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Multifunctional flame-retardant polyimide aerogel as well as preparation method and application thereof

A technology of flame-retardant polyimide and polyimide, which is applied in thermal analysis of materials, coatings, instruments, etc., can solve the problems of poor mechanical properties, single functionality, insufficient thermal stability, etc., and achieve excellent mechanical properties , protect the internal structure, excellent fire safety effect

Active Publication Date: 2021-07-02
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a multifunctional flame-retardant polyimide (PI) airgel and its preparation for the defects of current organic aerogels such as easy combustion, poor mechanical properties, insufficient thermal stability and single functionality. method

Method used

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  • Multifunctional flame-retardant polyimide aerogel as well as preparation method and application thereof
  • Multifunctional flame-retardant polyimide aerogel as well as preparation method and application thereof
  • Multifunctional flame-retardant polyimide aerogel as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] 1) Preparation of water-soluble polyamic acid: slowly add 0.01mol of 4,4'-diaminodiphenyl ether and 50mL of N,N-dimethylacetamide into the reaction kettle at 0°C, 400r / min Stir mechanically at a rotating speed for 1 h to form a uniform solution to obtain a diamine monomer solution; gradually add 0.0125 mol of pyromellitic dianhydride to the above solution, continue stirring for 5 h, then slowly add 3 mL of triethylamine dropwise, at 400 r Reaction with mechanical stirring at 1 / min for 5 hours, washed 3 times with deionized water at 0°C, and freeze-dried at -50°C and 10Pa for 48 hours to obtain polyamic acid;

[0042] 2) Preparation of polyimide airgel: add 0.5g of polyamic acid, 0.02g of triethylamine and 99.48g of deionized water prepared in step 1) to the reactor, stir at 500r / min for 0.5h, then Freeze-dry at -40°C and 20Pa for 24 hours; heat at 5°C / min to 80°C for 1 hour under argon atmosphere, then heat at 5°C / min to 150°C for 1 hour, and finally heat at 5°C / min to ...

Embodiment 2

[0052] 1) Preparation of water-soluble polyamic acid: at 3°C, slowly add 0.02mol 3,4'-diaminodiphenyl ether and 300mL N-methylpyrrolidone into a three-necked flask, and mechanically stir at 200r / min for 2h to make it Dissolve so that it forms a homogeneous solution. Gradually add 0.02mol 3,3',4,4'-biphenyltetracarboxylic dianhydride into the above solution, continue to stir for 3h, then slowly add 5mL of dipropylamine dropwise, and react with mechanical stirring at 200r / min for 3h. It was washed 4 times with deionized water at 2° C., and freeze-dried at -20° C. and 230 Pa for 72 hours to obtain polyamic acid.

[0053] 2) Preparation of polyimide airgel: Add 4g of polyamic acid, 0.4g of dipropylamine and 95.6g of deionized water prepared in step 1) into the reaction kettle, stir at 300r / min for 1h, and then place it at -50 ℃, 50Pa under freeze-drying for 12 hours, heating under nitrogen atmosphere by heating at 10℃ / min to 100℃ for 3h, 5℃ / min to 120℃ for 2h and 20℃ / min to 250℃ ...

Embodiment 3

[0058]1) Preparation of water-soluble polyamic acid: slowly add 0.03mol 4,4'-diaminodiphenylmethane and 150mL dimethylformamide into the reaction vessel at 5°C, and mechanically stir at 500r / min for 0.5h , make it dissolve, make it form a uniform solution, and obtain a diamine monomer solution; gradually add 0.03mol 4,4'-biphenyl ether dianhydride to the above solution, continue stirring for 5 hours, and then slowly drop 10mL of n-hexylamine into , mechanically stirred at 500r / min for 3.5h, washed 3 times with deionized water at 1°C, and freeze-dried at -25°C and 180Pa for 24h to obtain polyamic acid;

[0059] 2) Preparation of polyimide airgel: Add 10g of polyamic acid, 0.6g of triethylamine and 89.4g of deionized water prepared in step 1) into the reaction kettle, stir at 400r / min for 3h, and then - Freeze drying at 40°C and 40Pa for 72 hours, heat imidization (under nitrogen atmosphere, heat up to 90°C at 5°C / min and keep for 3 hours, 5°C / min to 130°C for 2 hours, and 5°C / m...

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Abstract

The invention belongs to the technical field of organic aerogel, and discloses multifunctional flame-retardant polyimide aerogel as well as a preparation method and application thereof. The method comprises the following steps: firstly preparing polyimide aerogel, then carrying out plasma treatment on the polyimide aerogel, then dip-coating the polyimide aerogel with a two-dimensional thermoelectric nano-material dispersion liquid, washing and drying to obtain the multifunctional flame-retardant polyimide aerogel. The two-dimensional thermoelectric nano material dispersion liquid is obtained by dispersing a two-dimensional thermoelectric nano material in a solvent. The multifunctional flame-retardant polyimide aerogel prepared by the invention not only has excellent mechanical properties and flame retardancy, but also has sensitive temperature sensing, piezoresistive sensing and other functions, and can realize repeatable temperature sensing performance and fire early warning response. The aerogel disclosed by the invention is applied to the fields of aerospace, transportation, architectural decoration, electronic skin and the like.

Description

technical field [0001] The invention belongs to the technical field of organic airgel, and in particular relates to a multifunctional flame-retardant polyimide airgel and its preparation method and application. Background technique [0002] Due to the advantages of extremely low density, extremely high porosity, and excellent thermal insulation properties, aerogels have broad application prospects in the fields of building exterior wall insulation materials, piezoresistive sensing, and energy harvesting. Aerogels can be divided into organic and inorganic aerogels. Inorganic aerogels are high temperature resistant and flame retardant, such as silica aerogels and alumina aerogels, but they are brittle and brittle; organic aerogels are flexible, such as polyvinyl alcohol aerogels and polyvinyl chloride aerogels. Aerogels, cellulose aerogels and silicone aerogels. However, most organic aerogels have poor thermal stability and are easy to burn. Polyimide (PI) has a rigid aroma...

Claims

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Application Information

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IPC IPC(8): C08J9/36C08J9/40C08J9/28C08L79/08G01N25/00
CPCC08J9/36C08J9/40C08J9/365C08J9/28G01N25/00C08J2379/08C08J2201/0484C08J2205/026
Inventor 赖学军陈嘉韵曾幸荣李红强吴政忠丘昀坤
Owner SOUTH CHINA UNIV OF TECH
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