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Method for preparing modified silicon dioxide aerogel material through normal-pressure drying and by external circulation mode

A silica and aerogel technology, applied in chemical instruments and methods, inorganic chemistry, silicon compounds, etc., can solve the problems of increased cost, high cost of precursor tetraethyl orthosilicate, threats to the environment and operators, etc. , to achieve the effect of high cost

Active Publication Date: 2018-11-13
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the preparation period of this method is long, and the cost of the precursor tetraethyl orthosilicate used is relatively high, which is not conducive to large-scale industrial production
Trimethylchlorosilane itself is relatively active, and it can be hydrolyzed to generate corrosive hydrochloric acid gas when it meets water, which poses a serious threat to the environment and operators.
However, if organic solvents such as alcohols are used as solvents for exchanging pore water, the consumption of silane modifiers is still greater than the amount required for actual modification, resulting in the loss of silane surface modifiers, and correspondingly, the cost will be greatly increased. , limiting the popularization and use of airgel products

Method used

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  • Method for preparing modified silicon dioxide aerogel material through normal-pressure drying and by external circulation mode
  • Method for preparing modified silicon dioxide aerogel material through normal-pressure drying and by external circulation mode
  • Method for preparing modified silicon dioxide aerogel material through normal-pressure drying and by external circulation mode

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preparation example Construction

[0074] The invention provides a method for preparing a modified silica airgel material, comprising the following steps:

[0075] 1) Put the aged silica wet gel material and the modifier precursor in the reaction container, and at the same time, the modifier precursor is hydrolyzed by the external circulation, and then returned to the reaction container, and after the modification reaction, the improved Reactive silica airgel material;

[0076] The modifier is a modifier that can undergo polymerization reaction with water to generate a modifier precursor.

[0077] The modifying agent in the present invention is a modifying agent that can undergo polymerization reaction with water to generate a modifier precursor. The present invention is not particularly limited to the specific selection of the modifier, and it is sufficient to use conventional modifiers for hydrophobically modified silica aerogels well known to those skilled in the art, and those skilled in the art can accord...

Embodiment 1

[0138] Ⅰ. First dilute the water glass with water, take 1.2L of water glass and 6L of water, mix well and stir evenly to obtain the dilution of water glass. Slowly introduce the diluent of water glass into 244 mL of 10M hydrochloric acid solution to obtain a sol solution.

[0139] II. Adjust the pH of the sol solution obtained in I to 5.0 with 3M aqueous sodium hydroxide solution, and after stirring for several minutes, dip the glass fiber mat into the sol solution. After the sol solution is fully impregnated, the glass fiber mat is taken out, and the gel composite material is obtained by microwave irradiation treatment. The power of microwave irradiation is 0.4KW, and the microwave irradiation treatment time is 150s.

[0140] Ⅲ. Roll up the gel composite material obtained in Ⅱ and put it into the reaction kettle ①, aging at room temperature for 5 hours, then add HMDSO solution into the kettle until the wet gel composite material is just submerged.

[0141] Ⅳ. Then introduce ...

Embodiment 2

[0149] A method for preparing a silica airgel composite material by external circulation modified atmospheric pressure drying, comprising the steps of:

[0150] Ⅰ. First dilute the water glass with water, take 1.2L of water glass and 3.6L of water and fully mix and stir evenly to obtain the dilution of water glass. Slowly introduce the diluent of water glass into 710 mL of 5M hydrochloric acid solution to obtain a sol solution.

[0151] II. Adjust the pH of the sol solution obtained in I to 5.0 with diluted water glass solution, wherein the volume ratio of water glass to water is 3:1. After stirring for several minutes, the glass fiber mat is dipped into the sol solution. After the sol solution is fully impregnated, the glass fiber mat is taken out, and the gel composite material is obtained by microwave irradiation treatment. The power of microwave irradiation is 0.4KW, and the microwave irradiation treatment time is 60s.

[0152] Ⅲ. Roll up the gel composite material obtai...

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Abstract

The invention provides a preparation method of a modified silicon dioxide aerogel material. The preparation method comprises the following steps: placing an aged silicon dioxide wet gel and a modifierprecursor into a reaction container, performing external circulation hydrolysis on the modifier precursor, and returning to a reaction container and performing modified reaction to obtain the modified silicon dioxide aerogel material, wherein the modifier can encounter water to generate polymerization reaction to generate the modifier precursor. The traditional organic solvent exchange process link is abandoned, an external circulation one-step modification mode is adopted, the consumption quantity of the organic solvent is small, the cost is low, the environmental hazard is small, use and waste of the organic solvent in the link are avoided, a large amount of silane modifiers are saved for the subsequent surface modification process, the surface modification efficiency is improved, the cost is reduced and the environmental hazard is avoided; furthermore, the preparation method is short in preparation cycle, high in efficiency, simple and convenient to operate, mild in reaction condition and suitable for industrialized continuous production.

Description

technical field [0001] The invention relates to the technical field of high-performance porous materials, and relates to a preparation method of a modified silica airgel material. In particular, it relates to a method for preparing a modified silica airgel material by drying under normal pressure in an external circulation mode. Background technique [0002] Airgel, also known as xerogel, is a solid material form, a highly dispersed solid material that is composed of colloidal particles or polymer molecules aggregated into a nanoporous network structure, and filled with a gaseous dispersion medium in the pores , and one of the least dense solids among existing materials, aerogels have continuous mesoporous pores, which are nanostructures composed of interconnected nanoparticles or polymer chains with a characteristic diameter of about 10 nm. These nanostructures endow them with high surface area, relatively large pore volume, low packing density, and low thermal and acousti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/158
CPCC01B33/1585C01P2004/03C01P2006/12C01P2006/16C01P2006/17C01P2006/32
Inventor 张和平潘月磊程旭东龚伦伦
Owner UNIV OF SCI & TECH OF CHINA
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