Carbon-black-filled polyimide-based compound aerogel material and preparation method thereof

A composite airgel and polyimide-based technology, applied in the field of composite airgel, can solve the problems of high price and limited use of crosslinking agents, and achieve low raw material cost, low heat resistance, and microscopic morphology uniform effect

Inactive Publication Date: 2017-05-10
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention aims at the problem that the cross-linking agent used in the preparation process of the polyimide airgel is expensive and limited in use, and proposes a method of using carbon black as the cross-linking agent and improving the carbon density by preparing oxidized carbon black. Dispersibility of black, method for preparing carbon black-filled polyimide composite airgel

Method used

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  • Carbon-black-filled polyimide-based compound aerogel material and preparation method thereof
  • Carbon-black-filled polyimide-based compound aerogel material and preparation method thereof
  • Carbon-black-filled polyimide-based compound aerogel material and preparation method thereof

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Embodiment 1

[0038] This embodiment includes the following steps:

[0039] by N,N -Dimethylacetamide is used as a solvent, and 4,4'-diaminodiphenyl ether and pyromellitic anhydride are used as monomers to carry out condensation polymerization in an ice-water bath to prepare polyamic acid filaments. The specific process is as follows: at room temperature, 8 g (0.04 mol) of 4,4′-diaminodiphenyl ether was fully dissolved in 95 g N,N -Dimethylacetamide, based on the clarity of the solution and the absence of particles. Then 8.85 g (0.046 mol) pyromellitic anhydride was added slowly, and then the reaction was moved to an ice-water bath and stirred for 2 h. Then add 0.04 mol triethylamine, continue to stir and react for about 2 h, and prepare a polyamic acid solution with a solid content of 15%. The prepared polyamic acid solution is sealed and stored, and after standing for two days, it is slowly poured into ice water, washed, frozen, and dried to obtain a water-soluble polyamic acid filam...

Embodiment 2

[0043] This embodiment includes the following steps:

[0044] The steps for preparing water-soluble polyamic acid are the same as in Example 1.

[0045] The steps of preparing oxidized carbon black are as follows:

[0046] Acetylene black (specific surface area 75 m 2 / g, apparent density 90-120 g / L) as an example to prepare oxidized carbon black. Add 5 g of carbon black to a 1000 mL beaker, add 3.75 g of sodium nitrate, and stir for 10 min; then add 150 mL of concentrated sulfuric acid, and stir for 0.5 h; slowly add 20 g of potassium permanganate, after 0.5 h, stir for 20 h ; Slowly add 500 mL of deionized water, add 50 mL of 30% hydrogen peroxide after cooling, and stir for 1 h; filter the mixture with suction and wash with 10% hydrochloric acid until no sulfate ion is detected to obtain oxidized carbon black Wet filter cake; then dried at 70°C for 5 h to obtain oxidized carbon black solid.

[0047] The steps of preparing polyimide-carbon black composite airgel are as f...

Embodiment 3

[0050] This embodiment includes the following steps:

[0051] The steps for preparing water-soluble polyamic acid are the same as in Example 1, and the steps for preparing oxidized carbon black are the same as in Example 2.

[0052] The steps of preparing polyimide-carbon black composite airgel are as follows:

[0053] Take 80 mg of oxidized carbon black and add it into 30 mL of deionized water, and sonicate for 0.5 h to make the oxidized carbon black disperse evenly. All the other are with embodiment 3. Obtain polyimide-carbon black composite airgel, denoted as PI / CB 4% .

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Abstract

The invention belongs to the technical field of compound aerogel, and in particular relates to a carbon-black-filled polyimide-based compound aerogel material and a preparation method thereof. The compound aerogel is prepared from the following raw materials: one or more water-soluble polyimide precursor-polyamide acids and one or more carbon black. The preparation method comprises the steps of preparing oxidized carbon black dispersion liquid; preparing polyamide acid-oxidized carbon black hydrogel by means of a sol-gel process; preparing polyamide acid-oxidized carbon black aerogel by means of freeze drying; preparing polyimide-carbon black compound aerogel by means of hot imidization. The raw materials for preparing the polyimide-based compound aerogel are low-cost, and the preparation method is simple and easy to implement; the prepared compound aerogel is uniform in micro-morphology. Furthermore, the prepared polyimide-based compound aerogel has excellent mechanical strength and heat resistance, and a lower dielectric constant, thus being an ideal high-temperature dielectric material.

Description

technical field [0001] The invention belongs to the technical field of composite airgel, and in particular relates to a polyimide-based composite airgel material filled with carbon black and a preparation method thereof. Background technique [0002] Polymer airgel is a kind of porous gel material based on natural or synthetic polymers, which has the characteristics of easy molding, high porosity, high specific surface area, low density, and low thermal conductivity. Therefore, polymer airgel is gradually used as a matrix material in heat insulation, sound insulation and dielectric materials. However, polymer aerogels generally have problems such as poor mechanical properties, poor thermal stability, and flammability. The reason is mainly caused by the poor mechanical properties of the polymer matrix and the low thermal decomposition temperature. [0003] As an engineering plastic, polyimide has good mechanical properties and thermal stability, and is an ideal polymer airg...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J9/28C08J3/075C08L79/08C08K9/02C08K3/04
Inventor 刘天西左立增樊玮郜伟鲁恒毅顾华昊赖飞立
Owner FUDAN UNIV
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