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Environmentally friendly preparation method and product of flexible polyimide thermal insulation foam

A polyimide and environment-friendly technology, which is applied in the field of environment-friendly preparation of flexible polyimide thermal insulation foam, achieves the effects of saving preparation costs, realizing environmental friendliness, and high controllability of experimental operations.

Active Publication Date: 2022-07-26
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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  • Environmentally friendly preparation method and product of flexible polyimide thermal insulation foam
  • Environmentally friendly preparation method and product of flexible polyimide thermal insulation foam
  • Environmentally friendly preparation method and product of flexible polyimide thermal insulation foam

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0034] see in combination figure 1 , figure 1 The digital photograph of the carboxylate solution prepared by using tert-butanol in Example 1 at room temperature of 20° C. for 36 hours.

Embodiment 2

[0039] To the di-tert-butyl pyromellitic acid solution prepared in Example 1, add 2.2 grams of compound catalysts composed of Dabco33-LV, dibutyltin dilaurate and triethanolamine, 3 grams of AK8805 foam stabilizer, 2.6 grams of The ionized water foaming agent is mixed 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 foamed slurry, and quickly pour it into a mold for free foaming to obtain a foam intermediate. After the body is set, it is put into a high temperature oven at 180°C for 1.5 hours of high temperature curing, and then the temperature is raised to 240°C and cured for 1 hour. A flexible polyimide insulating foam with regular cell structure was obtained.

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

Embodiment 3

[0044] Add 9 grams of polar solvent N,N-dimethylformamide to 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 condensation reflux device. When the temperature of the emulsion reaches 135° C., 19 g of isoamyl alcohol is added thereto to carry out esterification reaction. After 6 hours, the esterification reaction was complete, the solution was clear and transparent, stirring and heating were stopped to obtain a solution of diisoamyl pyromellitic acid, and the solution was cooled to room temperature for use, and the solid content was 82.4%.

[0045] To above-mentioned diisoamyl pyromellitic acid solution, add compound catalyst 3.0 grams, 4 grams of AK8805 foam stabilizer, 4 grams of deionized water foaming agent composed of Dabco33-LV, dibutyltin dilaurate and triethanolamine , and stir evenly to obtain a compound slurry. Add 2...

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Abstract

The invention discloses an environment-friendly preparation method and product of a flexible polyimide thermal insulation foam, and also discloses a preparation method of an aromatic carboxylate solution; the invention uses carbon atoms to connect two or more branched aliphatic hydrocarbon groups. The aliphatic alcohol with large steric hindrance reacts with pyromellitic dianhydride in a polar solvent to obtain a low-cost aromatic carboxylic acid ester solution with high concentration and long-term storage. The prepared carboxylate solution is uniformly mixed with compound catalyst, foam stabilizer and foaming agent to obtain compound slurry; after isocyanate and compound slurry are quickly mixed uniformly, foamed slurry is obtained, and the foamed slurry is free at room temperature The polyimide foam intermediate is obtained by foaming, and after post-curing treatment, flexible polyimide foam is obtained, so as to realize low-cost and simple process preparation of flexible polyimide thermal insulation foam, and can greatly reduce the amount of solvent , to achieve the environmental friendliness of the preparation process.

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 product of flexible polyimide insulating foam. Background technique [0002] Polyimide foam has been widely used in aerospace, ships and other fields due to its advantages of light weight, high and low temperature resistance, extremely high flame retardancy, low combustion smoke toxicity, heat insulation and sound absorption. 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 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 , CN106...

Claims

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Application Information

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Patent Type & Authority Patents(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