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Preparation method and product of a density-adjustable flexible polyimide foam

A polyimide and polyimide precursor technology, applied in the field of preparation of flexible polyimide foam with adjustable density, can solve the problems of increasing the complexity of the preparation process, increasing the preparation cycle, and cracking

Active Publication Date: 2022-04-22
HARBIN ENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above methods can improve the density and mechanical strength of the polyimide foam material, these methods all increase processing steps or adopt special equipment and control molds on the basis of the original polyimide foam preparation technology, which will increase The complexity of the preparation process increases the preparation cycle, which is not conducive to the development of polyimide foam. At the same time, a set of process system may only produce foam materials with one density, which is not conducive to the diversification of polyimide foam with a wide density range. preparation of
[0004] At the same time, in the past polyimide foam preparation process, the curing temperature for the transformation of the precursor to polyimide is generally above 200 ° C, which consumes a lot of energy; and the foam molding process and the imidization process need to be separated It is carried out in different microwave and high-temperature oven equipment, which increases the demand for equipment and increases the entire process flow line; the further problem is that the foam intermediate after foaming is taken out from the microwave equipment and transferred to the oven. During the process, it will be exposed to the lower room temperature outside, and the change of temperature difference often easily causes internal cracking, and the brittle foam intermediate is prone to collapse and other problems during the transfer process, resulting in a large number of unqualified products.

Method used

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  • Preparation method and product of a density-adjustable flexible polyimide foam
  • Preparation method and product of a density-adjustable flexible polyimide foam
  • Preparation method and product of a density-adjustable flexible polyimide foam

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Dissolve 161.12g of 3,3',4,4'-benzophenone tetraacid dianhydride in 100g of tetrahydrofuran solvent while stirring at 95°C, then add 182g of methanol for esterification reaction, and cool the solution to 5 ℃ and add 49.58g diaminodiphenylmethane, FSO surfactant 1.8g and 0.3g isoquinoline to react to prepare anhydride group-terminated polyimide precursor solution I; then adjust the reaction temperature to 25 ℃ and Slowly add 63g of polyphenyl polymethylene polyisocyanate to completely react the isocyanate group with the anhydride group and residual acid anhydride in the precursor solution, and cool to room temperature to obtain the polyimide precursor solution II.

[0037] Then use a rotary evaporator to remove most of the polar solvent in the polyimide precursor solution II by rotary evaporation at a vacuum degree of 50kPa and 45°C. The polyimide precursor evaporates during the desolvation process in the rotary evaporation bottle Steep and fill the rotary evaporator. S...

Embodiment 2

[0041] Dissolve 161.12g of 3,3',4,4'-benzophenone tetraacid dianhydride in 170g of tetrahydrofuran solvent while stirring at 100°C, then add 140g of methanol for esterification reaction, and cool the solution to 10 ℃ and add 75g diaminodiphenyl ether, FSO surfactant 2.0g and 1.0g isoquinoline to react to prepare anhydride group-terminated polyimide precursor solution I; then adjust the reaction temperature to 25 ℃ and slowly 31.5 g of diphenylmethane diisocyanate was added to completely react the isocyanate groups with the anhydride groups and residual acid anhydride in the precursor solution, and cooled to room temperature to obtain a polyimide precursor solution II.

[0042] Then use a rotary evaporator to remove most of the polar solvent in the polyimide precursor solution II by rotary evaporation at a vacuum degree of 50kPa and 45°C. The polyimide precursor evaporates during the desolvation process in the rotary evaporation bottle Steep and fill the rotary evaporator. Sub...

Embodiment 3

[0046] Dissolve 148g of 3,3',4,4'-biphenyltetraacid dianhydride in 160g of N,N-dimethylacetamide while stirring at 90°C, then add 120g of methanol for esterification reaction, and the reaction is complete After cooling the solution to 10°C and adding 52g of p-phenylenediamine, 1.0g of FSO surfactant and 0.9g of isoquinoline to react, the polyimide precursor solution I of anhydride group end-capping was obtained; the reaction temperature was adjusted to Slowly add 6.5g of diphenylmethane diisocyanate at 20°C to completely react the isocyanate group with the anhydride group and residual anhydride in the precursor solution, and cool to room temperature to obtain the polyimide precursor solution II.

[0047] Then use a rotary evaporator to remove most of the polar solvent in the polyimide precursor solution II by rotary evaporation at a vacuum degree of 40kPa and 45°C. The polyimide precursor evaporates during the desolvation process in the rotary evaporation bottle Steep and fill...

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Abstract

The invention discloses a preparation method and product of a density-adjustable flexible polyimide foam. The preparation method includes the following steps: (1) firstly prepare an anhydride group-terminated polyimide precursor solution I; then slowly add polyisocyanate Reaction is complete, cooled to room temperature to obtain polyimide precursor solution II; (2) first remove most of the polar solvent in polyimide precursor solution II, and then solidify in a vacuum oven under vacuum conditions to obtain Partially imidized polyimide precursor foam; finally, the foam in the rotary steamer is taken out, and after being pulverized and ground by a planetary ball mill, a fine and uniform partially imidized polyimide precursor is obtained (3) After pressing the polyimide precursor powder into a foaming master, place it in microwave equipment; set the microwave equipment parameters to complete the foaming molding process; then, adjust the microwave equipment parameters to complete the curing get the product. The invention realizes the effective control of the density and strength of the flexible polyimide foam.

Description

technical field [0001] The invention relates to the technical field of polyimide foam preparation, in particular to a preparation method and product of density-adjustable flexible polyimide foam. Background technique [0002] Polyimide foam material is an organic polymer foam material containing imide structure in the molecular main chain. Polyimide foam has excellent thermal stability, flame retardancy, heat preservation and chemical corrosion resistance. It is an ideal thermal insulation, sound absorption and shockproof material in advanced fields such as aerospace and marine ships. material application field. However, different laying locations have certain requirements for the density and strength of the thermal insulation material, and the special sound absorption frequency band and thermal insulation performance of polyimide foams with different densities are quite different. Therefore, how to prepare polyimide foam materials with different densities and strengths, r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/10C08J9/00C08L79/08
CPCC08G73/1067C08G73/1071C08G73/1007C08G73/1035C08G73/1003C08J9/00C08J2379/08
Inventor 孙高辉段天娇韩世辉陈蓉蓉王君
Owner HARBIN ENG UNIV
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