A kind of deformable airgel material and preparation method thereof

An aerogel and polyimide wet gel technology, which is applied in the field of deformable aerogel materials and their preparation, can solve the problems of low shape recovery rate and poor deformability, and achieves high shape recovery rate and porosity. The effect of high rate and high temperature resistance

Active Publication Date: 2022-02-18
AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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Problems solved by technology

Chinese patent application CN201610640949.7 discloses a preparation method of cross-linked polyimide airgel, which has the characteristics of wide applicability, cheap and easy-to-obtain raw materials, simple reaction process, and low overall cost. The material has a nanoscale multi-level microstructure; Chinese patent application CN201810672858.0 discloses a hydrophobic silica / polyimide airgel composite material and its preparation method, and the hydrophobic silica prepared by the patent application / Polyimide airgel composites can effectively improve polyimide airgel hydrophobicity, mechanical properties and thermal insulation properties; however, the deformability of the airgel materials prepared by these patents is poor, and the shape after deformation low response rate
[0004] So far, the research direction of polyimide is mainly the application research of structure and function. There is no report on the one-dimensional, two-dimensional and three-dimensional structure construction of materials, and the making of polyimide into deformable airgel The material has not been reported

Method used

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  • A kind of deformable airgel material and preparation method thereof
  • A kind of deformable airgel material and preparation method thereof
  • A kind of deformable airgel material and preparation method thereof

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preparation example Construction

[0030] The present invention provides a kind of preparation method of deformable airgel material in the first aspect, it is characterized in that, described method comprises the following steps:

[0031] (1) Under the protection of an inert gas (such as nitrogen or argon), mix 2,2'-bis[4-(3-aminophenoxy)phenyl]hexafluoropropane (m-6FBAPP) and 4,4' -(hexafluoroisopropylene) diphthalic anhydride (6FDA) (non-coplanar crosslinking agent) is dissolved in a first organic solvent (such as N,N-dimethylacetamide (DMAc)) for polycondensation reaction to obtain a reaction solution ; Specifically, for example, under nitrogen protection, 2,2'-bis[4-(3-aminophenoxy)phenyl]hexafluoropropane (m-6FBAPP) was dissolved in N,N-dimethyl Acetamide (DMAc), stirring for 10 minutes; then adding 4,4'-(hexafluoroisopropylene) diphthalic anhydride (6FDA) to the above solution, and stirring the whole system at room temperature for 5-48 hours to obtain the reaction solution.

[0032](2) Add 1,1,1-tris[4-...

Embodiment 1

[0060] ① Preparation of polyimide wet gel

[0061] Under nitrogen protection, 1.020g of 2,2'-bis[4-(3-aminophenoxy)phenyl]hexafluoropropane (m-6FBAPP) was dissolved in 10g of N,N-dimethylacetamide (DMAc) (the first organic solvent), stirring for 10 minutes; then adding 0.885g 4,4'-(hexafluoroisopropylene) diphthalic anhydride (6FDA) to the above solution, and stirring the whole system at room temperature for 28 hours to obtain the reaction solution; add 0.0116g 1,1,1-tris[4-(aminophenoxy)phenyl]ethane (TAPE) and 5.4g N,N-dimethylacetamide (DMAc) to the reaction solution (second organic solvent), to obtain a uniform polyamic acid (PAA) solution, this time, adding 0.02g particle diameter to the PAA solution is the fumed silica nanoparticles of 30nm, stirred for 30min; The PAA solution was divided into two 50mL beakers, sealed with plastic wrap, and placed in a vacuum oven (the temperature of the vacuum oven was 40°C) for 1 hour, and then left to stand for 5 minutes to defoam; t...

Embodiment 2

[0068] Example 2 is basically the same as Example 1, except that the first organic solvent N,N-dimethylacetamide (DMAc) is used in an amount of 20g, and the second organic solvent N,N-dimethyl The amount of acetamide (DMAc) used is 10.8 g, and the total amount of the first organic solvent and the second organic solvent is 30.8 g.

[0069] Embodiments 3-9 are basically the same as Embodiment 1, and the differences are shown in Table 1.

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Abstract

The invention relates to a deformable airgel material and a preparation method thereof. The method comprises: carrying out polycondensation reaction with dianhydride and diamine as monomers, and then adding 1,1,1-tris[4-(aminophenoxy)phenyl]ethane as a curing agent to obtain a polyamic acid solution , and adding fumed silica nanoparticles to obtain a polyamic acid solution mixed with fumed silica nanoparticles, which is then treated in a vacuum oven and heated at different temperature stages for thermal imidization to obtain polyimide Wet gel: The polyimide wet gel is subjected to aging, solvent replacement and supercritical drying in sequence to obtain a deformable airgel material. The airgel material of the present invention can be deformed and fixed under heating conditions, and recovers its shape under the next thermal response, and the material has good temperature resistance. The airgel material of the present invention has a high porosity (88% to 99%), It has the advantages of high shape recovery rate (90% to 100%) and adjustable deformation and recovery temperature.

Description

technical field [0001] The invention belongs to the technical field of airgel preparation, and in particular relates to a deformable airgel material and a preparation method thereof. Background technique [0002] As a nanoporous material, airgel has a continuous three-dimensional nanoporous network structure composed of nanoparticles, endowing it with characteristics such as low density, high porosity, high specific surface area, and large pore volume. The unique structural characteristics make aerogels have good performance in heat insulation, gas adsorption and separation, water treatment, catalysis, etc., and have broad application prospects in aerospace, petrochemical, new energy, scientific research, energy-saving buildings, environmental protection, etc. . In the field of heat insulation materials, airgel materials have been recognized as the most efficient heat insulation materials, and have been widely used in heat insulation applications of various aerospace vehicl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J9/28C08L79/08C08K7/26C08G73/10
CPCC08J9/28C08G73/1039C08G73/1071C08J2201/0502C08J2379/08C08K7/26C08K2201/011
Inventor 张恩爽刘韬李文静雷朝帅贺丽娟杨洁颖张昊
Owner AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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