CN115449121A - Polypyrrole-coated polyimide hybrid aerogel/phase change material composite film with infrared/electromagnetic double stealth and preparation method thereof - Google Patents

Polypyrrole-coated polyimide hybrid aerogel/phase change material composite film with infrared/electromagnetic double stealth and preparation method thereof Download PDF

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CN115449121A
CN115449121A CN202211279261.2A CN202211279261A CN115449121A CN 115449121 A CN115449121 A CN 115449121A CN 202211279261 A CN202211279261 A CN 202211279261A CN 115449121 A CN115449121 A CN 115449121A
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hybrid aerogel
change material
polyimide hybrid
polypyrrole
phase
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CN115449121B (en
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汪晓东
史涛
刘欢
敬建伟
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Beijing University of Chemical Technology
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    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0066—Use of inorganic compounding ingredients
    • C08J9/0071—Nanosized fillers, i.e. having at least one dimension below 100 nanometers
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    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/36—After-treatment
    • C08J9/365—Coating
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J9/36—After-treatment
    • C08J9/40—Impregnation
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F41—WEAPONS
    • F41H—ARMOUR; ARMOURED TURRETS; ARMOURED OR ARMED VEHICLES; MEANS OF ATTACK OR DEFENCE, e.g. CAMOUFLAGE, IN GENERAL
    • F41H3/00—Camouflage, i.e. means or methods for concealment or disguise
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    • C08J2201/00—Foams characterised by the foaming process
    • C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
    • C08J2201/048—Elimination of a frozen liquid phase
    • C08J2201/0484—Elimination of a frozen liquid phase the liquid phase being aqueous
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    • C08J2205/00—Foams characterised by their properties
    • C08J2205/02—Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
    • C08J2205/026—Aerogel, i.e. a supercritically dried gel
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    • C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
    • C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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    • C08J2479/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2461/00 - C08J2477/00
    • C08J2479/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C—CHEMISTRY; METALLURGY
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    • C08J2487/00—Characterised by the use of unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
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    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/14—Thermal energy storage

Abstract

The invention discloses a polypyrrole-coated polyimide hybrid aerogel/phase-change material composite film with infrared/electromagnetic double stealth and a preparation method thereof. The composite membrane takes a phase-change material as a core material, a polyimide hybrid aerogel membrane as a porous framework and polypyrrole as a coating layer, the polyimide hybrid aerogel is synthesized by taking polyamic acid salt as a matrix and taking a metal organic framework material and a carbon material as a doping filler, the latent heat capacity of the composite membrane exceeds 150J/g, and effective thermal buffering and thermal isolation can be realized on a target object. The preparation method of the composite membrane comprises the following steps: polymerizing, hybridizing, freeze drying, thermal imidizing to obtain polyimide hybrid aerogel film, impregnating and surface spraying. The flexible composite membrane prepared by the invention is foldable, adjustable in shape, good in dynamic temperature regulation and control capability and microwave absorption performance, and capable of realizing infrared and electromagnetic double-stealth function effects.

Description

Polypyrrole-coated polyimide hybrid aerogel/phase change material composite film with infrared/electromagnetic double stealth and preparation method thereof
Technical Field
The invention relates to the technical field of novel military equipment and electronic devices, in particular to a polyimide hybrid aerogel/phase-change material composite film with infrared/electromagnetic double stealth and a preparation method thereof.
Background
With the rapid development of advanced composite detection technology, the multi-physical field stealth technology has received extensive attention. Currently, radar detection and infrared detection are two mainstream detection technologies. In most cases, the two detection technologies need to be used simultaneously in military practice, so that the stealth material compatible with the infrared and electromagnetic integration technology can be developed to effectively reduce the probability of detecting a military target and better realize the electromagnetic and infrared double stealth functions.
The infrared stealth material has the characteristics of high reflectivity and low absorption, and the total radiant heat energy of a unit surface area of a radiant target is in direct proportion to the fourth power of all wavelength emissivity and temperature according to the Stefan-Boltzmann law. In order to reduce the infrared characteristics of the target object, on one hand, infrared stealth can be achieved by reducing the thermal emissivity; on the other hand, controlling the target surface temperature through heat flow control and heat blocking is another effective means to achieve thermal infrared stealth and thermal camouflage.
