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A kind of polyimide foam composite material and preparation method thereof

A technology of polyimide and composite materials, which is applied in the field of polyimide foam composite materials and its preparation, and can solve problems such as the inability to foam polyimide foaming rate, difficulty in adjusting the foaming process, and affecting foam performance , to achieve the effect of good mechanical properties, high glass transition temperature and uniform pore size

Active Publication Date: 2016-02-03
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, compared with polyimide resin, the foaming process of polyimide foam directly affects its internal cell structure, and its foaming process is influenced by many factors, such as foaming temperature, imidization temperature, The difference in the type and amount of additives may cause polyimide to be unable to foam or the foaming rate is low, and the cells are not uniform, thereby affecting the foam performance, and it is difficult to control the foaming process. Therefore, graphite has not yet been used. A report on polyimide foam reinforced with vinyl as filler

Method used

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  • A kind of polyimide foam composite material and preparation method thereof
  • A kind of polyimide foam composite material and preparation method thereof

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[0034] The present invention also provides a method for preparing the above-mentioned polyimide foam composite material, comprising the following steps: A1) mixing graphene or graphene oxide with polyamic acid, and concentrating to obtain the first foaming precursor; A2) mixing The first foaming precursor is subjected to heat treatment, and the first foam block is obtained after foaming; A3) The first foam block is subjected to thermal imidization treatment to obtain a polyimide foam composite material.

[0035] Wherein said graphene or graphene oxide is graphene or graphene oxide well known to those skilled in the art, and there is no particular limitation; said polyamic acid is polyamic acid well known to those skilled in the art, and There are no special restrictions.

[0036] In the present invention, the graphene is preferably prepared according to the following method: the graphite powder is ultrasonicated in water, and the upper liquid is collected after low-speed centr...

Embodiment 1

[0058] 1.1 Disperse the graphite powder in water, perform ultrasonication at 500W for 60min, then centrifuge at 8000rpm for 8min, collect the upper layer liquid, centrifuge at 15000rpm for 5min, collect the precipitate, and dry it in vacuum to obtain graphene powder. Take 0.053g of graphene powder and disperse it in absolute ethanol, and ultrasonicate at 500W for 150min to obtain a uniform graphene suspension.

[0059] 1.2 Mix 32.23g of 3,3′,4,4′-benzophenone tetracarboxylic dianhydride with 50ml of absolute ethanol, heat to 70°C for 4h under reflux to obtain a diacid diester solution, cool to room temperature, add 19.83g4 , 4′-diaminodiphenylmethane, 0.3g polysiloxane, 0.25g 1,2-dimethylimidazole and 25ml absolute ethanol were stirred and reacted for 8 hours to obtain a polyamic acid solution.

[0060] 1.3 Mix the graphene suspension obtained in 1.1 with the polyamic acid solution obtained in 1.2, stir for 10 hours, concentrate, dry and pulverize to obtain a foaming precursor...

Embodiment 2

[0066] 2.1 Mix 3g of graphite powder, 18g of potassium permanganate, 360ml of concentrated sulfuric acid and 40ml of concentrated phosphoric acid, stir, the reaction is exothermic, and after stabilization, react at 50°C for 12h, cool to room temperature, transfer the reaction solution to ice water, stir and add 30wt% 20ml of hydrogen peroxide was centrifuged, and the precipitate was collected, ultrasonically washed with 30% hydrochloric acid, ultrasonically washed with water, and vacuum-dried to obtain graphene oxide. Take 0.053 g of graphene oxide and disperse it in absolute ethanol, and ultrasonicate for 150 min to obtain a uniform graphene oxide suspension.

[0067] 2.2 Mix 32.23g of 3,3′,4,4′-benzophenone tetracarboxylic dianhydride with 50ml of absolute ethanol, heat to 70°C for 4h under reflux to obtain a diacid diester solution, cool to room temperature, add 19.83g4 , 4′-diaminodiphenylmethane, 0.25g polysiloxane, 0.3g 1,2-dimethylimidazole and 25ml absolute ethanol wer...

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Abstract

The invention provides a polyimide foamed composite, comprising one selected from the group consisting of a graphene sheet, a graphene oxide sheet and modified graphene oxide and polyimide foam, wherein the mass of the one selected from the group consisting of the graphene sheet, the graphene oxide sheet and the modified graphene oxide is 0.02 to 30% of the mass of the polyimide foam. Compared with polyimide foam in the prior art, the invention has the following advantages: since one selected from the group consisting of the graphene sheet, the graphene oxide sheet and the modified graphene oxide is used as an addition material for the polyimide foam and the proportion of the addition material is controlled, the problems of dispersibility and interfacial adhesiveness of graphene and graphene oxide in the polyimide foam are overcome, and the obtained polyimide foamed composite has a uniform bore diameter, no defects of breaking, combination and collapse of bubbles and incomplete imidization, good heat resistance, a high glass-transition temperature and good mechanical properties.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a polyimide foam composite material and a preparation method thereof. Background technique [0002] Polyimide foam refers to the soft and hard foam formed by polyimide resin as the main component, which contains microscopic / mesoscopic or macroscopic open-cell structures, closed-cell structures, or open-cell / closed-cell combined structures. Porous material, which has the characteristics of light weight, low density, good flexibility and rebound, heat insulation, sound absorption, etc., and compared with other foam materials such as polyurethane foam, polyethylene foam, polystyrene foam, etc., polyimide foam It also has excellent high temperature and low temperature barrier properties, flame retardancy, impact resistance, dimensional stability, etc., so it is widely used in aircraft, spacecraft, ships, weaponry, electronics and other fields. [0003] At prese...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L79/08C08K3/04C08K9/00C08K9/04C08K9/06C08G73/10C08J9/00
Inventor 董志鑫邱雪鹏陈文慧郭海泉高连勋
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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