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Polyimide-based composite aerogel, controllable preparation method thereof and application of aerogel

A composite aerogel, polyimide-based technology, applied in the field of polyimide-based composite aerogel materials and their controllable preparation, can solve the problems of poor thermal stability, flammability, poor mechanical properties, etc. Improve the effect of mechanics, low cost and ingenious design ideas

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

AI Technical Summary

Problems solved by technology

[0003] The present invention is aimed at the problems of poor mechanical properties, poor thermal stability, flammability and limited use of existing polymer-based aerogels, and proposes a polyimide gas reinforced with one-dimensional carbon nanotubes as fillers. Gel material and its controllable preparation method and application

Method used

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  • Polyimide-based composite aerogel, controllable preparation method thereof and application of aerogel
  • Polyimide-based composite aerogel, controllable preparation method thereof and application of aerogel
  • Polyimide-based composite aerogel, controllable preparation method thereof and application of aerogel

Examples

Experimental program
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Effect test

Embodiment 1

[0031] This embodiment includes the following steps:

[0032] 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. Then the polyamic acid hydrogel was obtained through the sol-gel process.

[0033] The obtained polyamic acid hydrogel was transferred to a mold, and ultrasonically sounded for 0.5h, then the mold was transferred to a refrigerator at about 4°C for 5h, and then put into liquid nitrogen to rapidly freeze it into a solid, and then Freeze drying under 10-20Pa vacuum 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 hour; To 300°C, rai...

Embodiment 2

[0036] This embodiment includes the following steps:

[0037] Take 2g of untreated carbon nanotubes, add 300mL of concentrated sulfuric acid and 100mL of concentrated nitric acid, and stir at 70°C for 2h. Washed repeatedly with 8% hydrochloric acid solution and deionized water, and freeze-dried to obtain acidified carbon nanotubes, denoted as a-CNT.

[0038] Take 30mL of 2mg / mL a-CNT dispersion, add 2g of polyamic acid and 1g of triethylamine, sonicate for 1h, stir for 0.5h, dissolve and disperse the polyamic acid evenly, and obtain acidified carbon nanotube polyamic acid aqueous solution. The acidified carbon nanotube polyamic acid hydrogel was obtained through a sol-gel process.

[0039] All the other steps are the same as in Example 1. The acidified carbon nanotube polyimide-based composite airgel was obtained, which was denoted as PI / a-CNT. The atomic ratio of oxygen-containing groups to nitrogen-containing groups in PI / a-CNT was determined to be 1:0.04 by X-ray electro...

Embodiment 3

[0041] This embodiment includes the following steps:

[0042] Take 2g of untreated carbon nanotubes, add 300mL of concentrated sulfuric acid and 100mL of concentrated nitric acid, and stir at 70°C for 2h. Washed repeatedly with 8% hydrochloric acid solution and deionized water, and freeze-dried to obtain acidified carbon nanotubes, denoted as a-CNT.

[0043]Take 30 mL of 2 mg / mL a-CNT 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. Acidified-aminated carbon nanotube dispersion liquid was obtained.

[0044] Take 30mL of 2mg / mL acidified-aminated carbon nanotube dispersion, add 2g polyamic acid and 1g triethylamine, sonicate for 1h, and stir for 0.5h to dissolve and disperse the polyamic acid evenly, and obtain acidified-aminated carbon nanotubes Tube polyamic acid aqueous solution. The acidified-aminated carbon nanotube polyamic acid hydrogel is obtained through a sol-gel process.

[0045] All the other step...

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Abstract

The invention discloses polyimide-based composite aerogel, a controllable preparation method thereof and an application of the aerogel. The polyimide-based composite aerogel provided in the invention comprises carbon nano tubes and polyimide, the atomic ratio of oxygen-containing groups to nitrogen-containing groups at the surfaces of the carbon nano tubes is (1:0.1)-(1:0.19). Raw material components comprise one or more water-soluble polyimide precursors polyamic acids, and one or more carbon nano tubes. The preparation method comprises the following steps: performing amination on carbon nano tubes subjected to acidification to prepare acidified and aminated carbon nano tubes, performing reaction on the acidified and aminated carbon nano tubes and the water-soluble polyamic acid to obtain acidified and aminated carbon nano tube polyamic acid hydrogel, and performing thermal imidization to prepare the acidified and aminated carbon nano tube polyimide-based composite aerogel. 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 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-polymer-based porous composite airgel, and specifically relates to a polyimide-based composite airgel material and its controllable preparation method and application. Background technique [0002] Since the appearance of airgel in the 1930s, due to its high porosity (80-99.8%), high specific surface area (200-1000m 2 / g), low density (<0.1g / cm 3 ) and other properties show broad application prospects in flame retardancy, heat insulation, sound insulation, etc. Aerogels can be divided into silica (SiO2) aerogels, carbon aerogels, polymer-based aerogels and other inorganic aerogels according to their components. Compared with SiO2 and carbon aerogels, polymer-based aerogels are widely used as flame retardant, thermal insulation, and dielectric materials due to their unique properties such as low cost, easy molding, high porosity, low density, and low thermal conductiv...

Claims

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Application Information

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IPC IPC(8): C08J9/28C08L79/08C08K9/04C08K7/24C08G73/10
CPCC08G73/10C08J9/28C08J2379/08C08K7/24C08K9/04C08L2201/02C08L79/08
Inventor 刘天西左立增张由芳樊玮尹一戈董玥
Owner FUDAN UNIV
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