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A post-cleanable ultra-low density transparent silica airgel and its preparation method and application

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 results analysis interference, affecting the cleanliness and transparency of aerogels, etc., to overcome hydrophobicity. The effect of reducing unevenness and simplifying process operation

Active Publication Date: 2022-02-15
AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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

Method used

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  • A post-cleanable ultra-low density transparent silica airgel and its preparation method and application
  • A post-cleanable ultra-low density transparent silica airgel and its preparation method and application
  • A post-cleanable ultra-low density transparent silica airgel and its preparation method and application

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preparation example Construction

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

[0033] (1) Use the first organic solvent to mix methyl orthosilicate (TMOS), citric acid and water evenly to obtain the first reaction system, which is subjected to pre-hydrolysis and distillation in sequence to obtain the 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 pre-hydrolysis reaction at 50-70°C for 12 hours, and completely distill out at 80°C The methanol produced by the pre-hydrolysis of the first organic solvent and methyl orthosilicate to obtain precursor liquid A; The methanol generated by pre-hydrolysis is the end point;

[0034] (2) Mix the precursor liquid A, long-chain alkyl trimethoxysilane, perfluoro long-chain alkyl trimethoxysilane and polyvinylpyrrolidone unif...

Embodiment 1

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

[0060]②Add 10.5g decyltrimethoxysilane (0.04mol), 2.3g perfluorodecyltrimethoxysilane (0.004mol), 7.2g polyvinylpyrrolidone (molecular weight 24kDa, 0.0003mol), 105.6g of n-amyl alcohol (1.2mol), magnetic stirring and mixing, heating up to 60°C, reflux reaction (pre-hydrolysis reaction) at this temperature for 2h, to obtain a mixed solution B, the raw materials of each component in the mixed soluti...

Embodiment 2

[0066] Embodiment 2 is basically the same as Embodiment 1, the difference is:

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

[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-amyl alcohol (1.2mol), magnetic stirring and mixing, heating up to 60°C, reflux reaction (pre-hyd...

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Abstract

The invention relates to a post-cleanable ultra-low density transparent silica airgel, a preparation method and application thereof. The method is as follows: a system composed of methyl orthosilicate, citric acid, water, and the first organic solvent and long-chain alkyl trimethoxysilane, perfluoro long-chain alkyl trimethoxysilane, polyvinylpyrrolidone, ammonia A system composed of 1,4-dioxane solution and a second organic solvent carries out a graded sol-gel reaction to obtain a wet gel; the wet gel is placed in a mother liquor containing high-concentration ammonia for aging at a high temperature, The structure-enhanced alcohol gel is obtained; the structure-enhanced alcohol gel is subjected to gradient solvent replacement, and then dried under normal pressure to obtain an ultra-low-density transparent silica airgel that can be post-cleaned. The silica airgel prepared by the present invention exhibits dual characteristics of superhydrophobic and superoleophobic, has unique post-cleaning and reusable properties, and has important applications in the fields of new generation deep space exploration and high energy physics value.

Description

technical field [0001] The invention belongs to the technical field of nanoporous materials, and relates to a preparation method of silica airgel, in particular to a post-cleanable ultra-low density transparent silica airgel and its preparation method and application. Background technique [0002] Ultra-low density transparent silica airgel is an important member of the silica airgel family, with ultra-low density (10-50mg / cm 3 ) and ultra-high transparency (light transmittance 85% to 95%) are the two most notable characteristics, which make it have important scientific research and practical application value in the field of deep space exploration. The capture of space high-speed particles is an 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 airgel has ultra-high porosity, and the three-dimensional network porous solid skeleton composed of silica nanoparticles i...

Claims

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Application Information

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Patent Type & Authority Patents(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
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