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High-specific-surface-area mesoporous methylsilsesquioxane aerogel block and preparation method thereof

A technology of mesoporous methyl silicon and sesquioxane, which is applied in ceramic products, other household appliances, applications, etc., can solve problems such as hidden safety hazards, flammability of petroleum ether, etc., and achieve the effect of high safety and reliability, and simple operation.

Active Publication Date: 2018-03-06
PAN ASIAN MICROVENT TECH JIANGSU CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has great limitations in industrial production. Both hydrofluoric acid and tetraethylammonium hydroxide are highly corrosive, and petroleum ether is extremely flammable, which will cause potential safety hazards in industrial production.

Method used

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  • High-specific-surface-area mesoporous methylsilsesquioxane aerogel block and preparation method thereof
  • High-specific-surface-area mesoporous methylsilsesquioxane aerogel block and preparation method thereof
  • High-specific-surface-area mesoporous methylsilsesquioxane aerogel block and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 1) Add 0.24 g of cetyltrimethylammonium chloride to 6 mL with a concentration of 5*10 -4 mol•L -1 In the hydrochloric acid solution, stir to dissolve, then add 3 mL of precursor methyltrimethoxysilane (MTMS), stir magnetically for 60 min under sealed conditions, then add 1.0 mL of 1,2-propylene oxide (PO), stir for 1 ~2 min, put in 40 o Aging in C oven for 2 to 3 days;

[0036] 2) The gel formed in step 1) was subjected to three solvent replacements with isopropanol to obtain a solvent-substituted gel;

[0037] 3) Use a mixture of hexamethyldisiloxane (HMDSO) / isopropanol with a volume ratio of 0.8:20 to modify the surface of the gel after solvent replacement in step 2) to obtain a surface-modified gel ;

[0038] 4), Step 3) The gel after surface modification is subjected to 40~60 o C dried under normal pressure for 1 day to obtain a complete high-surface mesoporous methylsilsesquioxane airgel block.

[0039] figure 1 For the scanning electron micrograph of the MSQ ...

Embodiment 2

[0049] 1) Add 0.2g of cetyltrimethylammonium chloride to 4 mL with a concentration of 4*10 -4 mol•L -1 Stir to dissolve in the hydrochloric acid solution, then add 2 mL of precursor methyltrimethoxysilane (MTMS), stir magnetically for 30 min under sealed conditions, then add 0.5 mL of 1,2-propylene oxide (PO), stir 1~2 min, put in 45 o Aging in C oven for 2 to 3 days;

[0050] 2) For the gel formed in step 1), use isopropanol for secondary solvent replacement to obtain the gel after solvent replacement. The solvent replacement process is to pour out the original solvent, pour isopropanol, and put it back after sealing. In the oven, the interval between each solvent replacement is 12~24h;

[0051] 3) Use a mixture of hexamethyldisiloxane (HMDSO) / isopropanol with a volume ratio of 0.8:20 to modify the surface of the gel after solvent replacement in step 2) to obtain a surface-modified gel ;

[0052] 4), Step 3) The gel after surface modification is subjected to 40~60 o C d...

Embodiment 3

[0054] 1) Add 0.3g of cetyltrimethylammonium chloride to 8 mL with a concentration of 6*10 -4 mol•L -1 Stir to dissolve in the hydrochloric acid solution, then add 5 mL of precursor methyltrimethoxysilane (MTMS), stir magnetically for 60 min under sealed conditions, then add 1.5 mL of 1,2-propylene oxide (PO), stir for 1 ~2 min, put in 50 o Aging in C oven for 2 to 3 days;

[0055] 2) For the gel formed in step 1), use isopropanol to perform solvent replacement four times to obtain the gel after solvent replacement. The solvent replacement process is to pour out the original solvent, pour isopropanol, and put it back after sealing. In the oven, the interval between each solvent replacement is 12~24h;

[0056] 3) Use a mixture of hexamethyldisiloxane (HMDSO) / isopropanol with a volume ratio of 0.8:20 to modify the surface of the gel after solvent replacement in step 2) to obtain a surface-modified gel ;

[0057] 4), Step 3) The gel after surface modification is subjected to...

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Abstract

The invention discloses a high-specific-surface-area mesoporous methylsilsesquioxane aerogel block, wherein the high-specific-surface-area mesoporous methylsilsesquioxane aerogel block is a compound taking methyltrimethoxysilane as a precursor, a hydrochloric acid solution as a solvent and a catalyst, and hexadecyl trimethyl ammonium chloride as a dispersing agent; a preparation method comprises the following steps: adding the dispersing agent into the hydrochloric acid solution, stirring to dissolve, then adding the precursor methyltrimethoxysilane, magnetically stirring under the sealed connection, then adding a gel accelerator, continuing to stir, ageing in an oven after finishing stirring; conducting solvent replacement on a gel through isopropanol for at least twice to obtain a solvent replaced gel; modifying the surface of the solvent replaced gel to obtain a surface modified gel; drying at the normal temperature to obtain the integrated high-specific-surface-area mesoporous methylsilsesquioxane aerogel block. Through the above mode, the high-purity high-specific-surface-area mesoporous methylsilsesquioxane aerogel block with a uniform mesoporous structure is prepared.

Description

technical field [0001] The invention relates to the field of airgel materials, in particular to a high specific surface mesoporous methylsilsesquioxane airgel block and a preparation method thereof. Background technique [0002] At the beginning of the 20th century, it was believed that airgel is a material with nanoporous network structure prepared by sol-gel process and supercritical drying process. The one obtained by evaporation and drying is called xerogel, and the one obtained by freeze drying is called It is cryogel. Now, it is believed that the drying process in the airgel preparation process is not necessarily supercritical drying. No matter what drying technology is used, as long as the liquid in the wet gel network is replaced by gas, the spatial network structure of the gel remains basically unchanged. , This material composed of solid and gas is called aerogel. [0003] Silica airgel is a low-density, porous nano-solid material with a unique nano-scale three-d...

Claims

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Application Information

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IPC IPC(8): C04B26/32C04B38/00
CPCC04B26/32C04B24/121C04B24/00C04B38/00
Inventor 郭兴忠单加琪雷伟高文炜王海文王世林张云王爱国丁荣华李建革邹东伟
Owner PAN ASIAN MICROVENT TECH JIANGSU CORP
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