Preparation method of high-strength organosilicon and polyimide composite foam

A polyimide and composite foam technology, which is applied in the field of preparation of high-strength silicone and polyimide composite foam, can solve the problems of unfavorable large-scale industrial production, unstable mechanical properties of materials, and incapable structural support materials. Achieve long-term maintenance of material mechanical properties, speed up the pace of progress, and reduce the effect of foaming ratio

Active Publication Date: 2018-02-13
HARBIN ENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, due to the limitations of the mechanical properties of polyimide foam, in the above-mentioned cutting-edge technical fields, polyimide foam is mainly used as a flexible material and cannot be used as a structural support material.
In order to effectively improve the mechanical properties of polyimide foam materials and further broaden the application fields of this type of high-performance polymer porous materials, patent documents such as CN101130632A have successively reported the improvement of the mechanical properties of polyimide foam by introducing inorganic functional fillers. However, the introduction of inorganic functional fillers often causes severe cell structure changes in foam materials; EP0514623A2, US5188879 and other patent documents have successively reported methods for improving the mechanical properties of polyimide foam by introducing honeycomb core materials, but this method The preparation process is complicated, which is not conducive to large-scale industrial production; in industrial production, the method of post-compression and post-processing of the original flexible foam is usually used to improve the mechanical properties of polyimide foam. During use, the deformation will gradually recover, which will lead to the instability of the mechanical properties of the material

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] In a 50ml three-neck flask, add 22.5 grams of N,N-dimethylformamide and 15.5 grams of 3,3',4,4'-benzophenone tetra-acid dianhydride (BTDA) into the magnetic sub, and then connect the reflux condenser Put cooling water into the tube, fully stir under the action of a magnetic stirrer and slowly heat up to 60°C, then drop 1.7 g of methanol into the turbid liquid with a constant pressure dropping funnel, and the dropping rate is controlled at 1-5 ml per minute. Make 3,3',4,4'-benzophenonetetraacid dianhydride (BTDA) begin to carry out esterification reaction, treat that esterification reaction is carried out completely, make nearly colorless transparent carboxylate solution, above-mentioned solution Allow to cool down to room temperature, and store away from light for later use.

[0030] Add 3 grams of polyoxyethylene surfactant, 0.2 gram of fluorocarbon surfactant, 1.5 grams of composite catalyst, 15 grams of BTDA, and 3 grams of deionized water to the above-mentioned diac...

Embodiment 2

[0037] Prepare the carboxylate solution of the same quality according to the formula described in the implementation example 1, add 3 gram polyethylene oxide surfactants, 0.2 gram fluorocarbon surfactants, 1.5 gram composite catalysts, 15 gram BTDA, 3 gram deionized water, After stirring well, a white material is formed. Add 15 grams of xylene and 30 grams of polydimethylsiloxane type hydroxy silicone oil with a viscosity of 10000 cP to the white material, and stir well to obtain a combined material.

[0038] Quickly pour 60 grams of PAPI into the white emulsion, and stir it evenly with a mechanical stirring paddle. When the mixture starts to foam and rise, quickly pour it into the mold to foam freely. The foam intermediate is allowed to stand at room temperature for 8 minutes Afterwards, it was transferred to an electric blast drying oven preheated to 240° C. for curing for 100 minutes to obtain a silicone-polyimide composite foam.

[0039] The performance and properties of ...

Embodiment 3

[0044] In a 50ml three-necked flask, add 22 grams of N-methylpyrrolidone and 15 grams of pyromellitic dianhydride (PMDA) into the magnet, connect the reflux condenser and feed cooling water, fully stir and slowly heat up under the action of a magnetic stirrer to 60°C, then drop 2.8 grams of ethanol into the turbid liquid with a constant pressure dropping funnel, the rate of addition is controlled at 1-5 milliliters per minute, so that pyromellitic dianhydride (PMDA) begins to undergo esterification reaction, After the esterification reaction is complete, a transparent carboxylate solution close to brownish yellow is obtained, and the above solution is left to cool down to room temperature, and stored away from light until use.

[0045]To above-mentioned carboxylate solution, add 3 grams of polyethylene oxide surfactants, 0.2 grams of fluorocarbon surfactants, 1.5 grams of composite catalysts, 10 grams of PMDA, 3 grams of deionized water, form white material after fully stirring...

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Abstract

The invention provides a preparation method for high-strength organosilicone and polyimide compound foam. The preparation method comprises the following steps of firstly, heating multiple aromatic anhydride in a strong polar solvent and reacting with fatty alcohol to obtain a multiple aromatic anhydride derivative carboxylic ester solution; secondly, sequentially adding a catalyst, a surfactant, residual multiple aromatic anhydride and deionized water into the carboxylic ester solution under room temperature conditions to obtain a white material; thirdly, adding a weak polar solvent and hydroxyl silicone oil into the white material to form a uniform combined material; fourthly, quickly adding isocyanate into the combined material for quickly and uniformly stirring to obtain mixed slurry, and quickly pouring the mixed slurry into a die for freely foaming to obtain a foam intermediate; fifthly, heating and curing the foam intermediate to obtain the organosilicone and polyimide compound foam. According to the preparation method provided by the invention, a free foaming mode is adopted, the operation flow is simple, industrial production is easily realized, the production cost is lower, the mechanical properties of products are remarkably improved, and the mechanical properties of materials can be permanently maintained.

Description

technical field [0001] The invention relates to a method for preparing a foam material, in particular to a method for preparing a high-strength organosilicon and polyimide composite foam. Background technique [0002] Polyimide is a kind of high-performance resin with alternating benzene rings and imine rings to form a polymer backbone. Polyimide foam combines the excellent heat resistance, radiation resistance, flame retardancy of polyimide resin and the remarkable heat insulation and vibration reduction properties of porous materials. Therefore, it is widely used in space exploration, cutting-edge equipment and other technical fields. Wait until unanimous approval and application. [0003] However, due to the limitation of the mechanical properties of polyimide foam, polyimide foam is mainly used as a flexible material in the above-mentioned cutting-edge technical fields at present, and cannot be used as a structural support material yet. In order to effectively improve ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/76C08G18/61C08G18/64C08G73/10C08G101/00
CPCC08G18/61C08G18/6438C08G18/7664C08G73/1003C08G2101/00
Inventor 韩世辉孙高辉刘连河王君王洪良王文鹏
Owner HARBIN ENG UNIV
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