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High-density hard flame-retardant polyimide foam material and preparation method thereof

A technology of foam materials and polyimide, which is applied in the field of preparation of high-density rigid flame-retardant polyimide foam materials, can solve the problems of difficult removal of solvents, uneven distribution of catalysts, severe local reactions, etc., and achieve thermal insulation Excellent thermal and flame retardancy, high economy and environmental friendliness, high density and high tensile strength

Active Publication Date: 2020-12-25
GUIZHOU AEROSPACE TIANMA ELECTRICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, in the traditional method, catalysts are mostly added sequentially, which may lead to uneven distribution of solid catalysts or catalysts with high viscosity, which will lead to severe local reactions in the system and uneven performance of the products produced.
[0005] High-density rigid polyimide foam has the possibility of using polyimide foam as a structural material due to its high compressive strength and energy-absorbing properties. Amine foam, because it is difficult to prepare large batches and large-size foam products by using hot pressing technology, and at the same time, α-BPDA is mainly used to cause high production components, and because it is a closed-cell foam, it also makes it difficult to remove the solvent.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031]1) Mix 70g of 2,3,3`,4`-biphenyltetracarboxylic dianhydride, 30g of methanol, 7g of AK-6602 and 8 parts of DC-5103 and stir evenly to obtain precursor A material, the stirring speed is 535r / min , the stirring time is 30min; mix 1.2g N,N-dimethylethanolamine, 0.8g triethylenediamine, 1.5g dibutyltin dilaurate, 2.3g n-pentane, 3.7g HFC-245fa and stir evenly to obtain Precursor B, the stirring rate is 480r / min, and the stirring time is 50min;

[0032] 2) Mix precursor A and material B in step 1), and continue stirring for 45 minutes at a stirring rate of 600r / min to obtain a foaming white material;

[0033] 3) Mix 35g polymethylene polyphenyl isocyanate, 35g methylcyclohexyl diisocyanate, 4.2g dimethyl ethyl phosphonate, 5.8g Fyrol A117S, 10g AK-6602 at a stirring rate of 719r / min Stir for 1.5h to obtain foaming black material;

[0034] 4) Mix the foaming white material and the foaming black material at a ratio of 1:0.65, stir for 18s at a stirring rate of 1300r / min, pour...

Embodiment 2

[0036] 1) 35g 2,2`-dimethyl-3,3`,4,4`-benzophenone tetracarboxylic dianhydride, 35g 3,3`,4,4`-benzophenone tetracarboxylic acid di Anhydride, 20g propanol, 10g methanol, 10gDC-193 and 6gAK-8805 were mixed and mechanically stirred to obtain precursor A material, the stirring speed was 719r / min, and the stirring time was 45min; 1.5g triethanolamine, 0.7g N-ethyl Morpholine, 1.8g stannous octoate, 3.6g HCFC-141b, 1.6g n-pentane were mixed and stirred evenly to obtain precursor B, the stirring speed was 800r / min, and the stirring time was 25min;

[0037] 2) Mix precursor A and material B in step 1), and continue stirring for 30 minutes at a stirring rate of 860r / min to obtain a foaming white material;

[0038] 3) Mix 40g of isophorone diisocyanate, 42g of hexamethylene diisocyanate, 5.1g of dimethyl methylphosphonate, 3.5g of Fyrol A117, 12g of AK-8805, and stir at a stirring rate of 824r / min for 1.0 h obtains foaming black material;

[0039] 4) Mix the foaming white material an...

Embodiment 3

[0041] 1) Mix 25g of 3,3`,4,4`-diphenyl ether tetraanhydride, 50g of pyromellitic anhydride, 18g of methanol, 21g of ethylene glycol, 12g of DC5098 and 8g of L-550 to obtain precursor A material , the stirring rate was 400r / min, and the stirring time was 1.5h; 1.2g diethylenetriamine, 0.4g N,N-dimethylbutylamine, 0.8g bis(dimethylaminoethyl)ether, 1.3g Stannous octoate, 0.8g potassium acetate, 2.0g isopentane, 1.5g HFC-134a, 1.8g water were mixed and stirred evenly to obtain precursor B, the stirring speed was 910r / min, and the stirring time was 22min;

[0042] 2) Mix precursor A and material B in step 1), and continue stirring for 30 minutes at a stirring rate of 1000 r / min to obtain a foaming white material;

[0043] 3) Mix 32g p-phenylene diisocyanate, 62g4,4'-diphenylmethane diisocyanate, 5.8g tetrakis(2-chloroethyl) diethylene ether diphosphate, 4.2g Antiblaze78, 15g JY-6404, Stir at a stirring rate of 1020r / min for 1.5h to obtain a foaming black material;

[0044] 4) M...

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PUM

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Abstract

The invention belongs to the technical field of high polymer materials, and relates to a preparation method of a high-density hard flame-retardant polyimide foam material. The preparation method comprises the following steps of: 1) uniformly mixing anhydride, low-molecular-weight alcohol and a surfactant I to obtain a precursor A material; uniformly mixing a catalyst and a foaming agent to obtaina precursor B; 2) mixing and stirring the precursor A and the precursor B to obtain a foaming white material; 3) mixing and stirring isocyanate, a flame retardant and a surfactant II to obtain a foamed black material; 4) mixing a foamed white material and the foamed black material in proportion, stirring the mixture at a high speed, pouring the mixture into a plastic mold, making the mixture standstill, carrying out microwave curing treatment on the product and the mold to obtain a foamed precursor, taking out the foamed precursor from the mold, and curing and shaping the foamed precursor inan oven to obtain a final foam material; According to the high-density hard flame-retardant polyimide foam material and the preparation method, organic solvent is used; and the prepared polyimide foammaterial has the characteristics of high density and tensile strength and excellent flame retardancy.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a preparation method of a high-density rigid flame-retardant polyimide foam material. Background technique [0002] Polyimide foam refers to a type of polymer foam material containing imide rings in its molecular structure. Due to the particularity of its molecular structure and cell structure, it has good flame retardant properties, thermal insulation properties, Sound absorption and noise reduction performance, high and low temperature resistance, mechanical properties, physical and chemical stability, water resistance, hygienic safety, etc. It has broad application prospects in aerospace, ships, petrochemical pipelines, construction, automobiles and rail transit. [0003] At present, the preparation technology of high-end polyimide foam materials is mainly in the hands of some companies in industrialized countries such as Europe and the United States. Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J9/14C08L79/08C08K5/5333C08K5/521C08G73/10
CPCC08J9/141C08J9/144C08J9/0038C08G73/1021C08G73/1035C08G73/1042C08G73/1039C08J2379/08C08J2203/142C08J2203/14C08J2203/182C08J2205/10Y02P20/10
Inventor 丁泽柴鲜花卢小莲张苏鹏杨大磊史建超刘方辉
Owner GUIZHOU AEROSPACE TIANMA ELECTRICAL TECH
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