Preparing method of polyimide aerogels and hybrid aerogels thereof

A polyimide and airgel technology, applied in the field of airgel, can solve the problems of large specific surface area, high porosity, low thermal conductivity, etc., achieve high specific surface area, reduce shrinkage, and simplify the preparation process Effect

Inactive Publication Date: 2017-01-11
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The invention provides a low density, high porosity, low thermal conductivity, large specific surface area, excellent mechanical properties, thermal stab

Method used

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  • Preparing method of polyimide aerogels and hybrid aerogels thereof
  • Preparing method of polyimide aerogels and hybrid aerogels thereof
  • Preparing method of polyimide aerogels and hybrid aerogels thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Embodiment 1, preparation of solid content 2% BPDA / ODA polyimide airgel:

[0051] 1) Weigh 1g of polyamic acid precipitated fiber, 49ml of deionized water, and 1.23g of triethylamine (TEA), stir magnetically, and dissolve for 2 hours. Divide into three 50ml syringes, and the thickness of the sample should not exceed 3cm.

[0052] 2) Put it into a refrigerator or liquid nitrogen to freeze into a solid, pull out the piston, and freeze-dry for 48 hours.

[0053] 3) Place the obtained polyamic acid airgel in a nitrogen atmosphere to control the temperature program, that is, heat up from room temperature to 135°C for 60 minutes, and keep it for 1h; Amine airgel, denoted as PI-0.

[0054] The obtained airgel is light yellow and cylindrical airgel with dense structure and flat surface, with a thickness of 1.2cm, a diameter of 1.35cm, and a density of 0.0676g / cm 3 . The dielectric constant is 1.2, and the dielectric loss is 10 -3 -10 -5 between. When the compression rate...

Embodiment 2

[0055] Example 2, preparation of solid content 2% BPDA / ODA polyimide-graphene nanocomposite airgel:

[0056] 1) Weigh 60mg of graphene oxide powder, dissolve it in 49ml of deionized water, and seal it for 0.5h. Add 1.23g triethylamine, 1g polyamic acid precipitation fiber magnetic stirring, dissolve for 3h to form a homogeneous dilute solution, 200W, ultrasonic for 20min.

[0057] 2) Put it in the refrigerator to freeze into a solid, freeze-dry for 48 hours, and obtain the polyamic acid-graphene oxide nanocomposite airgel.

[0058] 3) Put the obtained polyamic acid-graphene oxide nanocomposite airgel in a tube furnace in a nitrogen atmosphere to control the temperature program, that is, from room temperature to 135°C for 60 minutes, and keep it for 1 hour; from 135°C to 300°C, heat up for 90 minutes , and keep warm for 2h; the polyimide-graphene nanocomposite airgel can be obtained, which is denoted as rGO-PI-60.

[0059] The obtained hybrid airgel is a black, cylindrical ai...

Embodiment 3

[0060] Example 3, preparation of solid content 2% BPDA / ODA polyimide / -OH carbon nanotube nanocomposite airgel:

[0061] 1) Weigh 80mg-OH carbon nanotube powder, dissolve it in 49ml deionized water, crush the cells with 800W power, and sonicate for 30min. Add 1.23g triethylamine, 1g polyamic acid precipitation fiber magnetic stirring, dissolve for 3h to form a homogeneous dilute solution, 200W, ultrasonic for 20min.

[0062] 2) Put it in the refrigerator to freeze into a solid, and freeze-dry for 48 hours to obtain polyamic acid / -OH carbon nanotube nanocomposite airgel.

[0063] 3) Put the obtained polyamic acid / -OH carbon nanotube nanocomposite airgel in a tube furnace in a nitrogen atmosphere to control the temperature program, that is, from room temperature to 135 ° C for 60 minutes, and keep it for 1 hour; 135 ° C to 300 ° C , heating up for 90min, and keeping warm for 2h; the polyimide / -OH carbon nanotube nanocomposite aerogel can be obtained, denoted as -OH CNTs-PI-80. ...

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Abstract

The invention discloses a preparing method of polyimide aerogels and hybrid aerogels thereof, belonging to the field of aerogels. In the preparing of the polyimide precursor, the polyamic acid precipitated fiber having a large specific surface area is dissolved in an aqueous solution of triethylamine, then stirred and dissolved. And the thermal imidization is directly frozen and dried without a long sol-gel process to obtain the polyimide aerogels. At the same time, by introducing the filler with different functional characteristics, the functional diversity of polyimide hybrid aerogels is realized. The prepared hybrid aerogels can be used as flexible conductors, microstrip patch antennas, catalysts, water and oil separation membranes, high performance adsorbent materials, etc., and can be used in the fields of flexible wearable microelectronics, aerospace communications, photocatalysis and oil leakage, etc. The application scope of polyimide materials and aerogels materials is expanded, the value of products is enhanced, the preparing cycle is shortened, and its industrialization process is promoted.

Description

technical field [0001] The invention belongs to the technical field of airgel, and in particular relates to a preparation method of a polyimide airgel and a hybrid gel thereof. Background technique [0002] airgel [0003] It is a highly dispersed solid nanomaterial with nanoporous network structure, which is composed of high polymer or colloidal particles aggregated with each other. The gaseous dispersion medium filled in its nanopores endows the airgel with low density, ultra-high porosity (80%-99.8%), and high specific surface area (100-1600m 2 / g), low thermal conductivity and low acoustic impedance. Since Kistler (Nature, 1931, 227:741) prepared the first silicon aerogel in the 1930s, it is represented by silicon aerogel, carbon aerogel and multi-component composite functionalized aerogel. The basic research and application development of airgel has received extensive attention and rapid development of researchers, and has been gradually applied to the fields of heat...

Claims

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Application Information

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IPC IPC(8): C08G73/10D01F6/78C08J9/28C08L79/08C08K3/04C08K7/24C08K3/22
CPCC08G73/1071C08G73/1067C08J9/28C08J2379/08C08K3/04C08K3/22C08K7/24C08K2003/2241D01F6/78C08L79/08
Inventor 武德珍王雅楠田国峰齐胜利
Owner BEIJING UNIV OF CHEM TECH
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