However, radar stealth materials generally have the characteristics of low reflectivity and high absorption, and most of the traditional electromagnetic wave absorption materials cannot meet the requirements of light weight, thin matching thickness, effective absorption bandwidth and strong absorption capacity. Therefore, how to effectively absorb electromagnetic radiation, meet the requirements of electromagnetic wave absorption materials, and reduce detected infrared signals while realizing electromagnetic stealth, which has important research significance for military stealth and electromagnetic stealth application fields.
Aerogel and its hybrid materials are considered as ideal heat insulation and promising infrared stealth materials due to their unique porous properties. At present, polyimide aerogel has great application potential in the aspects of infrared stealth and thermal camouflage, and research can form a composite/hybrid state by introducing various inorganic nano-sized fillers so as to improve the heat insulation stealth effect of the polyimide aerogel. Furthermore, in recent years, phase change materials have received much attention in infrared stealth and thermal camouflage applications by virtue of their ability to modulate infrared emissions through passive thermal management. In addition, the phase change material is a latent heat storage material, can store and release a large amount of heat energy through reversible phase change in a physical state at almost constant temperature, has a simple and reliable structure and a wide phase change temperature selection range, can efficiently and economically store and regulate heat energy, and has a wide application prospect in an energy management system. Therefore, the phase change material is expected to adjust the target thermal emissivity through controllable latent heat absorption and release in the phase change temperature process of different backgrounds, and good infrared stealth performance is realized.
Therefore, how to effectively realize infrared/electromagnetic stealth by compounding the aerogel, the hybrid material thereof and the phase-change material and meet the requirements of light weight, thin matching thickness, effective absorption bandwidth and strong absorption capacity of the material are the current research hotspots and difficulties.
Disclosure of Invention
Aiming at the prior art, the invention aims to provide a polypyrrole-coated polyimide hybrid aerogel/phase-change material composite film with infrared/electromagnetic double stealth and a preparation method thereof.
In order to realize the purpose, the invention adopts the following technical scheme:
in a first aspect of the invention, a polypyrrole coated polyimide hybrid aerogel/phase change material composite film is provided.
The polypyrrole-coated polyimide hybrid aerogel/phase-change material composite membrane takes a phase-change material as a core material, a polyimide hybrid aerogel membrane as a porous framework, and polypyrrole as a coating layer.
Preferably, the polyimide hybrid aerogel has a porosity of 95% or more and a tensile strength of 0.5 to 3.0MPa.
More preferably, the polyimide hybrid aerogel has a porosity of 98% or more and a tensile strength of 1.0-2.5MPa
Preferably, the polyimide hybrid aerogel is synthesized by taking polyamic acid salt as a matrix and taking a metal organic framework material and a carbon material as a doping filler.
Preferably, the metal organic framework material is UiO series.
Preferably, the carbon material is one or more of graphene, carbon nanotubes and a new transition metal carbon-containing material MXene.
Preferably, the phase change material is one or more of polyethylene glycol, fatty acid and sugar alcohol.
Preferably, the thickness of the polypyrrole coated polyimide hybrid aerogel/phase change material composite film is 50-1000 μm.
Further preferably, the thickness of the polypyrrole coated polyimide hybrid aerogel/phase change material composite membrane is 400-800 μm.
In a second aspect of the present invention, a preparation method of a polypyrrole coated polyimide hybrid aerogel/phase change material composite membrane is provided, which comprises the following steps:
(1) Adding dibasic acid anhydride, diamine and an aminated metal-organic framework material into an organic solvent, performing polycondensation reaction to obtain a polyamic acid solution containing metal-organic framework material hybridization, adding organic base into the polyamic acid solution containing metal-organic framework material hybridization, separating out a solid in an acetone solvent, filtering and drying to obtain a polyamic acid salt solid containing metal-organic framework material hybridization;
(2) Adding the polyamic acid salt solid hybridized by the metal organic framework material into a dispersion solution containing organic alkali, stirring, adding a carbon material, after stirring, carrying out freeze drying and thermal imidization treatment to obtain a polyimide hybrid aerogel membrane;
(3) Soaking the polyimide hybrid aerogel film into the molten phase-change material to obtain a polyimide hybrid aerogel/phase-change material composite film;
(4) And spraying the pyrrole solution on the surface of the polyimide hybrid aerogel/phase-change material composite membrane, and oxidizing by using an oxidant to prepare the polypyrrole-coated polyimide hybrid aerogel/phase-change material composite membrane.
