Preparation method of silicon dioxide aerogel

A silicon dioxide and aerogel technology, applied in chemical instruments and methods, inorganic chemistry, silicon compounds, etc., can solve problems such as unfavorable large-scale production, achieve large-scale promotion and application, improve environmental adaptability, reduce The effect of production difficulty

Inactive Publication Date: 2018-11-13
SICHUAN KENINGTAI TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In view of the above-mentioned prior art, the present invention provides a method for preparing silica airgel to solve t

Method used

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  • Preparation method of silicon dioxide aerogel
  • Preparation method of silicon dioxide aerogel
  • Preparation method of silicon dioxide aerogel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Preparation of silica airgel with a molar ratio of MTMS:TEOS:APTES=1:1:1 at 0°C includes the following steps:

[0032] (1) Measure 11.2ml, 7.2ml, and 11.7ml of ethyl orthosilicate, methyltrimethoxysilane, and 3-aminopropyltriethoxysilane respectively, place them in container a, stir at room temperature for 100min, and obtain a mixture Reagent A: Measure 50ml and 12.5ml of acetonitrile and deionized water respectively, place them in container b, stir at room temperature for 60min, and obtain mixed reagent B;

[0033] (2) Place container a and container b in ice water respectively until the temperature of mixed reagent A and mixed reagent B therein drops to 0°C;

[0034] (3) Quickly pour the cooled mixed reagent B into mixed reagent A, first stir at 0°C for 3 minutes to complete the gelation; then pour the gelled solution into the pre-prepared mold for aging for 24 hours, wet gel;

[0035] (4) Place the obtained wet gel successively in an ethanol solution with a volume ...

Embodiment 2

[0039] Preparation of silica airgel with a molar ratio of MTMS:TEOS:APTES=7:1:4 at 0°C includes the following steps:

[0040] (1) Measure 11.2ml, 50.4ml, and 47ml of ethyl orthosilicate, methyltrimethoxysilane, and 3-aminopropyltriethoxysilane respectively, place them in container a, stir at room temperature for 100min, and obtain a mixed reagent A: Measure 50ml and 15ml of acetonitrile and deionized water respectively, place them in container b, and stir at room temperature for 40min to obtain mixed reagent B;

[0041] (2) Place container a and container b in ice water respectively until the temperature of mixed reagent A and mixed reagent B therein drops to 0°C;

[0042] (3) Quickly pour the cooled mixed reagent B into the mixed reagent A, first stir at 0°C for 10 minutes to complete the gelation; then pour the gelled solution into the pre-prepared mold for aging for 30 hours, wet gel;

[0043] (4) Place the obtained wet gel successively in an ethanol solution with a volum...

Embodiment 3

[0047] Preparation of silica airgel with a molar ratio of MTMS:TEOS:APTES=4:1:1 at 0°C includes the following steps:

[0048](1) Measure 8.9ml, 28.8ml, and 11.7ml of ethyl orthosilicate, methyltrimethoxysilane, and 3-aminopropyltriethoxysilane respectively, place them in container a, stir at room temperature for 95min, and obtain a mixture Reagent A: Measure 50ml and 13.5ml of acetonitrile and deionized water respectively, place them in container b, stir at room temperature for 50min, and obtain mixed reagent B;

[0049] (2) Place container a and container b in ice water respectively until the temperature of mixed reagent A and mixed reagent B therein drops to 0°C;

[0050] (3) Quickly pour the cooled mixed reagent B into the mixed reagent A, first stir at 0°C for 8 minutes to complete the gelation; then pour the gelled solution into the pre-prepared mold for aging for 28 hours, wet gel;

[0051] (4) Place the obtained wet gel successively in an ethanol solution with a volum...

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Abstract

The invention discloses a preparation method of silicon dioxide aerogel. The preparation method comprises the following steps: during preparation, firstly mixing TEOS (Tetraethyl Orthosilicte), MTMS (Methyl Trimethoxysilane) and APTES (Aminopropyl Triethoxysilane), thus obtaining a mixed reagent A; mixing acetonitrile with deionized water, thus obtaining a mixed reagent B; then cooling the mixed reagent A and the mixed reagent B to 0 DEG C; then mixing the cooled mixed reagent A with the cooled mixed reagent B, and aging at room temperature, thus obtaining wet gel; carrying out solvent exchange on the wet gel through ethanol and acetonitrile in sequence, firstly soaking the wet gel in an acetonitrile solution of hexamethylene diisocyanate, then transferring the wet gel into an acetonitrilesolution, keeping warm at 70 DEG C for 72 hours, and then carrying out the solvent exchange on the wet gel in the acetonitrile solution; finally, carrying out CO2 supercritical drying on the wet gel,thus obtaining isocyanate reinforced silicon dioxide aerogel. By adopting the preparation method disclosed by the invention, the technical problems that preparation of the aerogel requires to be carried out at -77 DEG C, and large-scale production is not facilitated can be effectively solved.

Description

technical field [0001] The invention belongs to the technical field of airgel preparation, and in particular relates to a preparation method of silica airgel. Background technique [0002] Silica airgel has the characteristics of low density, high porosity, high specific surface area, low thermal conductivity, high thermal stability, etc. Its superior properties make it widely used in the fields of high energy physics, catalysis, energy storage and space exploration. There are a wide range of applications. However, their applications are limited due to their inherent brittleness, hydrophilicity, and poor mechanical properties. So far, scientists have invented many methods to improve the mechanical properties of aerogels. For example, using a silicon source containing flexible long chains, covering the skeleton of the aerogel with a polymer through cross-linking, using fibers to dope the initial gel as a skeleton, etc. All in all, it is necessary to connect organic substan...

Claims

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Application Information

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IPC IPC(8): C01B33/158
CPCC01B33/1585
Inventor 郭丹岳晓华
Owner SICHUAN KENINGTAI TECH CO LTD
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