Preparation method of isocyanate-based polyimide foam

A technology of ester-based polyimide and isocyanic acid is applied in the field of preparation of polymer foam materials, which can solve the problem of reducing the heat resistance, thermal stability and flame retardancy of polyimide foam, and reducing polyimide foam. Problems such as low material density, poor thermal stability and flame retardancy, etc., to achieve the effect of reducing the amount of formation, inhibiting formation, and improving flame retardancy

Active Publication Date: 2015-08-12
HARBIN ENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the first way, due to the excessive amount of isocyanate, the amino group and residual isocyanate generated in the free foaming molding process will not continue to generate polyimide precursors but will form polyimide with poor thermal stability and flame retardancy. Urea, ultimately leading to a certain gap in the overall heat resistance and flame retardancy of the foam compared with pure polyimide foam, and the density of the foam obtained in this way is relatively high; in the second way Since the isocyanate is not pre-polymerized with the polybasic aromatic anhydride, the reaction between the isocyanate and water will be more violent in the foam molding process in this way compared to the first way, and the amount of amino groups and gas generated will be more, although The generated amino group will react with polybasic aromatic anhydride derivatives to form a polyimide precursor, but at the same time, the amino group will also react with a large number of unreacted isocyanate groups to form a large amount of polyurea, which will also greatly reduce the overall polyimide foam. Excellent heat resistance, thermal stability and flame retardancy, but the density of isocyanate-based polyimide foam produced in this way is relatively low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In a 500ml three-necked flask, add 200 grams of N,N-dimethylformamide and 109 grams of pyromellitic dianhydride and add a magnet, connect the reflux condenser tube to feed cooling water, and fully stir under the action of an electromagnetic stirrer Slowly raise the temperature to 90°C, stop heating when the pyromellitic dianhydride is completely dissolved, and the solution is in a clear state, and when the temperature drops to about 50°C, drop 32 grams of methanol into the turbid liquid with a constant pressure dropping funnel, The dropping rate is controlled at 1-5 milliliters per minute, so that pyromellitic dianhydride starts to undergo esterification reaction. After the esterification reaction is complete and the solution is clear and transparent again, the electromagnetic stirrer stops stirring, and the above solution is allowed to stand still to At room temperature, a nearly colorless hyaluronic acid diester solution was prepared, which was stored away from light u...

Embodiment 2

[0030] Take by weighing 21 grams of the above-mentioned diacid diester solution, add 3 grams of foam stabilizer, 3 grams of polyethylene oxide surfactant, 0.2 gram of fluorocarbon surfactant, 2 grams of compound catalyst, 4 grams of deionized water, and obtain after fully stirring white material.

[0031]In a 100ml three-necked flask, add 28 grams of N,N-dimethylformamide, 15 grams of pyromellitic dianhydride, 27 grams of polyphenyl polymethylene polyisocyanate and add magnets, place in an oil bath, Connect to a nitrogen protection device, fully stir under the action of an electromagnetic stirrer and slowly raise the temperature to 50°C, heat for 2 hours, the solution becomes orange-red and clear, and black material is obtained. Stop heating, quickly put the black material in an ice-water bath to cool to room temperature, then immediately pour it into the white material, stir quickly with an electric stirring paddle, and when the mixture starts to foam and rise, quickly pour i...

Embodiment 3

[0033] Take by weighing 35 grams of the above-mentioned diacid diester solution, add 3 grams of foam stabilizer, 3 grams of polyethylene oxide surfactant, 0.2 gram of fluorocarbon surfactant, 2 grams of compound catalyst, 4 grams of deionized water, and fully stir to obtain white material.

[0034] In a 100ml three-necked flask, add 20 grams of N,N-dimethylformamide, 11 grams of pyromellitic dianhydride, 27 grams of polyphenyl polymethylene polyisocyanate and add magnets, place in an oil bath, Connect to a nitrogen protection device, fully stir under the action of an electromagnetic stirrer and slowly raise the temperature to 50°C, heat for 2 hours, the solution becomes orange-red and clear, and black material is obtained. Stop heating, quickly put the black material in an ice-water bath to cool to room temperature, then immediately pour it into the white material, stir quickly with an electric stirring paddle, and when the mixture starts to foam and rise, quickly pour it into...

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Abstract

The invention provides a preparation method of isocyanate-based polyimide foam. The preparation method comprises that 1, polybasic aromatic anhydride is heated and dissolved in a polar solvent and undergoes a reaction with fatty alcohol to produce a polybasic aromatic anhydride derivative solution, 2, the polybasic aromatic anhydride derivative solution and a foam stabilizer are blended to form a white material, 3, polybasic aromatic anhydride and isocyanate undergo a reaction to produce a black material, 4, the foaming white material is immediately poured into the foaming black material at a room temperature under normal pressure, and the mixture is uniformly stirred, then is fast poured into a mold and is subjected to free foaming molding to form a foam intermediate and 5, the foam intermediate is heated and cured to form the isocyanate-based polyimide foam. The preparation method inhibits production of an amino group and an isocyanate group in foam material preparation, reduces a polyurea generation amount and improves isocyanate-based polyimide foam heat resistance, heat stability and flame resistance. The preparation method has the advantages of simple processes, excellent product comprehensive properties, and industrial production and wide application feasibility.

Description

technical field [0001] The invention relates to a method for preparing polymer foam material, in particular to a method for preparing isocyanate-based polyimide foam. Background technique [0002] Isocyanate-based polyimide foam belongs to a class of polyimide foams. Due to the free foaming molding process at room temperature and relatively low requirements for the purity of raw materials, it is different from the polyimide foam prepared by the powder method. Compared with the obvious industrial production advantages and market price advantages, it has stronger market competitiveness. [0003] According to patent documents such as US3300420, US4026833, US7541388, CN101812232A, CN102127225A and related paper reports of people such as Zhan Maosheng and Wang Liancai, the preparation method of isocyanate-based polyimide foam mainly contains two kinds of modes at present: 1. at first with polybasic aromatic anhydride and Excessive isocyanate reacts to form a black material, and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J9/08
Inventor 韩世辉孙高辉王文鹏刘连河王君王洪良魏浩
Owner HARBIN ENG UNIV
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