Preferably, in step (1), the dibasic acid anhydride is one or more of pyromellitic dianhydride, biphenyltetracarboxylic dianhydride and benzophenone tetracarboxylic dianhydride.
Preferably, in the step (1), the diamine is one or more of diaminodiphenyl ether, 4' diaminodiphenylmethane and p-phenylenediamine.
Preferably, in step (1), the metal organic framework material is in the UiO series.
Preferably, in the step (1), the mass ratio of the dibasic acid anhydride to the diamine is (1.00-1.02): 1.
More preferably, in the step (1), the mass ratio of the dibasic acid anhydride to the diamine is 1.01.
Preferably, in the step (1), the mass ratio of the total mass of the dibasic acid anhydride and the diamine to the mass of the aminated organometallic framework is 100: (1-5).
Preferably, in the step (1), the organic solvent is one or more of N, N-dimethylacetamide, N-dimethylformamide and N-methylpyrrolidone.
Preferably, in the step (1), the solid content of the polyamic acid in the polyamic acid solution hybridized by the metal-organic framework material is 10-30wt%.
Preferably, in the step (1), the organic base is one of triethanolamine, triethylamine and tripropylamine.
Preferably, in the step (1), the amount of the organic base is 2 to 4 times of the amount of the polyamic acid end-COOH substance hybridized by the metal-organic framework material.
Further preferably, in the step (1), the amount of the organic base is 1.5 to 3 times of the amount of the polyamic acid terminal-COOH substance hybridized by the metal-organic framework material.
Preferably, in the step (2), the organic base is one of triethanolamine, triethylamine and tripropylamine.
Preferably, in the step (2), the dispersant of the dispersion solution containing the organic base is deionized water or tert-butyl alcohol.
Preferably, in the step (2), the content of the metal-organic framework material hybrid polyamic acid salt solid in the organic base dispersion solution is 1-10wt%.
Further preferably, in the step (2), the content of the metal-organic framework material hybridized polyamic acid salt solid in the organic base dispersion solution is 4-8wt%.
Preferably, in the step (2), the mass ratio of the metal-organic framework material hybridized polyamic acid salt solid to the carbon material is 100: (1-10).
Preferably, the carbon material is one or more of graphene, carbon nanotubes and a new transition metal carbon-containing material MXene.
Further preferably, the mass ratio of the metal-organic framework material hybridized polyamic acid salt solid to the carbon material is 100: (5-8).
Preferably, in the step (2), the freezing method is one of unidirectional freezing, bidirectional freezing and random freezing.
Preferably, in the step (2), the freeze-drying temperature is-70 to-80 ℃, and the vacuum pressure is 0.5 to 5Pa.
Preferably, in the step (2), the freeze-drying time is 8-16h.
Preferably, in the step (2), the temperature increase condition of the thermal imidization treatment is: keeping the temperature for 1h at 0-150 ℃; keeping the temperature at 150-300 ℃ for 2h, wherein the heating rate is 1.25 ℃/min.
Preferably, in the step (2), the environment required for thermal imidization is nitrogen or argon.
Preferably, in step (3), the phase change material is one or more of polyethylene glycol, fatty acid and sugar alcohol.
Preferably, in the step (4), the oxidizing agent is one or two of ferric trichloride solution and ammonium persulfate solution.
Preferably, in the step (4), the mass ratio of the pyrrole solution to the oxidant is 1: (2-4).
Preferably, in the step (4), the dosage of the pyrrole solution is 5-10mL.
The third aspect of the invention provides application of a polypyrrole-coated polyimide hybrid aerogel/phase-change material composite film in preparation of an electromagnetic and infrared double-stealth material.
The invention has the beneficial effects that:
the polyimide hybrid aerogel membrane prepared by the technology of compounding organic components and inorganic components and freeze drying has good flexibility, the polypyrrole-coated polyimide hybrid aerogel/phase-change material composite membrane is obtained by the vacuum impregnation method and the spraying technology, the preparation process is simple, the raw materials are easy to obtain, and the polypyrrole-coated polyimide hybrid aerogel/phase-change material composite membrane is suitable for expanded production.
