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Microwave-assisted production method of aerogel and methylsilsesquioxane aerogel

A microwave-assisted, production method technology, applied in the field of methyl silsesquioxane airgel, can solve the problems of reducing drying time, etc., and achieve the effects of reduced production time, excellent performance and efficient preparation

Active Publication Date: 2022-01-25
PAN ASIAN MICROVENT TECH JIANGSU CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to overcome the above problems, the prior art uses water glass as a precursor to prepare airgel materials by microwave heating and curing, solvent replacement and drying, which greatly reduces the drying time. However, due to the use of water glass as a precursor, even microwave curing Its gel time is still as long as 2~3h

Method used

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  • Microwave-assisted production method of aerogel and methylsilsesquioxane aerogel
  • Microwave-assisted production method of aerogel and methylsilsesquioxane aerogel
  • Microwave-assisted production method of aerogel and methylsilsesquioxane aerogel

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Effect test

Embodiment 1

[0031] A microwave-assisted production method of methylsilsesquioxane airgel, comprising the following steps:

[0032] 1) Add the template agent dodecyltrimethylammonium chloride to the hydrochloric acid solution; then add methyltrimethoxysilane and dimethyldimethoxysilane as precursors, the volume ratio of the precursors is 1:2, after magnetic stirring for 30 minutes under airtight conditions, add 0.8 mL propylene oxide gel accelerator to the solvent at the ratio of 0.8 mL per 5 mL of solvent, stir again and put it into a microwave device for gelation and aging; The time for gelation and aging is 15 minutes, and the microwave frequency is 500 W;

[0033] 2) The gel formed in step 1) was replaced by isopropanol solvent under the assistance of microwave to obtain the gel after sol replacement; the number of solvent replacement was 2 times, the microwave-assisted replacement time was 3-5 min, and the microwave frequency was 500W;

[0034] 3) Place the gel after solvent replace...

Embodiment 2

[0039] A microwave-assisted production method of methylsilsesquioxane airgel, comprising the following steps:

[0040] 1) Add the template agent dodecyltrimethylammonium chloride to the mixed solution of hydrochloric acid and methanol, then add methyltrimethoxysilane as the precursor, the volume ratio of the precursor is 1:2, After magnetic stirring for 30 min under airtight conditions, add 1 mL of propylene oxide gel accelerator into the solvent according to the ratio of 1 mL of propylene oxide gel accelerator for every 6 mL of solvent, stir again and put it into microwave for gelation and aging; gelation, aging The time is 10 min, and the microwave frequency is 750 W;

[0041] 2) The gel formed in step 1) was replaced by isopropanol solvent under the assistance of microwave to obtain the gel after sol replacement; the number of solvent replacement was 2 times, the microwave-assisted replacement time was 3-5 min, and the microwave frequency was 750W;

[0042] 3) Place the g...

Embodiment 3

[0047] A microwave-assisted production method of methylsilsesquioxane airgel, comprising the following steps:

[0048] 1) Add the template agent dodecyltrimethylammonium chloride to the mixed solution of acetic acid and methanol; then add methyltriethoxysilane as a precursor, the volume ratio of the precursor is 1:2 ; After magnetically stirring for 30 min under airtight conditions, add 1.5 mL of propylene oxide gel accelerator to the solvent at a ratio of 1.5 mL per 8 mL of solvent, stir again and put it in a 40°C oven for gelation and aging for 1.5 hours.

[0049] 2) The gel formed in step 1) was replaced by methanol solvent twice in an oven at 40°C, 8~24h / time, and then replaced by isopropanol and n-heptane at 60°C for 2~3 times, 8~ 24 h / time.

[0050] 3) The gel after solvent replacement was placed in a microwave drying equipment for microwave drying, the drying time was 30 min, and the microwave frequency was 500 W.

[0051] Figure 5 It is a scanning electron microgra...

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Abstract

The invention discloses a microwave-assisted production method of airgel and methyl silsesquioxane airgel, comprising the following steps: adding a template agent into a solvent, then adding a precursor containing methyl silicon alkoxide, sealing the After magnetic stirring under certain conditions, add a gel accelerator, stir again evenly, and then put it into a microwave for gelation and aging; perform solvent replacement on the formed gel under the assistance of microwaves to obtain a gel after sol replacement; The replaced gel was placed in a microwave oven for microwave drying. Through the above method, the present invention realizes the continuous and efficient preparation of various aerogels with the assistance of microwave technology, which greatly reduces the production time, and at the same time, the prepared methylsilsesquioxane aerogel retains the nanoporous structure, Has excellent performance.

Description

technical field [0001] The invention relates to a microwave-assisted production method of airgel and methylsilsesquioxane airgel. Background technique [0002] Traditional silica airgel usually uses supercritical drying to prevent the collapse of the pore structure during drying. It is mainly divided into two types: ethanol supercritical drying and carbon dioxide supercritical drying. The principle is similar, that is, through specific temperature and pressure. The supercritical ethanol or carbon dioxide fluid replaces the original solvent in the wet gel, and the supercritical fluid avoids the surface tension of the solvent in the capillary structure during the removal process, effectively preventing the collapse of the airgel nanopore structure. [0003] For example, the invention patent (application number 201710454634.8) applied by He Song et al. of Wuhan University of Technology involves a drying method for silica airgel thermal insulation materials, which discloses that...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J9/26C08L83/04
CPCC08J9/26C08J2383/04C08J2205/026C08J2201/0424
Inventor 郭兴忠单加琪张云丁荣华
Owner PAN ASIAN MICROVENT TECH JIANGSU CORP
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