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Ultra low density aerogel material, and preparation method and applications thereof

An ultra-low density, aerogel technology, applied in chemical instruments and methods, inorganic chemistry, non-metallic elements, etc., can solve problems such as high cost, difficulty in size control, and no reports on the application of large-scale materials, and achieve high Effects of Strength and Flexibility, Significant Application Prospects

Active Publication Date: 2019-10-15
AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, domestic research on ultra-low-density aerogels focuses on small samples and performance research in the laboratory, and there are no reports on the application of large-scale materials.
This preparation technology also has the following disadvantages: 1) the product size shrinkage rate is 15%, and the size shrinkage will bring greater difficulty to the size control in material application; 2) the product yield is low, and the literature reports only about 25%, resulting in Product production efficiency is low, cost is high; 3) this preparation method can only use supercritical ethanol drying technology, in supercritical CO 2 Under these conditions, ultra-low density aerogels are prone to cracks and become powder materials.

Method used

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  • Ultra low density aerogel material, and preparation method and applications thereof
  • Ultra low density aerogel material, and preparation method and applications thereof
  • Ultra low density aerogel material, and preparation method and applications thereof

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preparation example Construction

[0020] The present invention provides a kind of preparation method of ultra-low density airgel material in the first aspect, described method comprises the steps:

[0021] (1) Preparation of the sol precursor: add methyl orthosilicate, methanol and hydrochloric acid and mix together for reaction, then distill off the methanol, then add acetonitrile to obtain the sol precursor;

[0022] (2) Preparation of silica sol: mix the sol precursor with ammonia water, then add acetonitrile to prepare silica sol;

[0023] (3) Gelling and aging: gelling and aging the silica sol in turn to obtain a wet gel material;

[0024] (4) Moisture-proof treatment: using a hydrophobic agent to perform hydrophobic treatment on the wet gel material to obtain a hydrophobized gel material;

[0025] (5) Solvent replacement: performing solvent replacement on the hydrophobized gel material to obtain a solvent replacement gel;

[0026] (6) Supercritical drying: the solvent-displaced gel is put into a drying...

Embodiment 1

[0057] First prepare a concentration of 3*10 -3 mol / L hydrochloric acid, 0.6mol / L ammonia solution. The mass ratio of methyl orthosilicate:methanol:hydrochloric acid is 5:3:1, and the reaction temperature is 50°C in an oil bath for 24 hours; afterward, distillation is carried out at a distillation temperature of 80°C, and 70% of the silicon source is distilled. After mass % of methanol solvent, add acetonitrile solvent whose mass is twice as much as methyl orthosilicate, and stir for 10 minutes to obtain the sol precursor; then mix the glue according to the mass ratio of sol precursor: acetonitrile: ammonia water is 1:5:0.1 , and stirred for 20 minutes to obtain a silica sol; pour the silica sol into a mold and place it at room temperature for 48 hours, then continue to age it at 50°C for 48 hours, remove the mold after aging, and add 10% by mass of hexamethyldisilazol Azane was put into ethanol solvent for hydrophobization treatment; supercritical CO was carried out after tw...

Embodiment 2

[0059] First prepare a concentration of 3.5*10 -3 mol / L hydrochloric acid, 0.7mol / L ammonia solution. The mass ratio of methyl orthosilicate:methanol:hydrochloric acid is 5:3:1, and the reaction temperature is 50°C in an oil bath for 24 hours; afterward, distillation is carried out at a distillation temperature of 80°C, and 70% of the silicon source is distilled. After mass % of methanol solvent, add acetonitrile solvent whose mass is twice as much as methyl orthosilicate, and stir for 10 minutes to obtain the sol precursor; then mix the glue according to the mass ratio of sol precursor: acetonitrile: ammonia water is 1:5:0.1 , stirred for 20 minutes to obtain silica sol; pour the silica sol into the mold; after standing at room temperature for 48 hours, continue to age at 50°C for 48 hours, remove the mold after aging, and add 10% by mass of hexamethyl di Silazane was placed in ethanol solvent for hydrophobization treatment; supercritical CO 2 Drying, feeding at a low tempe...

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Abstract

The invention provides a preparation method of an ultra low density aerogel material. The preparation method comprises following steps: a silicon source, methanol, and hydrochloric acid are added formixed reaction, distillation is carried out to remove methanol, and acetonitrile is added so as to obtain a sol precursor; the sol precursor is mixed with ammoniacal liquor, and acetonitrile is addedto prepare silica sol; the silica sol is subjected to gelling and aging successively so as to obtain a wet gel material; a hydrophobic agent is adopted for hydrophobization treatment of the wet gel material so as to obtain a hydrophobized gel material; the hydrophobized gel material is subjected to solvent displacement so as to obtain a solvent displaced gel; the solvent displaced gel is introduced into a drying kettle for supercritical drying so as to obtain the ultra low density aerogel material. The largest complete size of the ultra low density aerogel material is 300mm*300mm, the thickness ranges from 10 to 30mm; the density is lower than 20kg / m3, the size shrinkage rate is lower than 1%, the agglutinable volatile matter content is 0.06% or lower. The invention also provides applications of the ultra low density aerogel material in the field of deep space detection.

Description

technical field [0001] The invention belongs to the field of thermal protection, in particular to the technical field of thermal protection materials for thermal control systems used in deep space exploration, and specifically relates to an ultra-low-density airgel material and its preparation method and application. Background technique [0002] Airgel material is a new type of low-density nanoporous material. It is the solid material with the best thermal insulation performance. Airgel is formed by the mutual accumulation of nanoparticles and has a three-dimensional network nanoporous structure. The Lawrence Livermore National Laboratory of the United States was the first to achieve a breakthrough in the preparation of ultra-low-density silica airgel, and the density of the prepared airgel material can be as low as 3kg / m 3 . The U.S. Jet Propulsion Laboratory used the laboratory technology to realize the application of ultra-low-density aerogels in the aerospace field; in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/145C01B33/158C01B33/159
CPCC01B33/145C01B33/1585C01B33/159C01P2006/10C01P2006/90
Inventor 张丽娟李健李文静孙阔杨洁颖赵英民
Owner AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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