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Production method of soft polyimide foam

A technology of polyimide and production method, which is applied in the production field of soft polyimide foam, can solve the problems of poor high temperature resistance of foam, poor mechanical properties of foam, high foam density, etc., and achieve good sound absorption performance, The effect of good thermal insulation performance

Active Publication Date: 2010-06-16
NEW YANGQIAO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Some soft thermoplastic polyimide foams are made of thermoplastic polyimide powder and foaming agent at high temperature, and the uniformity of the cells and the stability of the process are poor; the high temperature resistance of the foam is also poor.
However, some polyimide foams are obtained by directly using the esterification solution of dianhydride and isocyanate to react and ripen, and the mechanical properties of the foam are poor.
[0005] For example, in US 5,298,531 and 5,122,546,5,077,318, prepolymers are formed first, that is, one or two kinds of dianhydrides are dissolved in polar solvents, and small molecular alcohols such as methanol are added to make them esterified or half-esterified. Then add aromatic or aliphatic diamine to the solution. After the reaction is complete, the small molecules in the initial solution are removed to form a powder, and then the powder is foamed by high temperature to release small molecules such as water and methanol. The main disadvantage is that the drying of the prepolymer is extremely complicated and the density of the foam is too high to produce foams with lower densities
[0006] CN101402795A discloses a novel high-temperature-resistant polyimide foam, which also produces powder prepolymer by esterifying bisanhydrides and adding active diamines in the solution, and produces polyimide foam plastics by two-step method , and the foam is rigid foam with a density of 100-500kg / m 3 , not suitable for low density foam production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 200 grams of DMF solvent and 84 grams of PMDA into a 500 ml three-necked flask, slowly heat up to 100 ° C, stir to completely dissolve PMDA, the solution is yellow and transparent, add 3 grams of 1,1' di Amino diphenyl ether ODA, and the temperature was raised to 120 ° C, the solution turned into a rust red viscous liquid.

[0032] Cool the solution to 50°C, slowly add 12 grams of methanol, 2 grams of ethylene glycol ether, A-10.03 grams, A-330.03 grams, K-190.01 grams in order, and also add 12 grams of B8404 at the same time, mix well, and drop to 25°C.

[0033] Take 50 grams of the above solution, 2.5 grams of water, and 22 grams of PAPI, and quickly mix and stir in a high-speed mixer at a speed of 3000 rpm for 10 seconds. After stirring, quickly pour it into a paper mold and let it foam freely. After 15 minutes, , when the surface is dry and does not stick to hands, move the prepolymer foam into a microwave oven, and cure it for 10 minutes at a power of 1000W. ...

Embodiment 2

[0036] Add 200 grams of DMF solvent and 84 grams of PMDA in a 500 ml three-necked flask, slowly heat up to 100 ° C, stir to completely dissolve PMDA, the solution is yellow and transparent, add 6 grams of 1,1' di Amino diphenyl ether ODA, 6 grams of methylene dianiline MDA, and the temperature was raised to 120 ° C, the solution became rust red viscous liquid.

[0037] Cool the solution to 50°C, slowly add 6 grams of methanol, 1 gram of ethylene glycol ether, A-10.03 grams, A-330.03 grams, K-190.01 grams in order, and also add 12 grams of B8404 at the same time, mix well, and drop to 25°C.

[0038] Take 50 grams of the above solution, 2.2 grams of water, 15 grams of PAPI, and 9 grams of MDI in a high-speed mixer, and mix and stir rapidly at a speed of 2500 rpm for 7 seconds. After stirring, quickly pour it into a paper mold and let it foam freely , After about 10 minutes, when the surface is dry and not sticky, move the prepolymer foam into a microwave oven and cure it for 12...

Embodiment 3

[0041] Add 200 grams of DMF solvent, 75 grams of PMDA and 15 grams of BDTA into a 500 ml three-necked flask, slowly heat up to 100°C, stir to completely dissolve PMDA and BDTA, the solution is yellow and transparent, add 6 Gram 1,1' diaminodiphenyl ether ODA and the temperature was raised to 120°C, the solution turned into rust red viscous liquid.

[0042] Cool the solution to 50°C, slowly add 8 grams of methanol, 1 gram of ethylene glycol ether, A-10.03 grams, A-330.03 grams, K-190.01 grams in order, and also add 12 grams of B8404 at the same time, mix well, and drop to 25°C.

[0043] Take 50 grams of the above solution, 2.6 grams of water, and 27 grams of PAPI, and stir rapidly in a high-speed mixer at a speed of 2500 rpm for 10 seconds. After stirring, quickly pour it into a paper mold and let it foam freely for about 12 minutes Finally, when the surface is dry and does not stick to hands, the prepolymer foam is moved into a microwave oven and matured for 15 minutes at a p...

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Abstract

The invention provides a production method of soft polyimide foam, comprising the following steps: adding one or more than two kinds of aromatic dianhydride in polar solvent to be totally dissolved; then, adding aromatic diamine to generate amic acid; after reaction, adding two or more than two kinds of foaming agents, and adding one or more than two catalysts and surfactants; at room temperature, mixing the mixture with water and one or more than two kinds of aromatic isocyanate, and foaming; and finally, ripening generated foam in a microwave oven and a high temperature furnace. The polyimide foam obtained by the invention is soft, has elasticity and has favorable sound absorption performance and fire resistance; and the foam density is 4.0-8.0 kg / m3; foam stops firing when foam is far away from fire, so that the amount of emitted smog is small, and no drippage objects exist. Meanwhile, the polyimide foam of the invention has favorable thermal insulation property. The polyimide foam of the invention can be suitable for the fields of aerospace, military ships and the like.

Description

technical field [0001] The invention relates to a production method of polyimide foam, in particular to a production method of soft polyimide foam. Background technique [0002] The materials currently used for thermal insulation are mainly polyurethane foam and phenolic foam. However, polyurethane foam is not flame retardant at all, and produces a large amount of dripping and smoke when burning, with a smoke density of more than 80%; phenolic foam has good flame retardant performance, but the foam has no strength, is easy to pulverize, and the density is too high . However, polyimide foam does not drip when it burns, and its smoke density is only 8%. [0003] Polyimide is a polymer with excellent heat resistance. It has good mechanical and electrical properties, as well as radiation resistance and corrosion resistance. It is widely used in aerospace, military, electronics and other fields. The polyimide material with foam structure not only maintains the excellent heat r...

Claims

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Application Information

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IPC IPC(8): C08G73/10C08J9/04C08L79/08
Inventor 蒋卫民
Owner NEW YANGQIAO TECH
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