A kind of transparent, high strength polyimide airgel and preparation method thereof

A polyimide and aerogel technology, applied in high-strength polyimide aerogel and its preparation, in the transparent field, can solve the problem of loss of thermal insulation performance, specific surface area, high porosity, and inability to achieve silica aerogelation. The transparency of the glue, the inability to replace the silica aerogel, etc., to achieve the effect of low thermal conductivity, reduction of stress concentration points, and uniform unloading of pressure

Active Publication Date: 2021-02-09
AEROSPACE RES INST OF MATERIAL & PROCESSING TECH +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, traditional polyimide aerogels usually exhibit a certain color and cannot achieve the transparency of silica aerogels
Therefore, although polyimide airgel can solve the brittleness of silica airgel, it loses its transparency at the same time. In some occasions that require high transparency, it cannot replace silica airgel to prepare polyimide with high transparency. Amine airgel has become one of the important problems to be solved urgently
On the other hand, the porous structure of airgel makes it easy to collapse and close under the action of external force, thus losing its excellent thermal insulation performance, huge specific surface area, high porosity and other characteristics. Therefore, the preparation of rigid pores with resistance to external pressure Structured airgel is also an important problem to be solved in the application of polyimide airgel

Method used

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  • A kind of transparent, high strength polyimide airgel and preparation method thereof
  • A kind of transparent, high strength polyimide airgel and preparation method thereof
  • A kind of transparent, high strength polyimide airgel and preparation method thereof

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preparation example Construction

[0027] The embodiment of the present invention provides a method for preparing a transparent, high-strength polyimide airgel, comprising the following steps:

[0028] Step 1. Dissolving aromatic triamine monomers and dianhydride monomers in a solvent according to a certain amount of proportioning to carry out polycondensation reaction until the reaction system is completely transparent;

[0029] Specifically, in the embodiment of the present invention, it is preferable to carry out the reaction under stirring, and when the reaction is complete until the system is completely transparent, ensure that the system does not contain any solid impurities;

[0030] In the embodiment of the present invention, the solvent is N,N-dimethylformamide (DMF), N,N-dimethylacetamide (DMAc), dimethylsulfoxide (DMSO) or N-methylpyrrolidone (NMP); the aromatic triamine monomer is preferably 4,4',4"-triaminotriphenylmethane (TAPM); the dianhydride monomer is preferably 3,3',4, At least one of 4'-be...

Embodiment 1

[0041] (1) Synthesis of polyimide wet gel:

[0042] Take 10mmol TAPM and fully dissolve it in 60ml of anhydrous DMF, then add 10.5mmol BTDA under stirring, and stir at 0°C until completely dissolved, the solution viscosity increases and polyamic acid is formed, and the reaction system is completely transparent at this time; then add 80mmol BTDA A mixture of acid anhydride and triethylamine (the mass ratio of acetic anhydride and triethylamine is 1:1), after rapid stirring for 10 minutes, ultrasonic defoaming for 30 minutes; finally, the resulting solution was left to stand at 0°C, and formed after about 5 hours gel.

[0043] (2) Solvent replacement of gel:

[0044] Place the formed gel in 5 times the volume of DMF, change the DMF every 12 hours, replace it twice, then use 5 times the volume of ethanol for solvent replacement, change the ethanol every 5 hours, and obtain polyimide after 2 days Amino Gel.

[0045] (3) Drying of wet gel:

[0046] The substituted alcohol gel w...

Embodiment 2

[0049] (1) Synthesis of polyimide wet gel:

[0050] Take 11mmol TAPM, fully dissolve in 100ml anhydrous DMSO, then add 11mmol PMDA under stirring, stir at 40°C until completely dissolved, the viscosity of the solution increases, and polyamic acid is formed, and the reaction system is completely transparent at this time; then add 80mmol acetic anhydride and triethylamine (the mass ratio of acetic anhydride and triethylamine is 1:1), after rapid stirring for 5 minutes, ultrasonic defoaming for 10 minutes; finally, the obtained solution was left standing at 40°C, and after about 5 hours, a gel was formed. glue.

[0051] (2) Solvent replacement of gel:

[0052] Place the formed gel in 2 times the volume of DMSO, change the DMSO every 12 hours, and replace it 3 times, then use 2 times the volume of methanol for solvent replacement, change the methanol every 5 hours, and obtain polyimide after 2 days Amino Gel.

[0053] (3) Drying of wet gel:

[0054] The substituted alcohol gel...

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Abstract

The invention provides transparent and high-strength polyimide aerogel and a preparation method thereof, which belongs to the technical field of nano porous materials and heat insulation and heat preservation. The preparation method comprises the following steps: dissolving aromatic triamine monomers and dianhydride monomers in a solvent to be reacted until a reaction system is completely transparent; adding a dewatering agent into the transparent system, stirring, defoaming, then standing, and forming gel; and performing the solvent replacement for the gel, and drying the gel, thus obtainingthe polyimide aerogel. The polyimide aerogel obtained by the invention has the characteristics of low density (the density is 0.08 g / cm<3> to 0.3 g / cm<3>), high specific surface area (the specific surface area is greater than 200 m<2> / g), high strength (the compression Young modulus is greater than 10MPa), low heat conductivity, high heat stability (the thermal degradation temperature is greater than 400 DEG C) and high transparency (the transmittance is greater than 50 percent), and the like.

Description

technical field [0001] The invention relates to a transparent, high-strength polyimide airgel and a preparation method thereof, belonging to the technical field of nanoporous materials and thermal insulation. Background technique [0002] Airgel is a nanomaterial with a continuous and open pore structure. It is currently the lightest solid material with the best thermal insulation performance in the world. Airgel has a high specific surface area (400 ~ 1500m 2 / g), high porosity (80-99.8%), low density (0.003-0.6g / cm 3 ) and low thermal conductivity (0.013 ~ 0.038W / m) and other characteristics, so that it has broad application prospects in the fields of heat insulation, acoustic impedance coupling, adsorption, filtration, catalyst carrier, drug carrier, etc. So far, various types of aerogels have been prepared by chemical crosslinking, including silica aerogels (CN102424538A; CN102633269A), chitosan aerogels (CN102417606A), carbon aerogels (CN102423668A; CN102430369A ), m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J9/28C08G73/10C08L79/08
CPCC08G73/1007C08G73/1067C08J9/286C08J2379/08
Inventor 赵一搏马晶晶王锦李鑫张学同朱文俐马晓静胡杰
Owner AEROSPACE RES INST OF MATERIAL & PROCESSING TECH
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