The flexible polypyrrole coated polyimide hybrid aerogel/phase change material composite film prepared by the invention is flexible and foldable, has good mechanical property, fatigue resistance, excellent thermal regulation capability and thermal cycle stability, can realize temperature regulation and control due to good thermal management capability, has higher thermal shock performance and good thermal cycle stability, and can meet the long-term use requirements of stealth and electromagnetic double-stealth applications.
The invention can reduce the surface temperature of the target by utilizing the thermal regulation capability of the phase-change material, thereby effectively inhibiting the infrared radiation of the target and meeting the requirements of the target on high-efficiency infrared stealth and thermal camouflage application. Meanwhile, the carbon material and the electric loss type wave-absorbing material polypyrrole are combined, so that the electromagnetic loss can be enhanced, the impedance matching characteristic of the material can be improved, the magnetic energy dissipation capacity and the electromagnetic microwave absorption capacity can be enhanced, and the electromagnetic stealth effect can be further realized.
Because polyimide aerogel membrane has low heat conduction and three-dimensional porous structure's thermal-insulated effect, the heat-conduction of solid phase has been reduced, thereby realize the static regulation and control to high temperature target surface temperature, in addition, metal organic frame material, the inside light and heat conversion of carbon material all can reinforcing aerogel, the quick thermal response of phase change material on the heat source of effectual promotion load in the aerogel, absorb for the system provides the thermal cushion through phase change process latent heat, reduce surface temperature more effectively, the quilt detection time has been delayed, the stealthy effect is realized to dynamic control object surface temperature. Therefore, the polypyrrole-coated polyimide hybrid aerogel/phase change material composite film can effectively realize infrared stealth and thermal camouflage of a target in a wide temperature range.
The effective bandwidth (R) of the polypyrrole-coated polyimide hybrid aerogel/phase-change material composite membrane prepared by the invention L < -10 dB) covers the whole X-band and the minimum reflection loss peak can reach-56.8 dB, which is very attractive to military radars and direct broadcast satellites. Further, the prepared polypyrrole-coated polyimide hybrid aerogel/phase change material composite film has a relatively wide broadband absorption capacity, and the carbon material and the polypyrrole material have a synergistic enhancement effect, so that the electromagnetic wave absorption capacity is improved, electromagnetic stealth of a target in a wide temperature range and a wide electromagnetic frequency band range is realized, and the polypyrrole-coated polyimide hybrid aerogel/phase change material composite film is applicable to an electromagnetic stealth application scene.
Therefore, the polypyrrole coated polyimide hybrid aerogel/phase change material composite film with the infrared/electromagnetic double stealth function provides a new strategy for designing and developing a high-performance and light-weight infrared/electromagnetic double-function stealth material, and further has a wide application prospect.
The polypyrrole-coated polyimide hybrid aerogel/phase change material composite film prepared by the invention has a relatively wide broadband absorption capacity, the carbon material and the resistance loss type material have a synergistic enhancement effect, the electromagnetic wave absorption capacity is improved, the electromagnetic stealth of a target in a wide temperature and wide electromagnetic frequency band range is realized, and the polypyrrole-coated polyimide hybrid aerogel/phase change material composite film is suitable for an electromagnetic stealth application scene.
Drawings
FIG. 1: scanning electron micrographs of (a) the polyimide hybrid aerogel membrane of example 3, (b) the polyimide hybrid aerogel/phase change material composite membrane of example 3, and (c) the polypyrrole-coated polyimide hybrid aerogel/phase change material composite membrane of example 3;
FIG. 2 is a schematic diagram: differential scanning calorimetry of the polypyrrole coated polyimide hybrid aerogel/phase change material composite film in example 3;
FIG. 3: a thermal infrared imaging contrast plot of the polypyrrole coated polyimide aerogel/phase change material composite films of example 3 versus the composite films of comparative examples 1-3;
FIG. 4: a graph comparing the electromagnetic microwave absorption capacity of the polypyrrole-coated polyimide aerogel/phase change material composite film of example 3 with the composite films of comparative examples 1 to 3;
FIG. 5: comparative graphs of electromagnetic microwave absorption capacity of the polypyrrole-coated polyimide aerogel/phase change material composite films of examples 3 to 7.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
In order to make the technical solutions of the present application more clearly understood by those skilled in the art, the technical solutions of the present application will be described in detail below with reference to specific embodiments.
