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A kind of atmospheric pressure preparation method of transparent silica block airgel

A technology of silica and gel, applied in the field of normal pressure preparation of transparent silica block aerogel, can solve problems such as shortening the production cycle, and achieve the effect of excellent physical and structural properties

Active Publication Date: 2019-01-15
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a normal-pressure preparation method of transparent silica block airgel, modifying the surface by classification, eliminating the low surface tension solvent replacement process in the later stage of the gel, shortening the production cycle, and overcoming It solves the problems of powder and small pieces prepared by the general atmospheric pressure drying method, and realizes the preparation of monolithic SiO by atmospheric pressure drying. 2 airgel material

Method used

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  • A kind of atmospheric pressure preparation method of transparent silica block airgel
  • A kind of atmospheric pressure preparation method of transparent silica block airgel
  • A kind of atmospheric pressure preparation method of transparent silica block airgel

Examples

Experimental program
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Effect test

Embodiment 1

[0041] At 50°C, mix and stir ethyl orthosilicate, ethanol, and deionized water in a molar ratio of 1:6:3, add hydrochloric acid to adjust the pH to 3, and stir for 30 minutes; add ammonia water to the obtained sol to adjust the pH to 6.5 , after stirring evenly, stand still and seal to obtain a wet gel, add absolute ethanol and age in a water bath at 50°C for 12 hours to obtain an alcohol gel. Add a surface modification solution mixed with trimethylchlorosilane, n-hexane, and ethanol in a water bath at 50°C. The concentration of the silane coupling agent is 0.6 mol / L for 6 hours of initial modification, and continue to add 0.8 mol / L L surface modification solution for 8 hours of modification, at this time the light blue transparent gel is separated from the mold and suspended in the surface modification solution; continue to add 1mol / L surface modification solution for the third modification modification, modification time 8 Hours, during which the gel turns from transparent t...

Embodiment 2

[0044] At room temperature, mix and stir ethyl orthosilicate, ethanol, and deionized water according to the molar ratio of 1:10:5, add hydrochloric acid to adjust the pH to 2, and stir for 60 minutes; add ammonia water to the obtained sol to adjust the pH to 7, After stirring evenly, leave it to stand and seal to obtain a wet gel, add absolute ethanol and age at room temperature for 3 days to obtain an alcohol gel. Add trimethylchlorosilane / n-hexane / ethanol mixed surface modification solution in a water bath at 50°C. The concentration of the modification agent is 0.8mol / L for 8 hours of initial modification. At this time, the wet gel is still transparent; remove Reaction by-products, continue to add 0.8mol / L surface modification solution, carry out the second modification for 8 hours, the wet gel will gradually turn white from transparent, remove reaction by-products, continue to add 1.5mol / L surface modification solution , carry out the third to fifth hydrophobic modification...

Embodiment 3

[0047] At room temperature, mix and stir ethyl orthosilicate, ethanol, and water according to the molar ratio of 1:10:5, add hydrochloric acid dropwise to adjust the pH to 2, and stir for 60 minutes; add ammonia water to adjust the pH to 7, stir well, and let stand Seal it to obtain a wet gel, add absolute ethanol and age at room temperature for 3 days to obtain an alcohol gel. At room temperature, add trimethylchlorosilane / n-hexane / ethanol mixed surface modification solution to the alcohol gel, the concentration of the modification agent is 0.5mol / L, and carry out the initial hydrophobic modification for 12 hours, until the light blue transparent gel detaches The mold floats in the surface modification solution, and the gel is still transparent at this time; pour off the surface modification solution, then add 1mol / L surface modification solution, carry out the second hydrophobic modification for 8 hours, pour off the surface modification solution, and add 1.5 mol / L surface m...

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Abstract

The invention discloses a normal pressure preparation method for transparent silica bulk aerogel and belongs to the field of silica aerogel. The method comprises the following steps: firstly, dissolving organo-siloxane and alcohol in deionized water so as to obtain a mixed solution; adding an acid catalyst into the mixed solution, and stirring so as to obtain silica sol; adding a basic catalyst into the silica sol, stirring, sealing, and standing so as to obtain silica gel; performing ageing, grading surface modification and solvent replacement on the silica gel so as to obtain modified wet gel; and finally, cleaning the modified wet gel by using a non-polar solvent, and performing graded drying, thereby obtaining the transparent silica bulk aerogel. The silica aerogel prepared by the method is crack-free transparent silica bulk aerogel and has excellent physical and structural performances.

Description

technical field [0001] The invention relates to the preparation of silica airgel, in particular to a method for preparing transparent silica block airgel at normal pressure. Background technique [0002] Silicon dioxide (SiO 2 ) Airgel is a lightweight nanoporous amorphous solid material with a space network structure composed of colloidal particles or polymer molecules cross-linked with each other. Its porosity can reach 80%-99.9%, and the pore size and skeleton particle size are between 1-100nm and 1-50nm respectively. Silica airgel has many unique properties, such as high specific surface area and high porosity. , high thermal insulation, low density, etc., and its performance can be continuously adjusted with the control of its structure. The excellent performance of silica airgel makes it have extensive and huge application prospects in the fields of optics, heat insulation, acoustics, catalyst carrier, microelectronics, chemical industry, aerospace and other fields. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/16
CPCC01B33/163C01P2006/10C01P2006/12C01P2006/14C01P2006/16C01P2006/32
Inventor 郭建军李杰许高杰
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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