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Environment-friendly preparation method of flexible polyimide heat insulation foam, and product

A polyimide, environment-friendly technology, applied in the field of environment-friendly preparation of flexible polyimide heat insulation foam, to achieve the effect of high controllability of experimental operation, environmental friendliness and simple process flow

Active Publication Date: 2020-06-02
HARBIN ENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In view of the above defects and problems, in order to solve the shortcomings of the existing one-step technology in the preparation of flexible polyimide foam materials, the present invention provides an environmentally friendly preparation method and products of flexible polyimide heat insulation foam

Method used

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  • Environment-friendly preparation method of flexible polyimide heat insulation foam, and product
  • Environment-friendly preparation method of flexible polyimide heat insulation foam, and product
  • Environment-friendly preparation method of flexible polyimide heat insulation foam, and product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 11 grams of polar solvent N,N-dimethylformamide into a 100ml three-necked flask, put a magnet, add 23 grams of pyromellitic dianhydride, then put the flask into an oil bath, and set the heating temperature 125°C. Turn on the stirring and install the condensing reflux device. When the temperature of the emulsion reached 125° C., 17 grams of tert-butanol was added thereto for esterification. After 5 hours, the esterification reaction was complete, and the solution was clear and transparent. Stirring and heating were stopped to obtain a di-tert-butyl pyromellitic acid solution. The solution was lowered to room temperature for use, and the solid content was 78.4%.

[0034] see in conjunction figure 1 , figure 1 This is a digital photo of the carboxylate solution prepared with tert-butanol in Example 1 after it was placed at room temperature at 20° C. for 36 hours.

Embodiment 2

[0039] In the di-tert-butyl pyromellitic acid solution prepared in embodiment example 1, 2.2 grams of composite catalysts, 3 grams of AK8805 foam stabilizer, 2.6 grams of desulfurized The ionic water foaming agent is stirred evenly at room temperature to obtain a compound slurry. Add 27 grams of diphenylmethane diisocyanate to the compound slurry, stir and mix quickly with a high-speed stirring paddle to obtain a foam slurry, quickly pour it into a mold for free foaming, and obtain a foam intermediate. After the body is shaped, it is placed in a high-temperature oven at 180°C for 1.5 hours of high-temperature curing, and then the temperature is raised to 240°C for another hour of curing. A flexible polyimide thermal insulation foam with regular cell structure was obtained.

[0040] During the preparation process of the flexible polyimide foam, the volatilization amount of the solvent is only 12.8% of the mass of the foam slurry, and the three-dimensional shrinkage rate of len...

Embodiment 3

[0044] Add 9 grams of polar solvent N,N-dimethylformamide into a 100ml three-necked flask, put in a magnet, add 23 grams of pyromellitic dianhydride, then put the flask into an oil bath, and set the heating temperature 125°C. Turn on the stirring and install the condensing reflux device. When the temperature of the emulsion reached 135° C., 19 grams of isoamyl alcohol was added thereto for esterification. After 6 hours, the esterification reaction was complete, and the solution was clear and transparent. Stirring and heating were stopped to obtain a diisoamyl pyromellitic acid solution, which was cooled to room temperature for use. The solid content was 82.4%.

[0045] Add 3.0 grams of composite catalyst, 4 grams of AK8805 foam stabilizer, and 4 grams of deionized water blowing agent to the above-mentioned diisoamyl pyromellitic acid solution. , and stir evenly to obtain compound slurry. Add 27.5 grams of triphenylmethane triisocyanate to the compound slurry, stir and mix q...

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Abstract

The invention discloses an environment-friendly preparation method of flexible polyimide heat insulation foam, and a product, and also discloses a preparation method of an aromatic carboxylic ester solution. Fatty alcohol with large steric hindrance, of which carbon atoms are connected with two or more aliphatic hydrocarbon branched chains, reacts with pyromellitic dianhydride in a polar solvent to obtain the low-cost aromatic carboxylate solution which is high in concentration and can be stored for a long time. The prepared carboxylate solution is uniformly mixed with a compound catalyst, a foam stabilizer and a foaming agent to obtain a compound slurry; and isocyanate is quickly and uniformly mixed with the compound slurry to obtain a foamed slurry, the foamed slurry is freely foamed atroom temperature to obtain a polyimide foam intermediate, and the polyimide foam intermediate is subjected to post-curing treatment to obtain the flexible polyimide foam. Low-cost and simple-process preparation of the flexible polyimide heat-insulating foam is achieved, the solvent consumption is greatly reduced, and environmental friendliness in the preparation process is achieved.

Description

technical field [0001] The invention relates to the technical field of flexible polymer foam materials, in particular to an environment-friendly preparation method and products of flexible polyimide heat-insulating foam. Background technique [0002] Due to its light weight, high and low temperature resistance, high flame retardancy, low combustion smoke toxicity, heat insulation and sound absorption, polyimide foam has been widely used in aerospace, ships and other fields. The flexible polyimide foam can be bent at will and has good adaptability to the tortuosity of the application interface, so it has a wider range of applications and fields than rigid and rigid polyimide foams. [0003] 根据美国专利US4656198、US4670478、US6133330、US60840000、US6180746B1、US4900761、US5096932、US5900440、US4177333、US5153234、US4804504、US4855332、US6956066B2、US2006063834、US20040249002以及中国专利CN104774330、CN101407594A、CN101402743A、CN102093714A、CN102134395A、CN105237766B、CN102134396A、CN104774330A , CN106380600...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J9/12C08L79/08C07C67/08C07C69/76C07D307/89
CPCC08G73/1035C08G73/1067C08J9/125C07C67/08C07D307/89C08J2379/08C08J2203/10C07C69/76
Inventor 孙高辉张洁任晓荷韩世辉陈蓉蓉王君段天娇
Owner HARBIN ENG UNIV
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