The test materials used in the examples of the present invention are all conventional in the art and commercially available.
Example 1
(1) 5.49g of p-phenylenediamine and 0.39g of UiO-66-NH were weighed out 2 Adding 50.0mL of N-methyl pyrrolidone solvent into the particles, stirring for 30min, adding 16.5g of benzophenone tetracarboxylic dianhydride in batches, vigorously stirring in an ice-water bath for 3h to obtain a metal organic framework material hybridized polyamic acid solution, wherein the solid content of the polyamic acid in the solution is 30wt%, then slowly dropwise adding 78.1mL of tripropylamine into a flask, stirring for 5h to obtain a metal organic framework hybridized polyamic acid solution, then precipitating in acetone, filtering, washing to obtain a precipitate filament, and finally drying in a 65 ℃ vacuum oven for 24h to obtain the metal organic framework hybridized polyamic acid solid.
Wherein, the amino functional metal organic framework UiO-66-NH 2 The preparation of (1): adding 5.044g of acetic acid and 0.12g of 2-amino terephthalic acid into 30mL of N, N-dimethylformamide solvent, and performing ultrasonic treatment until the acetic acid and the 2-amino terephthalic acid are completely dissolved to form a solution A; then, 0.14g of zirconium chloride is dissolved in 20mL of N, N-dimethylformamide and is subjected to ultrasonic treatment to form a solution B, the solution A and the solution B are stirred and mixed, and the mixture is placed into a vacuum drying oven and is heated for 12 hours at the temperature of 120 ℃; finally, the solution with the diluted white precipitate is taken out of the oven and centrifuged for 15min at a rotating speed of 9000r/min in a centrifuge. Finally washing the precipitate by ethanol once, and drying the precipitate in vacuum to obtain UiO-66-NH 2 And (3) granules.
(2) And (2.0) g of metal organic framework hybridized polyamide acid solid is added into the tripropylamine dispersion solution, wherein 1.0mL of tripropylamine and 46.9mL of deionized water are uniformly mixed to obtain the tripropylamine dispersion solution. Adding 0.06g of MXene into the solution, stirring at room temperature for 6h, coating to form a film, performing two-way freeze drying for 8h at the freezing temperature of-70 ℃ and the vacuum pressure of 0.5Pa to obtain a polyimide hybrid aerogel film containing MXene, and performing high-temperature thermal imidization in a nitrogen environment to finally obtain the polyimide hybrid aerogel film.
Wherein the temperature rise conditions of the thermal imidization treatment are as follows: keeping the temperature for 1h at 0-150 ℃; keeping the temperature at 150-300 ℃ for 2h, wherein the heating rate is 1.25 ℃/min.
(3) And (3) immersing the polyimide hybrid aerogel membrane in the step (2) into molten sugar alcohol in a vacuum oven at 180 ℃ for 8 hours to obtain the polyimide hybrid aerogel/phase-change material composite membrane.
(4) 13.7g of ammonium persulfate and 5.68g of ferric trichloride are weighed and dissolved in 100mL of distilled water, and the solution is named as solution A; 5mL of pyrrole was added to 50mL of isopropanol and mixed well, designated solution B. And (4) uniformly spraying the A and the B on the surface of the polyimide hybrid aerogel/phase-change material composite membrane prepared in the step (3) to obtain the polypyrrole coated polyimide hybrid aerogel/phase-change material composite membrane.
Example 2
(1) 4.74g of 4,4' -diaminodiphenylmethane and 0.39g of UiO-66-NH were taken 2 Adding 50.0ml N, N-dimethylformamide solvent into the granules, stirring for 30min, adding 7.11g biphenyltetracarboxylic dianhydride in batches, and vigorously stirring in ice water bath for 3h to obtain gold-containing granulesThe polyamic acid solution belongs to an organic framework hybrid polyamic acid solution, wherein the solid content of the polyamic acid in the solution is 20wt%, 22.8mL of triethanolamine is slowly dripped into a flask, the solution is stirred for 5 hours to obtain a polyamic acid salt solution hybridized with a metal organic framework material, then the solution is precipitated in acetone, filtered and washed to obtain a precipitate filament, and finally the precipitate filament is dried in a vacuum oven at 65 ℃ for 24 hours to obtain a polyamic acid salt solid hybridized with the metal organic framework.
