Low-thermal-conductivity polyimide foam material and preparation method thereof

A technology of polyimide and foam materials, which is applied in the field of low thermal conductivity polyimide foam materials and its preparation, can solve the problems of low imidization degree, complex process, and many foam defects, and achieve shape integrity Good, simple process operation, low thermal conductivity effect

Pending Publication Date: 2020-08-28
GUIZHOU AEROSPACE TIANMA ELECTRICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] At present, the preparation process of polyimide foam is divided into one-step method and two-step method. The one-step method refers to making a foam precursor solution in a certain solvent with dianhydride or diacid ester, low molecular weight alcohol, catalyst and other additives. Condensation reaction with isocyanate then produces small molecular gas as foaming agent to prepare PI foam. This method has relatively simple process and short production cycle, but the degree of imidization is not high; the two-step method refers to the dianhydride first mixed with Diamine is reacted to prepare precursor powder, which is then foamed under certain conditions to prepare PI foam. This method can prepare foam with higher density, but the process is more complicated and there are many defects in the foam; therefore, the production cost is reduced. And production process conditions are still the focus of research on polyimide foam materials, and optimizing its unique properties is also crucial

Method used

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  • Low-thermal-conductivity polyimide foam material and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 1) Add 90g of 3,3`,4,4`-biphenyltetracarboxylic dianhydride into a reaction kettle filled with 120g of tetrahydrofuran, stir at 105°C for 30min to fully dissolve the dianhydride, the stirring method is magnetic stirring, stirring The speed is 400r / min to prepare the dianhydride solution; slowly add 20g of methanol into the dianhydride solution, keep the temperature at 60°C and stir for 1h to generate the precursor esterification solution. The stirring method is magnetic stirring, and the stirring speed is 550r / min;

[0040] 2) After the precursor esterification solution was lowered to room temperature, a catalyst composed of 0.8 g of stannous octoate, 0.8 g of triethanolamine, 1.1 g of tetramethylethylenediamine, 3.3 g of water and 2.5 g of p-toluenesulfonamidourea The composite foaming agent, 9.0g DC5950, and 8.6g polyethylene glycol 400 were sequentially added to the precursor esterification solution, and stirred for 10 minutes to make it evenly mixed to obtain a foa...

Embodiment 2

[0044] 1) Add 135g of pyromellitic dianhydride into a reaction kettle containing 160g of N,N-dimethylformamide, stir at 90°C for 45 minutes to fully dissolve the dianhydride, and prepare a dianhydride solution. The stirring method is magnetic Stir at a stirring rate of 1100r / min; slowly add 38g of propanol to the dianhydride solution, keep the temperature at 72°C and stir for 0.8h to generate a precursor esterification solution. The stirring method is magnetic stirring at a stirring rate of 660r / min. min;

[0045] 2) After the precursor esterification liquid is lowered to room temperature, a composite catalyst composed of 1.1g dibutyltin dilaurate, 1.2g pentamethyldiethylenetriamine, 0.8g triethylenediamine, 7.8g magnesium carbonate, The composite blowing agent composed of 6.9g n-hexane, 6.2g Span-60, 5.8g AK8803, and 8.6g polyethylene glycol 1000 were sequentially added to the precursor esterification solution, and stirred for 15 minutes to make it evenly mixed to obtain foam...

Embodiment 3

[0049] 1) Add 120g of 3,3`,4,4`-benzophenonetetracarboxylic dianhydride into a reaction kettle filled with 135g of dichloromethane, stir at 125°C for 25min to fully dissolve the dianhydride, and obtain di Anhydride solution, the stirring method is magnetic stirring, and the stirring rate is 800r / min; slowly add 36g of ethylene glycol into the dianhydride solution, keep the temperature at 82°C and stir for 1.5h to form a precursor esterification solution, the stirring method is Magnetic stirring, the stirring rate is 710r / min;

[0050] 2) After the precursor esterification solution was lowered to room temperature, 4.6g Triton x-100, 6.8g AK8805, 10.2g polyethylene glycol 600, composed of 4.5g petroleum ether and 7.8g dioxane were sequentially added to it Composite foaming agent, composite catalyst composed of 0.8g bismuth laurate, 0.6g triethylenediamine, 2.1g triethylenediamine, and stirred for 1h to make it mix uniformly to obtain foaming white material, the stirring method i...

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Abstract

The invention discloses a low-thermal-conductivity polyimide foam material and a preparation method thereof. The method comprises the following steps: mixing aromatic dianhydride with a polar solvent,dissolving under a heating condition, adding low-molecular-weight alcohol, and continuously heating to carry out esterification on each component to obtain an esterification precursor solution; adding a catalyst, a foaming agent, a surfactant, polymer polyol and a foaming agent, uniformly dispersing to obtain a foaming white material, finally adding isocyanate into the white material, quickly stirring for uniform dispersion, then putting the mixture into a mold, foaming and molding, and heating and curing after foaming is finished to obtain the polyimide foam material. The polyimide foam material prepared by the method has the advantages of low heat conductivity coefficient, high limit oxygen index, good flame retardance, uniform cell size, controllable density and high mechanical strength, and can be widely applied to the fields of aerospace, military ships and warships, building insulation, vehicle construction and the like.

Description

technical field [0001] The invention belongs to the technical field of polymer foaming materials, and in particular relates to a low thermal conductivity polyimide foaming material and a preparation method thereof. Background technique [0002] Polyimide foam material is a kind of lightweight porous foam plastic with specific chemical structure. Quality and other performance characteristics, excellent performance. It is widely used in aerospace, ships, construction, automobiles, electronic appliances, machinery industry and other fields or has great application potential. [0003] At present, the thermal insulation materials widely used are mainly inorganic materials such as rock wool, glass wool, and expanded perlite, and organic materials such as polyurethane foam and polystyrene board. Among them, rock wool and glass wool have poor thermal insulation performance, high moisture absorption rate, poor environmental protection performance, and are harmful to human health. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J9/08C08J9/10C08J9/12C08J9/14C08L79/08
CPCC08G73/1035C08J9/125C08J9/105C08J9/08C08J9/141C08J9/142C08J2379/08C08J2203/184C08J2203/14C08J2203/06C08J2203/04C08J2203/204C08J2203/10C08J2203/12
Inventor 丁泽柴鲜花杨大磊史建超刘方辉
Owner GUIZHOU AEROSPACE TIANMA ELECTRICAL TECH
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