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Preparation method of crosslinked polyimide silicon dioxide mixed gas gel

A polyimide and silicon dioxide technology, which is applied in the field of nanoporous material preparation, can solve problems such as poor mechanical properties aerogel, and achieve the effects of high specific surface area, high strength and low density

Inactive Publication Date: 2015-02-11
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the extremely poor mechanical properties are the biggest obstacle to the widespread use of aerogels.

Method used

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  • Preparation method of crosslinked polyimide silicon dioxide mixed gas gel
  • Preparation method of crosslinked polyimide silicon dioxide mixed gas gel
  • Preparation method of crosslinked polyimide silicon dioxide mixed gas gel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1 : Preparation of cross-linked polyimide-silica hybrid airgel

[0023] Diamine, dianhydride and silane coupling agent (p-phenylenediamine: diaminodiphenyl ether: 3,3',4,4'-biphenyltetracarboxylic dianhydride: bis[3-(trimethoxysilane base) propyl] amine=1mol:1mol:2.07mol:4.14mol) dissolved in N-methylpyrrolidone, mixed into 27ml of A solution, deionized water, organic silicon source and ammonia water (deionized water: methyl trimethyl Oxygen silicon source: ammonia water = 0.15ml: 3ml: 0.15ml) dissolved in N-methylpyrrolidone and mixed to form 3ml of B solution. Stir the A solution evenly, then pour into the B solution, stir rapidly, then add 6.1ml of dehydrating agent (oxalic acid: pyridine = 1mol: 1mol), stir rapidly and then 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 use pure acetone to replace the solvent for 3 times, each time for 8-1...

Embodiment 2

[0024] Example 2 : Diamine, dianhydride and silane coupling agent (p-phenylenediamine: diaminodiphenyl ether: 3,3',4,4'-biphenyltetracarboxylic dianhydride: bis[3-(trimethoxy Silicon-based) propyl] amine = 1mol: 1mol: 2.07mol: 4.14mol) dissolved in N-methylpyrrolidone, mixed into 27ml of A solution, deionized water, organic silicon source and ammonia water (deionized water: methyl Trimethoxysilane source: ammonia water = 0.1ml: 1ml: 0.1ml) was dissolved in N-methylpyrrolidone and mixed to form 3ml of B solution. Stir the A solution evenly, then pour into the B solution, stir rapidly, then add 6.1ml of dehydrating agent (oxalic acid: pyridine = 1mol: 1mol), stir rapidly and then 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. The gel was then replaced with pure acetone three times for 8-12 hours each time, and finally supercritically dried.

Embodiment 3

[0025] Example 3: Diamine, dianhydride and silane coupling agent (p-phenylenediamine: diaminodiphenyl ether: 3,3',4,4'-biphenyltetracarboxylic dianhydride: bis[3-(trimethoxysilane base) propyl] amine=1mol:1mol:2.07mol:4.14mol) dissolved in N-methylpyrrolidone, mixed into 27ml of A solution, deionized water, organic silicon source and ammonia water (deionized water: methyl trimethyl Oxygen silicon source: ammonia water = 0.5ml: 10ml: 0.5ml) dissolved in N-methylpyrrolidone and mixed to form 3ml of B solution. Stir the A solution evenly, then pour into the B solution, stir rapidly, then add 6.1ml of dehydrating agent (oxalic acid: pyridine = 1mol: 1mol), stir rapidly and then 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. The gel was then replaced with pure acetone three times for 8-12 hours each time, and finally supercritically dried.

[0026] figure 2 As shown...

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Abstract

The invention belongs to the technical field of gel material and particularly relates to a preparation method of crosslinked polyimide silicon dioxide mixed gas gel. The preparation method is a sol / gel-organic / inorganic hybridization method and specifically comprises the following steps: mixing an organic silicon source containing a silane coupling agent with polyamide acid, carrying out imidization to form wet gel and carrying out a supercritical drying process to obtain the crosslinked polyimide silicon dioxide mixed gas gel. The preparation method has the characteristics of easily available raw materials, simple reaction process and the like; the prepared material has a nano-scale multi-stage microstructure, and has the density of less than 175mg / cm<3>, the specific area of more than 450m<2> / g and the elasticity modulus high up to 17MPa at most; and the problems that conventional silica aerogel is fragile and low in strength are solved.

Description

technical field [0001] The invention belongs to the technical field of preparation of nanoporous materials, and in particular relates to a general method for airgel materials widely used in aerospace deep space exploration, light-weight high-strength heat insulation and the like. Background technique [0002] As a special engineering material, polyimide has been widely used in aviation, aerospace, microelectronics, nanometer, liquid crystal, separation membrane, laser and other fields. Recently, countries are listing the research, development and utilization of polyimide as one of the most promising engineering plastics in the 21st century. Aerogels are a class of nanoporous functional materials with hierarchical fractal structures. Due to the combination of macroscopic properties and nano-effects, it exhibits many unique properties and has broad application prospects. However, the extremely poor mechanical properties are the biggest obstacle to the widespread use of aerog...

Claims

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Application Information

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IPC IPC(8): C08G73/10C08K3/36C08L79/08C08J3/075C08J9/28
Inventor 周斌闫彭杜艾
Owner TONGJI UNIV