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Polyimide foamed plastic and preparation method thereof

A technology of polyimide and foam plastics, which is applied in the field of polyimide foam plastics and its preparation, can solve the problems of difficult crushing into uniform powder, complicated process preparation, and no reports, and achieve consistent temperature resistance and preparation The effect of simple process and increased compression modulus

Inactive Publication Date: 2017-06-20
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the above-mentioned patents, most of them use the two-step reaction of esterification to obtain the polyimide precursor solution, and finely adjust the proportion of raw materials or add additives to improve the performance of polyimide foam, and the process preparation is relatively complicated.
The higher viscosity precursor means that it is difficult to crush into uniform powder, and it is difficult to prepare polyimide foam with uniform pore size.
Changing part of the dianhydride to four acids is one of the methods used to reduce the viscosity of the precursor solution when preparing polyimide materials, but there are basically no reports in the foam field

Method used

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  • Polyimide foamed plastic and preparation method thereof
  • Polyimide foamed plastic and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Mix 20.02g (0.1mol) of 4'4-diaminodiphenyl ether with 40.38g of methanol and 161.53g of tetrahydrofuran and add 27.92g (0.09mol) of 3,3',4,4' - diphenyl ether tetra-acid dianhydride, react at 50° C. for 4 hours, then add 2.54 g (0.01 mol) of pyromellitic acid and continue the reaction for 4 hours to obtain a polyimide precursor solution.

[0034] (2) The solution in step (1) was dried at room temperature, and then placed in a vacuum oven at 60° C. for 10 hours to form a brittle solid. Take it out and crush it into powder with uniform particle size.

[0035] (3) paving the powder in step (2) on a volume of 1670cm 3 In the mold, put it into a high-temperature furnace at 250° C. to close the mold and foam for 1 hour to obtain the final polyimide foam.

[0036] The polyimide foamed plastics in the present embodiment is measured, and the density of this foam is 33.3Kg / m 3 , the glass transition temperature is 275°C, the 5% thermal weight loss is 570°C, the compressive...

Embodiment 2

[0038] (1) Mix 20.02g (0.1mol) of 4'4-diaminodiphenyl ether with 40.38g of methanol and 161.53g of tetrahydrofuran, then add 21.71g (0.07mol) of 3,3',4,4' -Diphenyl ether tetraacid dianhydride, react at 30°C for 2 hours, then add 7.62g (0.03mol) of pyromellitic acid to continue the reaction for 1 hour, then add 1.03g of polydimethylsiloxane to obtain polyimide precursor solution.

[0039](2) Pour out the solution in step (1) until it stops flowing, and then put it into a vacuum oven at 60° C. for 20 hours to vacuum dry to form a brittle solid. Take it out and crush it into powder with uniform particle size.

[0040] (3) pave the powder in step (2) to a volume of 960cm 3 In the mold, put it into a high-temperature furnace at 240° C. to close the mold and foam for 1 hour to obtain the final polyimide foam.

[0041] The polyimide foamed plastics in the present embodiment is measured, and the density of this foam is 47.5Kg / m 3 , the glass transition temperature is 277°C, the 5...

Embodiment 3

[0043] (1) Mix 19.83g (0.1mol) of 4'4-diaminodiphenylmethane with 40.23g of methanol and 160.93g of tetrahydrofuran and add 27.92g (0.09mol) of 3,3',4,4' -Diphenyl ether tetraacid dianhydride, react at 40°C for 6 hours, then add 2.54g (0.01mol) of pyromellitic acid to continue the reaction for 4 hours, then add 1.03g of polydimethylsiloxane to obtain polyimide precursor solution.

[0044] (2) Pour the solution of step (1) into a container, put it into a vacuum oven at 40° C. for 10 hours and vacuum dry it to form a brittle solid after it stops flowing. Take it out and crush it into powder with uniform particle size.

[0045] (3) paving the powder in step (2) on a volume of 1670cm 3 In the mold, put it into a high-temperature furnace at 250° C. to close the mold and foam for 1 hour to obtain the final polyimide foam.

[0046] The polyimide foam plastic in the present embodiment is carried out performance measurement, and the density of this foam is 37.8Kg / m 3 , the glass tr...

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Abstract

The invention relates to a preparation method for a polyimide foamed plastic. The preparation method comprises the following steps: (1) adding aromatic diamine and a mixed solvent of low-molecular-weight alcohol and tetrahydrofuran into a reactor, carrying out uniform mixing under stirring and then adding aromatic dianhydride for a reaction; (2) adding aromatic tetracid into a reaction solution obtained in the step (1) and continuing a reaction so as to obtain a polyimide precursor solution, wherein the addition amount of aromatic tetracid allows a mol ratio of aromatic dianhydride and aromatic tetracid to aromatic diamine to be 1: 1; and (3) drying the polyimide precursor solution obtained in the step (2), carrying out crushing into powder and then spreading the powder into a die for heating and foaming so as to obtain the final polyimide foamed plastic. According to the preparation method, a part of aromatic diamine is replaced by a proper amount of aromatic tetracid, so the precursor solution with low bulk viscosity is obtained and the eventual performance of foam is maintained; and the foaming temperature of the plastic is ensured to be matched with traditional process.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a polyimide foam plastic and a preparation method thereof. Background technique [0002] Due to its excellent comprehensive performance, polyimide foam has become one of the research hotspots in various countries in recent years. Polyimide foam has many characteristics such as good temperature resistance (-250°C ~ 450°C), excellent flame retardant and heat insulation properties, radiation resistance, low toxicity, oxidation resistance, hydrolysis resistance, and excellent sound absorption performance. It can be widely used in military and aerospace industries such as heat insulation of rockets, aircraft, aircraft carriers, submarines, etc., as well as in the field of high temperature resistance, heat insulation and noise reduction for civilian use. However, there are few types of raw materials that can be used to synthesize high-performance polyimide foam, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J9/28
CPCC08G73/1067C08G73/1071C08J9/286
Inventor 郭宝华丁光敏徐军
Owner TSINGHUA UNIV
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