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Ultralow-density transparent silicon dioxide aerogel capable of being post-cleaned as well as preparation method and application of ultralow-density transparent silicon dioxide aerogel

An ultra-low density, silicon dioxide technology, applied in chemical instruments and methods, inorganic chemistry, silicon compounds, etc., can solve the problems of space dust capture final result analysis interference, affect the cleanliness and transparency of airgel, etc., to overcome hydrophobic The effect of non-uniformity and simplified process operation

Active Publication Date: 2021-02-02
AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is worth noting that during the preparation, assembly, transportation and use of ultra-low-density transparent silica aerogels, it is impossible to operate in an ultra-clean room, and pollutants such as dust in the environment will inevitably fall and accumulate. to the surface of the aerogel, which will greatly affect the cleanliness and transparency of the aerogel, and even cause great interference to the capture of space dust and the analysis of the final results. No relevant research has yet noticed this problem

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  • Ultralow-density transparent silicon dioxide aerogel capable of being post-cleaned as well as preparation method and application of ultralow-density transparent silicon dioxide aerogel
  • Ultralow-density transparent silicon dioxide aerogel capable of being post-cleaned as well as preparation method and application of ultralow-density transparent silicon dioxide aerogel
  • Ultralow-density transparent silicon dioxide aerogel capable of being post-cleaned as well as preparation method and application of ultralow-density transparent silicon dioxide aerogel

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preparation example Construction

[0032]In the first aspect, the present invention provides a method for preparing a post-cleanable ultra-low density transparent silica aerogel. The method includes the following steps:

[0033](1) Use the first organic solvent to mix methyl orthosilicate (TMOS), citric acid and water uniformly to obtain a first reaction system. The first reaction system is subjected to pre-hydrolysis reaction and distillation treatment in sequence to obtain a precursor liquid A; In the present invention, for example, use the first organic solvent to mix methyl orthosilicate (TMOS), citric acid and water uniformly, carry out the pre-hydrolysis reaction at 50~70℃ for 12h, and completely distill out at 80℃ The methanol generated by the pre-hydrolysis of the first organic solvent and methyl orthosilicate to obtain the precursor liquid A; in the present invention, the time of the distillation treatment is, for example, to completely distill off the first organic solvent and the methyl orthosilicate The meth...

Embodiment 1

[0059]①Add 15.2g of methyl orthosilicate (0.1mol), citric acid (0.004mol), 5.4g of water (0.3mol), and 9.6g of methanol (0.3mol) into a single-necked flask, stir and mix with magnetic force, and heat to 60 ℃, the reflux reaction (pre-hydrolysis reaction) at this temperature for 12h, change the reflux device to a distillation device, raise the temperature to 80°C, and completely distill out the methanol in the reaction solution to obtain precursor fluid A and each group of precursor fluid A The raw materials are divided into molar ratio of methyl orthosilicate: citric acid: water: methanol 1:0.04:3:3.

[0060]②Add 10.5g of decyltrimethoxysilane (0.04mol), 2.3g of perfluorodecyltrimethoxysilane (0.004mol), 7.2g of polyvinylpyrrolidone (molecular weight 24kDa, 0.0003mol) to the precursor fluid A, respectively, 105.6g n-pentanol (1.2mol), magnetic stirring and mixing, heating to 60℃, reflux reaction (pre-hydrolysis reaction) at this temperature for 2h to obtain mixture B. The raw materials...

Embodiment 2

[0066]Embodiment 2 is basically the same as embodiment 1, except that:

[0067]In step ①, add 15.2g of methyl orthosilicate (0.1mol), citric acid (0.001mol), 3.6g of water (0.2mol), and 9.6g of methanol (0.3mol) into a single-necked flask, stir and mix evenly. , Heat up to 60℃, reflux reaction (pre-hydrolysis reaction) at this temperature for 12h, change the reflux device to a distillation device, raise the temperature to 80℃, and completely distill the methanol in the reaction solution to obtain precursor liquid A, precursor liquid The raw materials of each component in A are 1:0.01:2:3 in molar ratio of methyl orthosilicate: citric acid: water: methanol.

[0068]In step ②, add 5.25g decyltrimethoxysilane (0.02mol), 1.15g perfluorodecyltrimethoxysilane (0.002mol), 2.4g polyvinylpyrrolidone (molecular weight 24kDa, 0.0001mol), 105.6g n-pentanol (1.2mol), magnetic stirring and mixing, heating to 60℃, reflux reaction (pre-hydrolysis reaction) at this temperature for 2h to obtain mixed liqui...

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Abstract

The invention relates to ultralow-density transparent silicon dioxide aerogel capable of being post-cleaned as well as a preparation method and application of the ultralow-density transparent silicondioxide aerogel. The method comprises the steps that a system composed of methyl orthosilicate, citric acid, water and a first organic solvent and a system composed of long-chain alkyl trimethoxy silane, perfluoro long-chain alkyl trimethoxy silane, polyvinylpyrrolidone, a 1, 4-dioxane solution of ammonia and a second organic solvent are subjected to a graded sol-gel reaction, and wet gel is obtained; the wet gel is placed in mother liquor containing high-concentration ammonia to be aged at the high temperature, and structure-enhanced alcohol gel is obtained; and gradient solvent replacement is carried out on the structure-enhanced alcohol gel, and normal-pressure drying is carried out to obtain the ultralow-density transparent silicon dioxide aerogel capable of being post-cleaned. The silicon dioxide aerogel prepared by the invention shows super-hydrophobic and super-oleophobic dual characteristics, has unique post-cleaning and reuse performance, and has high application value in thefields of new generation deep space exploration, high-energy physics and the like.

Description

Technical field[0001]The invention belongs to the technical field of nanoporous materials, and relates to a preparation method of silica aerogel, in particular to a post-cleanable ultra-low density transparent silica aerogel, and a preparation method and application thereof.Background technique[0002]Ultra-low density transparent silica aerogel is an important member of the silica aerogel family. It has an ultra-low density (10~50mg / cm) that conventional silica aerogels do not have.3) And ultra-high transparency (transmittance of 85%-95%), the two most significant features, which make it has important scientific research and practical application value in the field of deep space exploration. The capture of high-speed particles in space is ultra-low-density transparent gas. Gel is the most common application scenario in the field of deep space exploration. On the one hand, ultra-low-density silica aerogel has ultra-high porosity, and the three-dimensional network porous solid framewor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/158
CPCC01B33/1585C01P2006/10C01P2006/60C01P2006/32
Inventor 张晚林刘圆圆李文静张恩爽纪旭阳杨洁颖赵英民张昊
Owner AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH