanical properties, and improved compatibility

Active Publication Date: 2020-05-05
NEW MATERIAL INST OF SHANDONG ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese invention patent application CN 108794766 A discloses a cross-linked polyimide airgel and its preparation method. The intermediate product is obtained by cross-linking the amino-terminated polyamic acid and the polyanhydride-based cross-linking agent. Solvent thermal imidization to obtain polyimide wet gel, which is then obtained by solvent replacement and supercritical drying; the intermediate product is a polyamic acid wet gel with a cross-linked structure; the invention prepares a wet gel with a cross-linked The intermediate product (polyamic acid wet gel) of the network is imidized by solvothermal to convert it into a cross-linked polyimide wet gel, which overcomes the inability to obtain a real cross-linked structure in the prior art. The problem of polyimide airgel
The polyimide prepared by the method of diamine and dianhydride can make the polyimide airgel have good mechanical strength, excellent specific surface area and low density due to the rigid structure of the monomer itself, but the polyimide airgel has excellent specific surface area and low density. Imide itself still lacks toughness, and its effect is not obvious in the application field of receiving relatively large impact force or shock absorption and noise reduction
[0005] Therefore, how to find a reasonable preparation method to obtain a flexible polyimide airgel, overcome the defect of polyimide airgel lack of toughness, and maintain good mechanical strength, specific surface area and low density , has become one of the focuses of many applied researchers in the industry

Method used

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  • Flexible polyimide aerogel and preparation method thereof
  • Flexible polyimide aerogel and preparation method thereof
  • Flexible polyimide aerogel and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Embodiment 1 prepares flexible polyimide airgel

[0034] Proceed as follows:

[0035] 1) Mix 6.4g of 3,3',4,4'-biphenyltetracarboxylic dianhydride, 0.855g of trifunctional polypropylene glycol with a molecular weight of 400, and 1.69g of 4,4'-diphenylmethane diisocyanate, add 50 g of N,N-dimethylacetamide was heated to 90° C. for 3 hours to obtain a flexible polyamic acid.

[0036] 2) Put the flexible polyamic acid in 50g of acetone and place it for 12 hours for solvent replacement; after filtering out the solvent, add 50g and place it for 24 hours for a second solvent replacement to obtain the flexible polyamic acid after solvent replacement.

[0037] 3) The flexible polyamic acid is subjected to supercritical CO 2 Dry, CO 2 The gas pressure is 10MPa, the temperature is 32°C, and the drying time is 24 hours to obtain a flexible polyamic acid airgel.

[0038] 4) The flexible polyamic acid airgel is post-cured at 80° C. for 12 hours to form a flexible polyimide.

Embodiment 2

[0039] Embodiment 2 prepares flexible polyimide airgel

[0040] Proceed as follows:

[0041] 1) Mix 1g of 4,4'-biphenyl ether dianhydride, 1.2g of difunctional polypropylene glycol with a molecular weight of 400, 1.01g of a trifunctional polypropylene glycol with a molecular weight of 400, and 3g of 4,4'-diphenylmethane diisocyanate , add 42g of N,N-dimethylacetamide, heat up to 90°C and react for 2 hours to obtain flexible polyamic acid.

[0042] 2) Put the flexible polyamic acid in 42g of acetone for 12 hours for solvent replacement; after filtering out the solvent, add 42g of acetone for 12 hours for secondary solvent replacement; after filtering out the solvent, add 42g of acetone for 12 hours Hour, carry out solvent replacement three times, obtain the flexible polyamic acid after solvent replacement.

[0043] 3) The flexible polyamic acid is subjected to supercritical CO 2 Dry, CO 2 The gas pressure is 8 MPa, the temperature is 32° C., and the drying time is 12 hours ...

Embodiment 3

[0045] Embodiment 3 prepares flexible polyimide airgel

[0046] Proceed as follows:

[0047] 1) 1.18g of 3,3',4,4'-biphenyltetracarboxylic dianhydride, 4g of difunctional polypropylene glycol with a molecular weight of 2000, 1.01g of a trifunctional polypropylene glycol with a molecular weight of 400, 4,4'-bis 2.5 g of phenylmethane diisocyanate was mixed, 63 g of N,N-dimethylacetamide was added, and the temperature was raised to 90° C. for 2 hours to obtain a flexible polyamic acid.

[0048] 2) Put the flexible polyamic acid in 63g of acetone for 12 hours for solvent replacement; after filtering out the solvent, add 63g of acetone for 24 hours for secondary solvent replacement; after filtering out the solvent, add 63g of acetone for 12 hours Hour, carry out solvent replacement three times, obtain the flexible polyamic acid after solvent replacement.

[0049] 3) The flexible polyamic acid is subjected to supercritical CO 2 Dry, CO 2 The gas pressure is 8 MPa, the temperatu...

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Abstract

The invention discloses flexible polyimide aerogel which is prepared by the following method: (1) reacting a dianhydride monomer, an isocyanate monomer and a polyether polyol monomer in a polar aprotic organic solvent to form flexible polyamide acid; (2) putting flexible polyamide acid into acetone for replacement to obtain a semi-finished product; (3) performing supercritical CO2 drying on the semi-finished product to obtain polyamide acid aerogel; and (4) carrying out post-curing on the polyamide acid aerogel to obtain the polyimide aerogel. According to the flexible polyimide aerogel, the polyether polyol is used as a flexible long chain, the polyamide acid precursor is prepared by combining an isocyanate monomer and a dianhydride monomer to form flexible polyimide through reaction withdiamine,and a supercritical CO2 drying method is adopted to prepare the polyurethane-modified flexible polyimide, such that the polyurethane-modified flexible polyimide has advantages of polyurethane modification, excellent shock absorption, excellent noise reduction, excellent thermal insulation and excellent dimensional stability, and has broad application prospects especially in the field ofapplications requiring impact resistance.

Description

technical field [0001] The invention relates to a flexible polyimide airgel and a preparation method thereof, belonging to the technical field of polymer porous materials. Background technique [0002] Polyimide is a kind of organic polymer material with imide ring in the main chain. It has good mechanical strength, heat resistance and heat insulation stability, and anti-friction and anti-wear properties. It is usually used as a high-performance heat-resistant structural part in Many high-end application fields have been applied. Due to the wide selectivity of polyimide raw materials dianhydride and diamine, polyimide materials with specific properties can be synthesized according to specific conditions of use. [0003] Airgel is a solid form of matter and is one of the least dense solids in the world. Because of its excellent lightweight characteristics and heat insulation effect, airgel has been applied in special clothing industry and combat vehicles. At present, the t...

Claims

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Application Information

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IPC IPC(8): C08J9/28C08G73/10C08L79/08
CPCC08J9/28C08G73/1035C08G73/1046C08J2205/026C08J2379/08C08J2205/042Y02P20/54
Inventor 李冰赵宁刘本学于一涛李金辉王峰张方志彭丹张硕
Owner NEW MATERIAL INST OF SHANDONG ACADEMY OF SCI