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Preparation method of polyimide aerogel adsorption material

A technology of polyimide and adsorption materials, which is applied in the field of preparation of nanoporous materials, can solve the problems of large brittleness, hygroscopicity, and limitations, and achieve the effect of high porosity and high specific surface area

Inactive Publication Date: 2019-06-11
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to its greater brittleness and hygroscopicity, it is limited in many applications

Method used

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  • Preparation method of polyimide aerogel adsorption material

Examples

Experimental program
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Effect test

example 1

[0029] Add 0.750g of ODA (the molar ratio of ODA to 1,3-propanediamine is 1:2) into 40mL of NMP, stir for 20min, until all ODA is dissolved, add 0.64ml of 1,3-propanedi under magnetic stirring Amine, stirring for 20min, until 1,3-propanediamine is completely dissolved. Then, 1.15 g of BPDA was added to the mixed solution and stirred at room temperature for about 6 hours to obtain a homogeneous solution. Next, add 0.031g of TAB to 17ml NMP solution, pour it into the mixed solution after dissolution, stir for 5 minutes, add 4.0ml acetic anhydride and 4.0ml pyridine to the solution, stir until the mixed solution is transparent, then pour it into In the mold. The samples were left at room temperature until gelation. After aging for 18 hours, an acetone solution containing 50% NMP was added to the mold for solution replacement. Subsequently, the acetone solution was replaced every 18 hours for a total of 4 washes. Finally, take out the sample that has been replaced by the solution...

example 2

[0031] Add 0.750g of ODA (the molar ratio of ODA to 1,3-propanediamine is 1:3) into 50mL of NMP, stir for 40min, until all ODA is dissolved, add 0.96ml of 1,3-propanedi under magnetic stirring Amine, stirring for 40min, until 1,3-propanediamine is completely dissolved. Then, 1.75 g of BPDA was added to the mixed solution and stirred at room temperature for about 7 hours to obtain a homogeneous solution. Next, add 0.052g of TAB to 18ml of NMP solution, pour it into the mixed solution after dissolution, stir for 7 minutes, add 5.0ml of acetic anhydride and 5.0ml of pyridine to the solution, stir until the mixed solution is transparent, then pour it into In the mold. The sample was left at room temperature until gelling. After 20 hours of aging, an acetone solution containing 60% NMP was added to the mold for solution replacement. Subsequently, the acetone solution was replaced every 20 hours for a total of 6 washes. Finally, take out the sample that has been replaced by the sol...

example 3

[0033] Add 0.750g of ODA (the molar ratio of ODA to 1,3-propanediamine is 1:1) into 60mL of NMP, stir for 30min, until all the ODA is dissolved, add 0.32ml of 1,3-propanedi under magnetic stirring Amine, stirring for 30min, until 1,3-propanediamine is completely dissolved. Then, 2.27 g of BPDA was added to the mixed solution and stirred at room temperature for about 8 hours to obtain a homogeneous solution. Next, add 0.066g of TAB to 21ml of NMP solution and pour it into the mixed solution after dissolution. After stirring for 10 minutes, add 5.8ml of acetic anhydride and 5.0ml of pyridine to the solution, stir until the mixed solution is transparent, and then pour it into In the mold. The sample was left at room temperature until gelling. After 24 hours of aging, an acetone solution containing 75% NMP was added to the mold for solution replacement. Subsequently, the acetone solution was replaced every 24 hours for a total of 5 washes. Finally, take out the sample that has be...

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Abstract

The invention belongs to a preparation method of a polyimide aerogel adsorption material. A sol-gel method is adopted, and a mixed diamine component of conventional polyimide aerogel is changed. Aromatic oxydianiline (ODA) and aliphatic 1,3-propane diamine are used as mixed diamine, 3,3',4,4'-biphenyltetracarboxylic dianhydride (BPDA) is used as a dianhydride, 1,3,5-tris(4-aminophenoxy)benzene (TAB) is used as a cross-linking agent, acetic anhydride and pyridine are used as imidization reagents, and polyimide hydrogel is synthesized at normal temperature; replacing and aging is carried out onthe solution, and then CO2 supercritical drying is carried out to obtain the complete block-shaped polyimide aerogel. The polyimide aerogel prepared by the method has relatively low heat conductivityand good mechanical properties, and meanwhile, a flexible structure is obtained. Experiments prove that the polyimide aerogel can be used for adsorbing CO2. The density of the polyimide aerogel adsorption material is 0.08-0.11 g / cm<3>, the compression modulus is 2.03-3.26 MPa, and the CO2 adsorption amount is 8.2-11.5 cm<3> / g.

Description

Technical field [0001] The invention belongs to the field of preparation technology of nanoporous materials, and in particular relates to a low density, high specific surface area, and high CO 2 Preparation method of polyimide aerogel adsorption material with adsorption capacity. Background technique [0002] As a special engineering material, polyimide is one of the organic polymers with the best comprehensive performance. It has no obvious melting point, high insulation performance, low dielectric loss and good mechanical properties. The NASA Research Center in the United States compared the performance of polyimide aerogels prepared with different diamines and dianhydrides and found that the use of monomers with rotatable chemical bonds can give polyimide aerogels a flexible structure, such as ODA, etc. . Kistler prepared SiO for the first time in 1931 2 Since aerogels, inorganic aerogels have developed tremendously. Aerogel is a solid material with a nanoporous network stru...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J9/28C08L79/08B01D53/02B01J13/00B01J20/26B01J20/28B01J20/30
CPCY02C20/40Y02P20/151
Inventor 朱昆萌刘思佳沈晓冬崔升王雪彭长鑫
Owner NANJING UNIV OF TECH
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