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Hydrophobic high-elasticity methylsilsesquioxane aerogel block and preparation method thereof

A technology of sesquioxane and methyltrimethoxysilane, which is applied in the field of preparation of airgel materials, can solve the problems of slowly increasing pH and affecting the purity and performance of MSQ airgel, and achieves simple operation, safety and The effect of high reliability, good hydrophobicity and high elasticity

Active Publication Date: 2018-05-08
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 certain limitations in production. Although urea can slowly increase the pH as a gel accelerator, a large amount of urea will remain in the MSQ airgel during the preparation process and introduce a large amount of impurities. Thus affecting the purity and performance of MSQ airgel

Method used

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  • Hydrophobic high-elasticity methylsilsesquioxane aerogel block and preparation method thereof
  • Hydrophobic high-elasticity methylsilsesquioxane aerogel block and preparation method thereof
  • Hydrophobic high-elasticity methylsilsesquioxane aerogel block and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0036] 1) Add 0.32g of cetyltrimethylammonium chloride to 6 mL to a concentration of 5*10 -4 mol•L -1 Hydrochloric acid solution, then 1.25 mL of MTMS and 0.75 mL of DMDMS two precursors, magnetically stirred for 60 min under airtight conditions, then added 1.5 mL of gelling accelerator 1,2-propylene oxide, magnetically stirred for 1~2 set to 40 after min o Gel in oven C for 2 hours, and age for 3 days;

[0037] The reaction in step 1 is all carried out at room temperature, and the reaction is carried out in an airtight container.

[0038] 2) The gel formed in step 1) was subjected to three solvent replacements with isopropanol to obtain a solvent-substituted gel;

[0039] The process of solvent replacement is to pour out the original solvent, pour it into isopropanol, and put it back into the oven after sealing it. The interval between each solvent replacement is 12~24h.

[0040] 3) Place the gel after solvent replacement at 40 o C drying slowly in an oven for 1 day to obt...

Embodiment 2

[0051] 1) Add 0.28g of cetyltrimethylammonium chloride to 5 mL to a concentration of 4*10 -4 mol•L -1 hydrochloric acid solution, then 1 mL of MTMS and 1 mL of DMDMS two precursors, magnetically stirred for 30 min under airtight conditions, then added 1.2 mL of gel accelerator 1,2-propylene oxide, and magnetically stirred for 1-2 set to 40 after min o Gel in oven C for 3 hours and age for 2 days;

[0052] The reaction in step 1 is all carried out at room temperature, and the reaction is carried out in an airtight container.

[0053] 2) The gel formed in step 1) is subjected to secondary solvent replacement with isopropanol to obtain the gel after solvent replacement;

[0054] The process of solvent replacement is to pour out the original solvent, pour it into isopropanol, and put it back into the oven after sealing it. The interval between each solvent replacement is 12~24h.

[0055] 3) Place the gel after solvent replacement at 45 o C drying slowly in an oven for 1.5 day...

Embodiment 3

[0057] 1) Add 0.36g of cetyltrimethylammonium chloride to 8 mL to a concentration of 6*10 -4 mol•L -1 hydrochloric acid solution, then 1.1 mL of MTMS and 0.9 mL of DMDMS two precursors, magnetically stirred for 70 min under airtight conditions, then added 1.6 mL of gelling accelerator 1,2-propylene oxide, and magnetically stirred for 1-2 set to 50 after min o Gel in C oven for 3.5h, aging for 4d;

[0058] The reaction in step 1 is all carried out at room temperature, and the reaction is carried out in an airtight container.

[0059] 2) The gel formed in step 1) was subjected to solvent replacement four times with isopropanol to obtain a gel after solvent replacement;

[0060] The process of solvent replacement is to pour out the original solvent, pour it into isopropanol, and put it back into the oven after sealing it. The interval between each solvent replacement is 12~24h.

[0061] 3) Place the gel after solvent replacement at 50 o C drying slowly in an oven for 2 days ...

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Abstract

The invention discloses a hydrophobic high-elasticity methylsilsesquioxane aerogel block and a preparation method thereof. The aerogel block is a compound with methyltrimethoxysilane and dimethoxydimethylsilane as a co-precursor, a hydrochloric acid solution HCl as a solvent and a catalyst and cetyltrimethylammonium chloride as a dispersant. The preparation method includes the following steps: adding cetyltrimethylammonium chloride into the hydrochloric acid solution, then adding the precursor, carrying out magnetic stirring under a closed condition, adding a gel accelerator, then stirring again, placing in a drying oven, gelling and aging; carrying out solvent replacement of the gel formed in the step 1) with isopropanol for at least two times, to obtain a gel after solvent replacement; and placing the gel after solvent replacement in a drying oven, and drying to obtain the complete hydrophobic high-elasticity methylsilsesquioxane aerogel block. Through the way, the methylsilsesquioxane aerogel block with good hydrophobicity and high elasticity can be obtained under the condition of ambient pressure drying.

Description

technical field [0001] The invention belongs to the field of preparation of airgel materials, and in particular relates to a hydrophobic and highly elastic 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 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B26/32C04B38/00
CPCC04B26/32C04B2201/20C04B2201/50C04B24/121C04B24/00C04B38/00
Inventor 郭兴忠单加琪雷伟赖中掌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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