Polysilsesquioxane aerogel and preparation method thereof

A technology of polysilsesquioxane and airgel, which is applied in the field of airgel, can solve the problems that research work has not received due attention, impurities such as surfactants are difficult to completely remove, and the application range of materials is limited. Achieve good tolerance, reduce irreversible shrinkage, and ensure uniformity

Active Publication Date: 2018-10-09
INST OF CHEM CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, like other silicon oxide aerogels, the preparation of polysilsesquioxane aerogels still has problems such as long preparation period and large amount of solvent used, and it is difficult to completely remove impurities such as surfactants introduced during the synthesis process.
On the other hand, the polysilsesquioxane airgel prepared by the existing technology is often white and opaque, which limits the application range of the material
Moreover, the chemical stability of micro-nanoporous materials such as airgel is often sensitive to environmental factors such as moisture, salt, acid, and alkali, but research work in this area has not received due attention

Method used

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  • Polysilsesquioxane aerogel and preparation method thereof
  • Polysilsesquioxane aerogel and preparation method thereof
  • Polysilsesquioxane aerogel and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Mix 10 mL of methyltriethoxysilane (MTES) with 2.0 mL of deionized water, 6.0 mL of absolute ethanol, and 0.5 uL of 40% HF aqueous solution, stir and react at 60° C. for more than 30 minutes and then cool to room temperature. Add 2.0 mL of deionized water, 6.0 mL of absolute ethanol, and 100 uL of triethylamine to the above solution. Leave to stand at 15℃ or above to form a gel, and age at 25℃ or above for more than 3 hours. It was washed three times with ethanol and three times with n-hexane. Drying at room temperature and pressure for more than 12 hours, with a heating rate of 2°C / min to 80°C, and holding for more than 1 hour; heating to 200°C or more at a heating rate of 3°C / min and holding for more than 2 hours to complete the drying.

[0039] Its density is 0.19g / cm 3 , The average pore diameter is 9.3nm, the static contact angle with water is 123°, the visible light transmittance at 700nm is 63%, and the transmittance of 190-400nm ultraviolet light region is less th...

Embodiment 2

[0041] Mix 10 mL of methyl trimethoxysilane (MTMS) with 3.0 mL of deionized water, 7.0 mL of propanol, and 0.7 uL of 40% HF aqueous solution, stir and react at 15°C for at least 30 minutes, and then cool to room temperature. Add 7.0 mL of deionized water, 2.5 mL of propanol, and 0.7 mL of 40% tetrabutylammonium hydroxide solution to the above solution. Leave to stand at 15℃ or above to form a gel, and age at 25℃ or above for more than 3 hours. Wash three times with propanol and three times with n-pentane. The drying procedure is similar to that of Example 1, but after the temperature is raised to 80 degrees Celsius, it becomes a reduced pressure operation to remove volatile impurities as much as possible, and the pressure value is not higher than 0.85 atm.

[0042] Its density is 0.16g / cm 3 , The average pore size is 9.6nm, the static contact angle with water is 122°, the visible light transmittance at 700nm is 64%, and the transmittance in the ultraviolet region of 190-400nm is...

Embodiment 3

[0044] The operation is similar to Example 2, but the tetrabutylammonium hydroxide solution in Example 2 is replaced with a tetraethylammonium hydroxide solution. Before drying, soak the gel with 1% 1H,1H,2H,2H-perfluorooctyltrichlorosilane petroleum ether solution equal to the volume of the gel for more than 3h, 1H,1H,2H,2H-perfluorooctyltrichlorosilane The concentration of the solution is preferably 30% or less.

[0045] Its density is 0.15g / cm 3 , The average pore diameter is 12.1nm, the static contact angle with water is 143°, the visible light transmittance at 700nm is 54%, and the transmittance in the ultraviolet region of 190-400nm is less than 1%. Soaking in water, 0.1M HCl solution, 3.5% NaCl solution, 0.1M NaOH solution and other systems for more than three hours can keep it intact, and the contact angle can still be kept above 120° after soaking.

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Abstract

The invention relates to a preparation method of a polysilsesquioxane material. The preparation method comprises the following steps that (1) in water and an organic solvent, acid is used for catalyzing a polysilsesquioxane precursor for hydrolysis to form sol; (2) organic alkali is added into a sol system for catalytic polycondensation to form gel; (3) the gel is aged and dried to obtain aerogel.The polysilsesquioxane aerogel has high tolerance degree on water, salt, acid, alkali and the like; high transmittance is realized in the visible light range; high shielding capability is realized onultraviolet light.

Description

Technical field [0001] The invention relates to an aerogel, in particular to a transparent polysilsesquioxane aerogel that uses a polysilsesquioxane precursor as a raw material and is dried under normal pressure or reduced pressure and a preparation method thereof. Background technique [0002] Aerogel is a solid form of matter. Usually it refers to the solid matter obtained by removing the solvent from the gel by a specific drying method without changing the microstructure and geometric shape of the gel, and replacing it with a gas. As an ultra-light material with a density comparable to air, aerogel generally has the characteristics of high porosity, large specific surface area, and low density because the microporous structure of the gel is better retained during the preparation process. In addition, aerogel also has low refractive index, low thermal conductivity, low acoustic impedance and certain transparency. This series of characteristics of aerogel makes it have great p...

Claims

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Application Information

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IPC IPC(8): C08J9/28C08L83/04C08G77/04
CPCC08G77/045C08J9/286C08J2205/026C08J2205/042C08J2205/05C08J2383/04
Inventor 杨国强张涛王双青李光武
Owner INST OF CHEM CHINESE ACAD OF SCI
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