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Method for preparing hard open-cell polyimide foam

A technology of porous polyimide and foam is applied in the field of preparation of polymer polyimide foam materials, which can solve the problems of high requirements of molds, high temperature and high pressure resistance of molds, easy cracking of foams, etc., so as to improve uniformity and reduce Effects, small toxic effects

Active Publication Date: 2017-12-12
AEROSPACE RES INST OF MATERIAL & PROCESSING TECH +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has higher requirements on the mold used, and the mold needs to be resistant to high temperature and high pressure; and the foam prepared by this method is prone to cracking due to a large amount of gas discharge when the mold is opened, and there is a large amount of solvent in the post-processing process. how to deal with the problem

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0052] A preparation method of a rigid open-cell polyimide foam material, the steps are as follows:

[0053] (1) Add aromatic dianhydride to polar solvent, then add aliphatic alcohol, heat and react for 0.5-3 hours until completely transparent; then add catalyst, deionized water and foam stabilizer, and react for 0.5-2 hours to obtain transparent polyamide Imine foam precursor solution A liquid;

[0054] (2) Use an end-capping agent to block the polycyanate to obtain liquid B, then quickly mix it with liquid A in step (1) and leave it to foam, then pulverize and remove the solvent to obtain precursor powder C;

[0055] (3) Put the dry powder obtained in step (2) in an autoclave, and raise the temperature to 120-170°C for 0.1-2 hours, set the pressure at 0.1-4MPa, then rapidly raise the temperature to 200-250°C, and balance for 0.5-2 hours After 3 hours, the pressure was slowly released to obtain a polyimide foam material.

[0056] The aromatic dianhydrides include 1,2,4,5-py...

Embodiment 1

[0068] A preparation method of rigid open-cell polyimide foam mainly comprises the following steps:

[0069] a, Synthesis of liquid A: Take 2080g of N,N-dimethylformamide, then add 3220g of 3,3',4,4'-benzophenonetetraacid dianhydride (BTDA) into it, and heat up to 60 ℃, add 400g of ethanol, stir at constant temperature for 2.5h, then add 480g of water, after the system is clarified, add 30g of catalyst triethanolamine, 40g of stannous octoate, 380g of silicone oil AK8805, stir and react for 1h, then cool to room temperature, put into foaming In machine A material barrel;

[0070] b. Mix 10000g PAPI with 650g ethanol, put it into the B liquid storage tank of the foaming machine after standing for 2 hours;

[0071] c. Use a high-pressure foaming machine to mix liquid A and liquid B at a mass ratio of 1:1, pour it into a 1m×1m×1m carton, let it stand for 24 hours, and crush it. Take 500g of powder, add 2000g of ethanol, and stir After standing still, then filter, re-add 2000g o...

Embodiment 2

[0074] A preparation method of rigid open-cell polyimide foam material, comprising the following steps:

[0075] a. Synthesis of liquid A: Take 2080g of N,N-dimethylformamide, then add 3220g of 3,3',4,4'-benzophenone tetra-acid dianhydride (BTDA) into it, and heat up to 60 ℃, add 380g of ethanol, stir at constant temperature for 3 hours, then add 480g of water, after the system is clarified, add 30g of catalyst triethanolamine, 40g of stannous octoate, 380g of silicone oil AK8805, stir for 1 hour, cool down to room temperature, and put into a small foam In machine A material barrel;

[0076] b. Mix 10000g of PAPI with 1300g of ethanol, and put it into the B liquid storage tank of the foaming machine after standing for 2 hours;

[0077] c. Use a high-pressure foaming machine to mix liquid A and liquid B at a mass ratio of 1:1, pour it into a 1m×1m×1m carton, let it stand for 24 hours, and then pulverize it. Take about 300g of powder and add 2000g of ethanol. After stirring, l...

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Abstract

The present invention relates to a method for preparing hard open-cell polyimide foam, and belongs to the technical field of preparation of macromolecular polyimide foam materials. The method comprises the following steps: adding aromatic dianhydride into a polar solvent, and then adding fatty alcohol, so as to perform heating reaction; adding a catalyst, deionized water and a foam stabilizer, so as to obtain precursor solution; mixing the precursor solution with an end-capped reagent end-capped polyisocyanate, leaving to stand, foaming, crushing and drying, so as to obtain powder; putting the powder into a pressure vessel, and performing heating and pressurization, so as to obtain a polyimide foam material. The method has the characteristics that the solvent is small in volatile quantity and can be recycled during foam preparation, and is applied to various anhydride systems, the preparation cost is low, and mass production is easy to realize. The formed foam material has the characteristics that a foam structure is uniform, the apparent density is adjustable, the material is heat-resistant, high in strength, and drop of dregs hardly occurs.

Description

technical field [0001] The invention relates to a method for preparing rigid open-cell polyimide foam, which belongs to the technical field of preparation of polymer polyimide foam materials. Background technique [0002] Polyimide foam material has excellent flame retardancy, high temperature resistance and open flame resistance, and is a kind of high-performance foam material. Compared with other types of foamed plastics, it does not produce harmful gases during use, has a low density, a wide range of performance adjustments, and is easy to install and disassemble. It has been widely used abroad as a heat insulation and noise reduction material. [0003] At present, there are mainly two types of methods for industrialized preparation of polyimide foam materials. One is a two-step method based on aromatic dianhydride and aromatic diamine as the main raw materials, and the other is based on aromatic dianhydride and aromatic diamine. One-step process with polyisocyanate as t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J9/12C08L79/08C08G73/10
CPCC08G73/1035C08J9/122C08J2203/06C08J2205/05C08J2205/10C08J2379/08
Inventor 马晶晶酒永斌赵一搏王方颉马晓静许小强杨汝平
Owner AEROSPACE RES INST OF MATERIAL & PROCESSING TECH
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