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Preparation method of polyimide/silicon dioxide aerogel powder composite aerogel material

A composite aerogel and silica technology, which is applied in the field of aerogel material preparation, can solve the problems affecting industrial production and application, poor mechanical properties, easy to break, etc., and achieves low overall cost, excellent thermal insulation performance, The effect of cheap raw materials

Inactive Publication Date: 2016-07-27
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the extremely poor mechanical properties of traditional silica airgel, it is extremely easy to break during actual production and application, and it is prone to "powder falling" phenomenon even after being compounded with other materials. This defect is extremely serious. The earth has influenced its industrial production and application

Method used

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  • Preparation method of polyimide/silicon dioxide aerogel powder composite aerogel material
  • Preparation method of polyimide/silicon dioxide aerogel powder composite aerogel material
  • Preparation method of polyimide/silicon dioxide aerogel powder composite aerogel material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1: Preparation of polyimide / silica airgel powder composite airgel

[0023] Diamine (any of aromatic dianhydrides such as 4,4'-diaminodiphenyl ether, benzophenone tetracarboxylic dianhydride or pyromellitic dianhydride) and dianhydride (dianhydride is 3,3'4 , any of aromatic diamines such as 4'-biphenyltetracarboxylic dianhydride, p-phenylenediamine, 2,2-bis[4-(4-aminophenoxy)phenyl]propane) dissolved in 200mL of N - In methylpyrrolidone (take diaminodiphenyl ether: 3,3',4,4'-biphenyltetracarboxylic dianhydride = 1.672g: 2.556g as an example), synthesize polyamic acid solution, and then add 16.912g Silica airgel powder with a particle size of 20-50um, and stirred rapidly for half an hour, then added 12.1mL of dehydrating agent (oxalic acid: pyridine = 6.5mL: 5.6mL), stirred rapidly and allowed to gel at room temperature . After 24 hours, the solution was replaced three times with a mixed solution of N-methylpyrrolidone and acetone, 8-12 hours each time. Then u...

Embodiment 2

[0024] Example 2: Preparation of polyimide / silica airgel powder composite airgel

[0025] Diamine (any of aromatic dianhydrides such as 4,4'-diaminodiphenyl ether, benzophenone tetracarboxylic dianhydride or pyromellitic dianhydride) and dianhydride (dianhydride is 3,3'4 , any of aromatic diamines such as 4'-biphenyltetracarboxylic dianhydride, p-phenylenediamine, 2,2-bis[4-(4-aminophenoxy)phenyl]propane) (diaminodiphenyl Ether: 3,3',4,4'-biphenyltetracarboxylic dianhydride=1.672g: 2.556g) dissolved in 200mL of N-methylpyrrolidone (diaminodiphenyl ether: 3,3',4 ,4'-biphenyltetracarboxylic dianhydride=1.672g: 2.556g as an example),, synthesize polyamic acid solution, then add 4.228g of silica airgel powder with a particle size of 20-50um, and quickly Stir for half an hour, then add 12.1mL of dehydrating agent (oxalic acid: pyridine = 6.5mL: 5.6mL), stir rapidly and then gel at room temperature. After 24 hours, the solution was replaced three times with a mixed solution of N-m...

Embodiment 3

[0026] Embodiment 3: Preparation of polyimide / silica airgel powder composite airgel

[0027] Diamine (any of aromatic dianhydrides such as 4,4'-diaminodiphenyl ether, benzophenone tetracarboxylic dianhydride or pyromellitic dianhydride) and dianhydride (dianhydride is 3,3'4 , any of aromatic diamines such as 4'-biphenyltetracarboxylic dianhydride, p-phenylenediamine, 2,2-bis[4-(4-aminophenoxy)phenyl]propane) (diaminodiphenyl Ether: 3,3',4,4'-biphenyltetracarboxylic dianhydride=1.672g: 2.556g) dissolved in 200mL of N-methylpyrrolidone (diaminodiphenyl ether: 3,3',4 ,4'-biphenyltetracarboxylic dianhydride=1.672g: 2.556g as an example),, synthesize polyamic acid solution, then add 1.057g of silica airgel powder with a particle size of 20-50um, and quickly Stir for half an hour, then add 12.1mL of dehydrating agent (oxalic acid: pyridine = 6.5mL: 5.6mL), stir rapidly and then gel at room temperature. After 24 hours, the solution was replaced three times with a mixed solution of ...

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Abstract

The invention relates to a preparation method of a polyimide / silicon dioxide aerogel powder composite aerogel material. Polyamide acid sol is synthesized from diamine and dianhydride monomers with a sol-gel method, common silicon dioxide aerogel particles and a polyamide acid solution are evenly mixed, composite gel is formed through a chemical imidization process, drying is performed with a supercritical drying technology, and the polyimide / silicon dioxide aerogel powder composite aerogel material is prepared. The method has the characteristics of wide application range, simple reaction process, low total cost and the like. High-temperature-resistant polymer polyimide plays roles in collecting and fixing silicon dioxide powder, and the nano-porous structure and excellent performance of the silicon dioxide aerogel are reserved. The introduction of inorganic silicon dioxide aerogel powder plays a role in inhibiting shrinking of organic polyimide. The material has excellent heat shielding performance and the heat conductivity is only 0.028-0.032 W / mK. The modulus of the composite aerogel is higher than that of pure silicon dioxide aerogel and is 0.8-11.8 MPa, and powder embedded in polyimide cannot fall off.

Description

technical field [0001] The invention belongs to the technical field of airgel material preparation, and in particular relates to a preparation method of polyimide / silicon dioxide airgel powder composite airgel material. Background technique [0002] As a special functional material with a nano-open pore structure, airgel is widely used in many fields due to its superior performance. However, due to the extremely poor mechanical properties of traditional silica airgel, it is extremely easy to break during actual production and application, and it is prone to "powder falling" phenomenon even after being compounded with other materials. This defect is extremely serious. The earth has influenced its industrial production and application. [0003] As a kind of organic aerogel with good mechanical properties, high thermal stability and good thermal insulation performance, polyimide airgel has attracted extensive attention in recent years. Large shrinkage is a difficult problem t...

Claims

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Application Information

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IPC IPC(8): C08L79/08C08K3/36C08J3/075C08G73/10
CPCC08K3/36C08G73/1067C08G73/1071C08J3/075C08J2379/08C08L2201/08C08L79/08
Inventor 周斌吴帅杜艾
Owner TONGJI UNIV
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