Deformable aerogel material and preparation method thereof

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

Active Publication Date: 2019-10-08
AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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  • Description
  • Claims
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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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  • Deformable aerogel material and preparation method thereof
  • Deformable aerogel material and preparation method thereof
  • Deformable aerogel material and preparation method thereof

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preparation example Construction

[0030] In the first aspect, the present invention provides a method for preparing a deformable aerogel material, which is characterized in that the method includes the following steps:

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

[0032] (2) Add 1,1,1-tri...

Embodiment 1

[0060] ①Preparation of polyimide wet gel

[0061] Under the protection of nitrogen, 1.020g 2,2'-bis[4-(3-aminophenoxy)phenyl]hexafluoropropane (m-6FBAPP) was dissolved in 10g N,N-dimethylacetamide (DMAc) (The first organic solvent), stir for 10 minutes; then add 0.885g 4,4'-(hexafluoroisopropylene) diphthalic anhydride (6FDA) to the above solution, and the whole system is stirred and reacted at room temperature for 28 hours to obtain a reaction Solution; Add 0.0116g 1,1,1-tris[4-(aminophenoxy)phenyl]ethane (TAPE) and 5.4gN,N-dimethylacetamide (DMAc) to the reaction solution (second Organic solvent) to obtain a uniform polyamic acid (PAA) solution. At this time, add 0.02g of fumed silica nanoparticles with a particle size of 30nm to the PAA solution and stir for 30 minutes; then add fumed silica nanoparticles 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℃) for 1 hour. After taki...

Embodiment 2

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

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

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Abstract

The invention relates to a deformable aerogel material and a preparation method thereof. The method comprises the steps of carrying out a polycondensation reaction using a diamine and a dianhydride asmonomers, and then adding 1,1,1-tri[4-(aminophenoxyl)phenyl]ethane as a curing agent to obtain a polyamic acid solution, and adding fumed silica nanoparticles to obtain that polyamic acid solution doped with fumed silica nanoparticles, and then treating the polyamic acid solution in a vacuum oven and subjecting to thermal imidization at different temperature stages heating procedures to obtain apolyimide wet gel; subjecting the polyimide wet gel to ageing, solvent replacement and supercritical drying to obtain the deformable aerogel material. The aerogel material of the invention can be deformed and fixed under the heating condition, and the shape is restored under the next thermal response, and the temperature resistance of the material is good. The aerogel material of the invention hasthe advantages of high porosity (88-99%), high shape recovery rate (90-100%), adjustable deformation and recovery temperature and the like.

Description

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

Claims

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Application Information

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Patent Type & Authority Applications(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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