Preparation method for polyimide-based composite aerogel and polyimide-based composite aerogel

A composite airgel and polyimide-based technology, which is applied in the field of preparation of new nanomaterial-polymer-based porous composite airgel, can solve the problems of limited use, flammability, poor thermal stability, etc., and achieve design Ingenious ideas, low cost, excellent mechanical effects

Active Publication Date: 2017-11-21
FUDAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The present invention aims at the problems of poor mechanical properties, poor thermal stability, flammability and

Method used

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  • Preparation method for polyimide-based composite aerogel and polyimide-based composite aerogel
  • Preparation method for polyimide-based composite aerogel and polyimide-based composite aerogel
  • Preparation method for polyimide-based composite aerogel and polyimide-based composite aerogel

Examples

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Embodiment 1

[0032] This embodiment includes the following steps:

[0033] Take 30 mL of deionized water, add 2 g of polyamic acid and 1 g of triethylamine, sonicate for 1 h, and stir for 0.5 h to dissolve and disperse the polyamic acid evenly to obtain an aqueous solution of polyamic acid. Triethylamine can be coated on the terminal carboxyl functional group of polyamic acid, so that polyamic acid is easily soluble in deionized water. Then transfer it to a mold and ultrasonically for 0.5h, then transfer the mold to a refrigerator at about 4°C for 5h pre-cooling, then put it in liquid nitrogen to make it solid quickly, and then freeze it under a vacuum of 10-20Pa Dry for 48 hours to obtain polyamic acid airgel.

[0034] Place the obtained polyamic acid airgel in a tube furnace, and control the temperature rise program in a nitrogen atmosphere, that is, from room temperature to 100°C, heat up for 30 minutes, and hold for 1 hour; from 100°C to 200°C, heat up for 30 minutes, and hold for 1 h...

Embodiment 2

[0036] This embodiment includes the following steps:

[0037] Take 30 mL of 2 mg / mL graphene oxide dispersion, add 2 g of polyamic acid and 1 g of triethylamine, sonicate for 1 h, and stir for 0.5 h to dissolve and disperse the polyamic acid evenly to obtain an aqueous solution of polyamic acid. All the other steps are the same as in Example 1. A graphene-enhanced polyimide-based composite airgel was obtained, denoted as PI / GO. The oxygen-containing group content of PI / GO was measured to be 36.8% by thermogravimetric analysis (TGA) and X-ray electron spectroscopy (XPS).

Embodiment 3

[0039] This embodiment includes the following steps:

[0040] Take 30 mL of 2 mg / mL graphene oxide dispersion, add 11 μL of 50 wt% hydrazine hydrate and 75 μL of 25 wt% ammonia water, and stir at 95° C. for 0.5 h. Obtain a partially reduced graphene oxide dispersion, denoted as GO 30 .

[0041] The steps for preparing polyimide-based composite airgel are the same as in Example 1. A polyimide-based composite airgel reinforced with graphene (the product of partially reduced graphene oxide through thermal imidization) was obtained, denoted as PI / G 30 . PI / G was measured by TGA and XPS methods 30 The oxygen-containing group content is 32.9%.

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Abstract

The invention discloses a preparation method for polyimide-based composite aerogel and the polyimide-based composite aerogel product. Raw material components for preparing the polyimide-based composite aerogel comprise one or more water-soluble polyimide precursors polyamic acids, and oxidized graphene. The preparation method comprises the following steps: (1) an aqueous dispersion liquid of the oxidized graphene and the water-soluble polyimide precursor polyamic acid are uniformly mixed according to a certain proportion, a sol-gel process and a lyophilization technology are used, and therefore oxidized graphene-polyamic acid aerogel is obtained; and (2) the graphene-polyimide aerogel is prepared through a thermal imidization process. The method for preparing the polyimide-based composite aerogel is simple and easy to implement, the prepared composite aerogel is controllable in micro morphology and adjustable in performance; and besides, the prepared polyimide-based composite aerogel has excellent flame retardance, and is an ideal heat-insulation material and a flame-retardant material.

Description

technical field [0001] The invention belongs to the technical field of preparation of novel nanomaterial-macromolecule-based porous composite airgel, and specifically relates to a preparation method and product of polyimide-based composite airgel. Background technique [0002] In recent years, airgel is known for its high porosity (80-99.8%), high specific surface area (200-1000m 2 / g), low density (<0.1g / cm 3 ) and low thermal conductivity (<0.05W / (m·K)) have shown broad application prospects in flame retardancy, heat insulation, sound insulation, etc. [0003] At present, the widely studied airgel is based on silica (SiO 2 ) is the inorganic aerogel of matrix material. Although SiO 2 Aerogels have superior high-temperature stability and low thermal conductivity, but SiO 2 Airgel has problems such as complex preparation process, high cost, and fragility, so its use is limited. [0004] with SiO 2 Compared with aerogels, polymer-based aerogels have attracted ext...

Claims

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Application Information

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IPC IPC(8): C08J9/28C08L79/08C08K3/04
CPCC08J9/28C08J2379/08C08K3/04C08L79/08
Inventor 刘天西左立增张由芳樊玮尹一戈董玥
Owner FUDAN UNIV
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