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Preparation method of flame-retardant and high-performance polyimide aerogel

A kind of polyimide wet gel, polyimide technology, applied in the field of preparation of flame-retardant high-performance polyimide aerogel

Inactive Publication Date: 2019-04-26
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, research on high-performance polyimide aerogels with high flame-retardant properties is still in its infancy
[0006] The preparation of polyimide airgel is based on a two-step method of synthesizing polyimide, first preparing polyamic acid, and then performing a dehydration reaction, but this method can only form a linear structure

Method used

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  • Preparation method of flame-retardant and high-performance polyimide aerogel
  • Preparation method of flame-retardant and high-performance polyimide aerogel
  • Preparation method of flame-retardant and high-performance polyimide aerogel

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Embodiment 1

[0026] Dissolve 1.1800 g of 3,3’,4,4’-diphenyl ether tetracarboxylic dianhydride (ODPA) and 0.7490 g of diaminodiphenyl ether (ODA) in 30 mL and 20 mL of NMP solvent, respectively. Heating and stirring can be used to speed up the dissolution. After complete dissolution, the diamine solution is added dropwise to the dianhydride solution, and reacted at room temperature for 8 hours to obtain a polyamic acid solution. Add a solution of 0.0150g of hexaaminocyclotriphosphazene dissolved in 2mL of NMP to the polyamic acid solution, and after stirring for 10 minutes, quickly add 5.7570g of acetic anhydride and 4.9270g of pyridine for dehydration treatment, and quickly stir evenly. After reacting for 6 hours, the solvent was replaced with 100 mL of acetone and 100 mL of cyclohexane, and then left to stand at room temperature for 12 hours. Finally, supercritical CO 2 Drying technology Dry the wet gel at 40°C and 15MPa for 8 hours to finally obtain a cross-linked airgel with low water ...

Embodiment 2

[0028] Dissolve 3.153g of pyromellitic dianhydride (PMDA) into 60ml of NMP, heat to 40°C and stir, then add 2.803g of 4,4'-diaminoanisole (ODA) into 50ml of NMP, After heating and stirring until dissolved, the diamine monomer and the dianhydride monomer were mixed and stirred at room temperature for 10 hours under the protection of nitrogen to obtain a polyamic acid solution. Add 0.112g of hexaaminocyclotriphosphazene dissolved in 5mL of NMP into the polyamic acid solution, stir rapidly, add 15.3g of acetic anhydride and 11.865g of pyridine after 10 minutes, and carry out the dehydration and cyclization reaction for a period of time. Solvent replacement was performed sequentially with 200 mL of acetone and 200 mL of cyclohexane solvent to obtain a polyimide wet gel. Finally, the wet gel was subjected to supercritical CO 2 Drying, 15MPa, 40°C, then vacuum drying at 80°C for 12 hours. The obtained product has a density of 0.28g / cm 3 , specific surface area 298m 2 / g, the gla...

Embodiment 3

[0030] Dissolve 1.820g of biphenyltetracarboxylic dianhydride (BPDA) in 40mL of NMP, and dissolve 1.196g of diaminodiphenyl ether (ODA) in 30mL of NMP until completely dissolved. The solutions were mixed and reacted at room temperature for 12 hours under the protection of nitrogen to obtain a polyamic acid solution. Then 0.0678g of hexa(p-aminophenoxy)cyclotriphosphazene was added to the polyamic acid solution, and after 10 minutes of reaction, 6.79g of acetic anhydride and 5.25g of pyridine were added to the solution to start to generate polyamide rings. Acetone and 140 mL of cyclohexane solvent were used for solvent replacement, and then left to stand at room temperature for 12 h. Finally, supercritical CO was applied to polyimide wet gels. 2 dry. The obtained product has a density of 0.22g / cm 3 , specific surface area 248m 2 / g, the glass transition temperature is 298°C, and the limiting oxygen index is 51%.

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Abstract

The invention provides a preparation method of flame-retardant and high-performance polyimide aerogel, and relates to a preparation method of aerogel. The preparation method comprises steps as follows: polyamide acid is prepared from aromatic dianhydride and diamine by a reaction, polyamino monomers (such as hexa(p-aminophenoxy)cyclotriphosphazene) containing a phosphonitrile ring is added, an organic network structure is formed, dehydration and drying are performed, and the high-performance cross-linked polyimide aerogel is obtained finally. The phosphonitrile ring belongs to a six-membered heterocyclic conjugate structure of total phosphorus and nitrogen, the chemical structure is stable, derivatives of the phosphonitrile ring also show excellent thermal stability, and the structure hashigh phosphorus and nitrogen content and is quite beneficial to flame retardance. Therefore, thermal stability and flame retardance of the polyimide aerogel can be remarkably improved with introduction of the phosphonitrile ring. An obtained product has quite good heat resistance, the glass-transition temperature (Tg) is at 260 DEG C or higher, the limit oxygen index can reach 53%, and meanwhile,the product has good resistance to atomic oxygen and ultraviolet light.

Description

technical field [0001] The invention relates to a preparation method of an airgel, in particular to a preparation method of a flame-retardant high-performance polyimide airgel. Background technique [0002] Airgel is a low-density porous material. The complex three-dimensional nanopore structure makes it have the characteristics of low density, high specific surface area, low thermal conductivity, low sound transmission velocity and low dielectric constant. At the same time, these excellent properties make it have broad application prospects in the fields of heat insulation, sound insulation and noise reduction, catalyst carrier and liquid adsorption. [0003] The research on organic aerogels can be traced back to 1984 when Pekala in the United States used resorcinol and formaldehyde as raw materials to prepare aerogels of organic monomer polycondensation through sol-gel process and supercritical drying under alkaline conditions. Since then, a large number of organogels hav...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J9/28C08G73/10C08L79/08
CPCC08G73/1071C08J9/28C08J2379/08
Inventor 牛永安马亚辉张鑫裴英锦李满园
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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