Intrinsic hydrophobic polyimide aerogel and preparation method as well as application thereof

A technology of airgel and polyamic acid, applied in the field of intrinsically hydrophobic polyimide airgel and its preparation, can solve the problem of not effectively improving the hydrophilicity of PI airgel, affecting the application effect and density Problems such as increased dielectric constant and high porosity, low density, low dielectric constant and dielectric loss are achieved

Active Publication Date: 2013-09-18
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the good mechanical flexibility of PI airgel, although the PI airgel that absorbs water will not be as good as inorganic SiO 2 Airgel is broken like that, but it will cause the increase of density and dielectric constant, which will affect its application effect
However, the traditional hydrophobization process will not effectively improve the hydrophilicity of PI airgel.

Method used

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  • Intrinsic hydrophobic polyimide aerogel and preparation method as well as application thereof
  • Intrinsic hydrophobic polyimide aerogel and preparation method as well as application thereof
  • Intrinsic hydrophobic polyimide aerogel and preparation method as well as application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] 1) Add 1.9741g (6.16mmol) 2,2'-bis(trifluoromethyl)-4,4'-diaminobiphenyl (TFDB) and 25 g of freshly distilled N-methylpyrrolidone (NMP) was bubbled with nitrogen. After TFDB was completely dissolved, 1.2479g (6.36mmol) of 1,2,3,4-cyclobutanetetracarboxylic dianhydride (CBDA) and 25g of NMP were added, and condensation polymerization was carried out at 25°C for 24h to obtain anhydride-terminated polycarbonate. Amic acid solution.

[0057] 2) Add 0.0574g (0.0497mmol) of amino group-containing polyfunctional capping agent octa(aminophenyl) polysilsesquioxane (OAPS) to the system, and carry out amidation reaction at 25°C for 24h to obtain crosslinked Polyamic acid solution.

[0058] 3) Add 2.52g (31.82mmol) of pyridine and 3.25g (31.82mmol) of acetic anhydride to the cross-linked polyamic acid solution obtained in step 2), stir for 20 minutes, and pour it into a mold for dehydration reaction. The system gels within 4 hours. A gel containing the compound of formula II is ...

Embodiment 2

[0071] 1) Add 1.1102g (6.16mmol) 3,5-diaminotrifluorotoluene (TFMDA) and 25g freshly distilled N-methylpyrrolidone (NMP) in a there-necked flask equipped with mechanical stirring, temperature and nitrogen inlet, Nitrogen was introduced. After TFMDA is completely dissolved, add 1.2479g (6.36mmol) 1,2,3,4-cyclobutanetetraacid dianhydride (CBDA) and 25g of NMP, and carry out condensation polymerization at room temperature (25°C) for 24h to obtain anhydride group Capped polyamic acid solution.

[0072] 2) Add 0.0574g (0.0497mmol) of octa(aminophenyl)polysilsesquioxane (OAPS) to the system in step 1), and carry out amidation reaction at room temperature (25°C) for 24h to obtain a cross-linked polyamide acid solution.

[0073] 3) Add 2.52g (31.82mmol) of pyridine and 3.25g (31.82mmol) of acetic anhydride to the crosslinked polyamic acid solution obtained in step 2). Stir for 20 minutes, pour into a mold for dehydration reaction, and the system gels within 1 hour to obtain a gel c...

Embodiment 3

[0081] 1) Add 1.0858g (6.16mmol) 2,3,5,6-tetrafluoro-p-phenylenediamine (TFPDA) and 25g of freshly distilled N-methyl to a three-neck flask equipped with mechanical stirring, temperature and nitrogen inlet Pyrrolidone (NMP) with nitrogen gas. After TFPDA was completely dissolved, 1.2479g (6.36mmol) of 1,2,3,4-cyclobutane tetra-acid dianhydride (CBDA) and 25g of NMP were added. The polycondensation reaction was carried out at room temperature (25° C.) for 24 hours to obtain an anhydride group-terminated polyamic acid solution.

[0082] 2) Add 0.0574g (0.0497mmol) of octa(aminophenyl)polysilsesquioxane (OAPS) to the system in step 1), and carry out amidation reaction at room temperature (25°C) for 24h to obtain a cross-linked polyamide acid solution.

[0083] 3) Add 2.52g (31.82mmol) of pyridine and 3.25g (31.82mmol) of acetic anhydride to the crosslinked polyamic acid solution obtained in step 2). Stir for 20 minutes, pour into a mold for dehydration reaction, and the system...

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Abstract

The invention discloses intrinsic hydrophobic polyimide aerogel and a preparation method as well as an application thereof. The structure of the aerogel is shown in a structural formula (I); special groups, such as a hydrophobic fluorin-containing group and an alicyclic group at low polarity are introduced to a polyimide molecular structure to endow a polyimide aerogel material with excellent hydrophobic performance; in addition, the polyimide aerogel has the characteristics of high porosity, low heat conductivity, low density, large specific surface area, low dielectric constant, low dielectric loss and the like, and therefore is of significant application values in the fields of thermal insulating components of spacecrafts, such as airplanes and satellites, interlayer dielectric materials of super-large-scale integrated circuits, thermal insulating layers of buildings, environment protection, deep ocean detection, oil exploration, energy-saving buildings, household appliances, warm-keeping clothes, sports equipment and the like. Formula I is shown in the specification.

Description

technical field [0001] The invention belongs to the field of high-performance polyimide materials, and relates to an intrinsic hydrophobic polyimide airgel and a preparation method and application thereof. Background technique [0002] Airgel is a kind of dry gel material whose dispersion medium is air, and its solid phase and pore structure are both on the nanometer scale. This structural feature makes airgel the solid material with the smallest density in the world (as low as 0.0002g / cm 3 ), is also the solid material with the smallest thermal conductivity in the world (up to 0.002W / m in air -1 K -1 , up to 0.001W / m under vacuum at room temperature -1 K -1 ), and airgel also has a very low dielectric constant (1.0-2.0) and dielectric loss. The above characteristics make aerogels have broad application prospects in the fields of integrated circuits, energy saving, aerospace and other fields (AegerterM A, Leventis N, Koebel M(eds). Aerogels handbook. Springer Science+Bu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08L79/08
Inventor 杨士勇沈登雄刘金刚
Owner INST OF CHEM CHINESE ACAD OF SCI
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