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Silica microparticle, composition forming polyimide aerogel, polyimide aerogel and manufacturing method thereof, and composite material

A technology of silica and polyimide, which is applied in the field of composite materials, can solve the problems of large manpower and time investment, high hazard, and high manufacturing cost, and achieve low chemical resistance, high porosity, and good flexibility sexual effect

Inactive Publication Date: 2017-07-04
TAIWAN TEXTILE RESEARCH INSTITUTE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the low surface energy solvents are highly hazardous due to their high neurotoxicity, and solvent replacement and / or drying using carbon dioxide supercritical fluids requires high-pressure processes, thereby consuming energy and requiring investment in special supercritical-resistant materials. The manufacturing cost is high due to equipment such as devices, and it also requires a lot of manpower and time.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Preparation of Silica Microparticles Containing Amino Groups

[0068] At room temperature, 4.17 g of tetraethoxysilane (produced by Acros) and 1.11 g of 3-aminopropyltriethoxysilane (produced by Acros) were dissolved in 10 g of DMAc as a solvent . Next, 0.5 g of NaOH was added as a catalyst over 30 minutes while stirring at room temperature. Then, at 30° C., the hydrolysis and condensation reaction was carried out with continuous stirring for 4 hours. Afterwards, the solvent was removed by centrifugation to obtain the amino group-containing silica microparticles of Example 1, wherein the equivalent number of amino groups in the amino group-containing silica microparticles was 8.5 mmol / g.

[0069] Preparation of compositions for forming polyimide airgel

[0070] 2.1229g (0.01mol) of 3,3'-dimethylbenzidinediamine (hereinafter referred to as DMB), 3.0893g (0.0105mol) of 3,3',4,4'-biphenyltetracarboxylic dianhydride (hereinafter referred to as BPDA), 1.7374g of the amin...

Embodiment 2

[0074] Preparation of Silica Microparticles Containing Amino Groups

[0075] The amino group-containing silica fine particles of Example 2 were produced according to the same production procedure as in Example 1.

[0076] Preparation of compositions for forming polyimide airgel

[0077] 2.0024g (0.01mol) of 4,4'-diaminodiphenyl ether (hereinafter referred to as ODA), 3.0893g (0.0105mol) of BPDA, 1.6972g of the amino group-containing silica microparticles of Example 2 and as Add 61g of NMP as a solvent into a 100mL three-necked flask with mechanical stirring, and stir for 8 hours in a nitrogen environment and at room temperature so that ODA, BPDA and the amino group-containing silica particles of Example 2 are in the solvent. Mix evenly to obtain the polyimide airgel-forming composition of Example 2 with a solid content of 10 wt%.

[0078] Preparation of polyimide airgel

[0079] At 30°C and under a nitrogen atmosphere, the composition for forming polyimide airgel in Example...

Embodiment 3

[0081] Preparation of Silica Microparticles Containing Amino Groups

[0082] The amino group-containing silica fine particles of Example 3 were produced according to the same production procedure as in Example 1.

[0083] Preparation of compositions for forming polyimide airgel

[0084] Add 2.1229g (0.01mol) of DMB, 3.0893g (0.0105mol) of BPDA, 1.7374g of the amino group-containing silica microparticles of Example 3, and 65g of NMP as a solvent into a 100mL three-necked three-neck device with mechanical stirring. In the flask, and under nitrogen environment and room temperature, stirred for 8 hours so that the DMB, BPDA and the amino group-containing silicon dioxide microparticles of Example 3 were mixed uniformly in the solvent, to obtain Example 3 with a solid content of 10wt%. Compositions for forming polyimide airgel.

[0085] Preparation of polyimide airgel

[0086] At 30°C and under a nitrogen atmosphere, the composition for forming polyimide airgel in Example 3 was c...

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Abstract

The invention provides a silica microparticle, a composition forming a polyimide aerogel, the polyimide aerogel and a manufacturing method thereof, and a composite material. The silica microparticle containing an amino group is prepared by subjecting alkoxy silane as shown in a formula (I) and alkoxy silane as shown in a formula (II) to hydrolytic condensation in the presence of a catalyst, wherein the formula (I) is Si(OR<1>)<4>, and the formula (II) is (NH<2>-Y)<m>-Si(OR<2>)<4-m>; in the formula (I), R<1> is an alkyl group with a carbon number of 1 to 10; and in the formula (II), Y is an alkyl group with a carbon number of 1 to 10 or an alkyl group with a carbon number of 2 to 10, R<2> is an alkyl group with a carbon number of 1 to 10, and m is an integer in a range of 1 to 3. According to the invention, the polyimide aerogel has the characteristics of high porosity, good thermal insulation properties, good flexural strength, flame resistance, resistance to UV light and chemicals, low dielectric coefficient and the like, does not need low-surface-energy solvents like hexane and pentane and a carbon dioxide supercutical fluid in the process of preparation, and is applicable to the composite material.

Description

technical field [0001] The invention relates to a silicon dioxide particle and a polyimide airgel prepared by using the silicon dioxide particle, in particular to an amino group-containing silicon dioxide particle and a composition for forming a polyimide airgel , polyimide airgel, its manufacturing method, and composite material. Background technique [0002] Aerogels are unique solids with high porosity. High porosity makes aerogels have the characteristics of high surface area, low refractive index, low dielectric constant, low heat loss coefficient and low velocity conduction medium. Therefore, aerogels have broad application prospects in integrated circuits, energy saving, aviation and other fields. [0003] In the traditional method of manufacturing airgel, in order to avoid the collapse of the porous structure during the drying process, it is usually necessary to use low surface energy solvents such as n-hexane and pentane for solvent replacement or use carbon dioxi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J9/28C01B33/12
CPCC08G73/106C01B33/12C08J9/28C08J2379/08
Inventor 周上智萧孟慈
Owner TAIWAN TEXTILE RESEARCH INSTITUTE
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