Method for preparing silica aerogel material

A silicon dioxide and aerogel technology, applied in the direction of silicon dioxide, silicon oxide, etc., can solve the problems of long preparation cycle and the preparation process route needs to be optimized, and achieve low density, good hydrophobicity, and concentrated pore size distribution. Effect

Active Publication Date: 2010-04-07
中科润资科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] Compared with the supercritical drying process, the preparation of SiO by atmospheric pressure drying 2 Airgel greatly reduces the cost and operational risk, the equipment used is simple and can be produ

Method used

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  • Method for preparing silica aerogel material
  • Method for preparing silica aerogel material
  • Method for preparing silica aerogel material

Examples

Experimental program
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Example Embodiment

[0044] Example 1

[0045] The molar ratio of raw materials is TEOS: EtOH: MTMS: H 2 O=1:10:0.3:8, add 5.5ml of TEOS and 14.4ml of absolute ethanol into the container to start stirring, then add 1.4ml of MTMS modifier, continue to stir, slowly add 4.5ml of Distilled water, after another 10 minutes, add hydrochloric acid alcohol solution evenly after stirring, adjust the pH value to make the pH value of the solution 1.5~2.0; after continuous stirring for 8 hours, slowly add a certain amount of ammonia water alcohol solution to make the final pH value of the system 7.5~ 8.0. After 10min, stop stirring and add SiO 2 Pour the sol into the mold and let it stand for about 1 hour until the sample gels. After the gel is formed, soak the wet gel in the ethanol solution and leave it for aging. The aging temperature is 55℃ and the aging time is 5h; after aging, the gel is immersed in the secondary mixing modification solution, and the components of the secondary modification solution The vo...

Example Embodiment

[0050] Example 2

[0051] The molar ratio of raw materials is TEOS: EtOH: MTES: H 2 O=1:10:0.4:6, add 5.5ml of TEOS and 14.4ml of absolute ethanol into the container to start stirring, then add 2ml of MTES modifier, continue to stir, slowly add 2.7ml of distilled water after 15min After stirring, add the hydrochloric acid alcohol solution dropwise to adjust the pH value to about 2.0; after continuous stirring for 8-10 hours, slowly add a certain amount of ammonia water alcohol solution to make the final pH value of the system about 8.0. Stop stirring after a few minutes, and add SiO 2 Pour the sol into the mold and let it stand for about 1 hour until the sample gels. The wet gel is soaked in ethanol solution for aging, the aging temperature is 50℃, and the aging time is 6h; after aging, the gel is immersed in the secondary mixing modification solution. The components of the secondary modification solution are TMCS: Anhydrous ethanol: n-hexane = 2:3:15; modified for 1 to 2 days u...

Example Embodiment

[0053] Example 3

[0054] The molar ratio of raw materials is TEOS: EtOH: MTMS: H 2 O=1:10:0.3:10, add 5.5ml of TEOS and 14.4ml of absolute ethanol to the container to start stirring, then add 1.1ml of MTMS modifier, continue to stir, slowly add 3.6ml of Distilled water, after another 15 minutes, evenly add the hydrochloric acid dilute alcohol solution, adjust the pH value of the solution at 1.5 ~ 2.0; control the stirring speed at 300 ~ 400 rpm / min, and continuously stir for 8 hours, then slowly add a certain amount of ammonia water dilute alcohol solution to make The final pH value of the system is between 7.5 and 8.0. After 10 minutes, the stirring is stopped and the SiO 2 Pour the sol into the mold and let it stand for about 1 hour until the sample gels. After the gel is formed, add a small amount of ethanol to the mold to soak the gel in ethanol for aging, and age at 60°C for about 6 hours; then use the prepared secondary modification solution for sealing modification. The p...

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Abstract

The invention discloses a method for preparing a silica aerogel material and relates to the method for preparing the aerogel material, in particular to the method for rapidly preparing a transparent SiO2 aerogel by being based on the sol-gel technology and adopting secondary modification and normal pressure drying. The invention provides the method for preparing the silica aerogel material, and the method has simple technology, short cycle, low cost and good safety and is conductive to large-scale production. Tetraethoxysilane is adopted as a silicon source, methyl trimethoxysilane or methyl triethoxysilane is taken as a modifier of a co-precursor, anhydrous ethanol is taken as a solvent, and hydrochloric acid and ammonia are taken as catalysts. The sol-gel acid-base two-step method is adopted for catalysis, thereby preparing the SiO2 wet gel; and the further modification is carried out on a wet gel sample after aging treatment under certain conditions, and the normal pressure low-temperature drying is finally carried out in air atmosphere, thereby preparing the SiO2 aerogel. The equipment cost during the preparation technology is low, the product has good performances and the reaction process is controllable.

Description

technical field [0001] The invention relates to a preparation method of an airgel material, in particular to a method based on sol-gel technology and adopting secondary modified atmospheric pressure drying to rapidly prepare transparent SiO 2 Airgel method. Background technique [0002] Airgel is the lightest solid known in the world, and it is included in the Guinness Book of World Records. Airgel is mainly divided into inorganic oxide aerogel, organic aerogel and carbon gas obtained by carbonization of organic aerogel. gel. Silicon dioxide (SiO 2 ) airgel was first prepared by Kistler of Stanford University in 1931 through sol-gel method and supercritical drying technology. [0003] SiO 2 Airgel is a kind of material with high specific surface area (500~1500m 2 / g), high porosity (80%~99.8%), low density (~0.03g / cm 3 ), low refractive index (1~1.1), low thermal conductivity (~0.01W·m -1 ·K -1 ), low dielectric constant (1.0-2.0) and other nano-porous solid material...

Claims

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Application Information

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IPC IPC(8): C01B33/14
Inventor 程璇吴国友余煜玺张颖
Owner 中科润资科技股份有限公司
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