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A kind of tough polymer/cage silsesquioxane hybrid airgel and its preparation method and application

A technology of silsesquioxane and polymer, which is applied in the field of tough polymer/cage silsesquioxane hybrid airgel and its preparation, can solve the problems of low preparation efficiency and long cycle, and achieve the The effect of good lumpiness, short cycle and low density

Active Publication Date: 2019-11-26
上海六零兴久生态科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above method requires the process of gel modification, solvent exchange and monomer diffusion, which has a long cycle and low preparation efficiency, and cannot fundamentally solve the brittleness problem of silicon-based airgel itself.

Method used

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  • A kind of tough polymer/cage silsesquioxane hybrid airgel and its preparation method and application
  • A kind of tough polymer/cage silsesquioxane hybrid airgel and its preparation method and application
  • A kind of tough polymer/cage silsesquioxane hybrid airgel and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) octaaminopropyl silsesquioxane and p-phenylene diisocyanate are mixed uniformly in a formamide solvent with a reactive functional group molar ratio of 1:0.5, and it is prepared into a solution whose solute mass concentration is 5g / L, and then Heating at 40°C for 24 hours to initiate polymerization reaction to obtain polymer / cage silsesquioxane hybrid wet gel;

[0038] 2) Aging the above wet gel in acetone, the aging time is 4h, the aging temperature is 30°C, and then the wet gel is subjected to supercritical CO 2 Dry to obtain polymer cage silsesquioxane hybrid airgel.

[0039] The tough polymer / cage silsesquioxane hybrid airgel prepared in Example 1 has a pore size distribution of 2 to 250 nm and a BET specific surface area of ​​1500 m 2 g -1 , with a density of 0.01g cm -3 , with a thermal conductivity of 0.01W·m -1 k -1 , the compressive modulus is 2MPa, the flexural modulus is 0.2MPa, the bending deformation is 95%, and it can withstand 500°C in the air atm...

Embodiment 2

[0041] 1) Mix octaaminophenylsilsesquioxane and bisphenol A type epoxy resin with a reactive functional group molar ratio of 1:1 evenly in an acetone solvent, and prepare a solution with a solute mass concentration of 40g / L, Then heating at 50°C for 16 hours to initiate a polymerization reaction to obtain a polymer cage-like silsesquioxane hybrid wet gel;

[0042] 2) Aging the above-mentioned wet gel in tetrahydrofuran for 24 hours at an aging temperature of 40°C, and then drying the wet gel at 60°C under normal pressure to obtain a polymer cage-like silsesquioxane hybrid aerogel .

[0043] The pore size distribution of the tough polymer / cage silsesquioxane hybrid airgel prepared in Example 2 is 5-300 nm, and the BET specific surface area is 1200 m 2 g -1 , with a density of 0.05g cm -3 , the thermal conductivity is 0.02W·m -1 k -1 , The compressive modulus is 10MPa, the flexural modulus is 1MPa, the bending deformation is 85%, and it can withstand 450°C in the air atmosp...

Embodiment 3

[0045] 1) The reactive functional group molar ratio is 1:1.5 decaaminopropyl silsesquioxane and triphenylmethane triisocyanate are mixed uniformly in acetamide solvent, and the solute mass concentration is prepared into a solution of 400g / L, Then heating at 60°C for 10 hours to initiate a polymerization reaction to obtain a polymer / cage silsesquioxane hybrid wet gel;

[0046] 2) Aging the above wet gel in acetone, the aging time is 4h, the aging temperature is 30°C, and then the wet gel is subjected to supercritical CO 2 Dry to obtain polymer cage silsesquioxane hybrid airgel.

[0047] The tough polymer / cage silsesquioxane hybrid airgel prepared in Example 3 has a pore size distribution of 2 to 500 nm and a BET specific surface area of ​​100 m 2 g -1 , with a density of 0.45g cm -3 , with a thermal conductivity of 0.05W·m -1 k -1 , the compressive modulus is 100MPa, the flexural modulus is 10MPa, the bending deformation is 40%, and it can withstand 500°C in the air atmosp...

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Abstract

The invention discloses strength-toughness polymer / polyhedral oligomeric silsesquioxane hybrid aerogel and a preparation method and application thereof. The aerogel is mainly prepared by mixing polyhedral oligomeric silsesquioxane containing an amino, vinyl or sulfydryl reactive functional group and an organic monomer or low polymer containing an isocyanate, sulfydryl, epoxy or vinyl reactive functional group in an organic solvent at the molar ratio of the functional groups of 1:(0.5-4). The aerogel is of a cross-linked structure formed by a C-S or C-N bond; the C-S or C-N bond has a low internal rotation potential barrier, so that the aerogel can be endowed with good toughness, is good in blocking property, has a nano porous structure, and is good in toughness, low in density, high in specific surface area, low in thermal conductivity, good in thermal stability and high in mechanical specific strength; and meanwhile, the preparation method is simple in process, high in efficiency and short in cycle. The prepared aerogel can be applied to the field of building energy conservation, high-temperature heat insulation, petrochemical industry or sewage treatment on a large scale.

Description

technical field [0001] The invention relates to chemical materials, in particular to a tough polymer / cage silsesquioxane hybrid airgel and its preparation method and application Background technique [0002] Silica airgel is a new material with a three-dimensional nanoporous structure, which has a low density (0.003~0.8g cm -3 ), high porosity (80-99.8%), high specific surface area (200-1000m 2 g -1 ), low thermal conductivity (~0.02W·m -1 K -1 ) and other properties, it has very broad prospects in aerospace, chemical industry, energy-saving buildings, military, communications, electronics, metallurgy and other application fields. However, silica aerogels have not been widely used, mainly because of the three-dimensional network structure of silica aerogels formed by weakly strained silicon-oxygen covalent bonds. The weak strain is easy to break and break under the action of external force, and the structure collapses, resulting in poor mechanical properties. [0003] ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J9/28C08G77/388C08G81/00C08G77/392
CPCC08G77/388C08G77/392C08G81/00C08J9/28C08J2201/0502C08J2205/026C08J2383/04C08J2387/00
Inventor 云山郭探李彦兴高晓燕李华举张加栋王金权何磊陈静
Owner 上海六零兴久生态科技有限公司