Wherein, uiO-66-NH 2 The preparation of the granules was carried out as in example 1.
(2) Adding 4.0g of metal organic framework hybridized polyamide acid solid into the dispersion solution of triethanolamine, wherein 1.0mL of triethanolamine and 45.9mL of tert-butyl alcohol are uniformly mixed to obtain the dispersion solution of triethanolamine. Adding 0.24g of carbon nano tube into the solution, stirring for 6h at room temperature, coating to form a film, performing unidirectional freeze drying for 12h at the freezing temperature of-75 ℃ and the vacuum pressure of 2.5Pa to obtain a polyimide hybrid aerogel film containing the carbon nano tube, and performing high-temperature thermal imidization in a nitrogen environment to finally obtain the polyimide hybrid aerogel film.
(3) And (3) immersing the polyimide hybrid aerogel membrane obtained in the step (2) into molten fatty acid in a vacuum oven at the temperature of 80 ℃ for 6 hours to obtain the polyimide hybrid aerogel/phase-change material composite membrane.
(4) 23.26g of ferric chloride is weighed and dissolved in 100mL of distilled water, and the solution is named as solution A; 8mL of pyrrole was added to 50mL of isopropanol and mixed well, designated solution B. And (4) uniformly spraying the A and the B on the surface of the polyimide hybrid aerogel/phase-change material composite membrane prepared in the step (3) to obtain the polypyrrole coated polyimide hybrid aerogel/phase-change material composite membrane.
Example 3
(1) Taking 6.12g of diaminodiphenyl ether and 0.39g of UiO-66-NH 2 Adding 100.0mL of N, N-dimethylacetamide solvent into the particles, stirring for 30min, adding 6.87g of pyromellitic dianhydride in batches, vigorously stirring for 3h in an ice-water bath to obtain a polyamide acid solution containing metal organic framework material hybridization, wherein the solid content of polyamide acid in the solution is 10wt%, then slowly dropwise adding 21.9mL of triethylamine into a flask, stirring for 5h, and then adding waterObtaining polyamic acid salt solution hybridized by the metal organic framework material, precipitating in acetone, filtering, washing to obtain precipitate filaments, and finally drying in a vacuum oven at 65 ℃ for 24h to obtain polyamic acid salt solid hybridized by the metal organic framework.
Wherein, uiO-66-NH 2 The preparation of the granules was carried out as in example 1.
(2) Adding 3.0g of metal organic framework hybridized polyamic acid salt solid into a triethylamine dispersion solution, wherein 1.0mL of triethylamine and 44.9mL of deionized water are uniformly mixed to obtain the triethylamine dispersion solution, adding 0.3g of graphene into the solution, stirring at room temperature for 6h, coating to form a film, randomly freezing and drying for 16h, wherein the freezing temperature is-80 ℃ and the vacuum pressure is 5.0Pa, obtaining a polyimide hybrid aerogel film containing the graphene, and then performing high-temperature thermal imidization in a nitrogen environment to finally obtain the polyimide hybrid aerogel film.
(3) And (3) immersing the polyimide hybrid aerogel membrane obtained in the step (2) into molten polyethylene glycol in a vacuum oven at 100 ℃ for 5 hours to obtain the polyimide hybrid aerogel/phase-change material composite membrane.
(4) 19.4g of ammonium persulfate is weighed and dissolved in 100mL of distilled water, and named as solution A; 10mL of pyrrole was added to 50mL of isopropanol and mixed well, designated solution B. And (4) uniformly spraying the A and the B on the surface of the polyimide hybrid aerogel/phase-change material composite membrane containing the graphene prepared in the step (3) to obtain the polypyrrole coated polyimide hybrid aerogel/phase-change material composite membrane.
The polypyrrole-coated polyimide hybrid aerogel/phase-change material composite film prepared in example 3 was subjected to gold spraying treatment and then characterized by a scanning electron microscope, and the obtained scanning electron microscope photographs are shown in fig. 1 and respectively include (a) a polyimide hybrid aerogel film, (b) a polyimide hybrid aerogel/phase-change material composite film, and (c) a polypyrrole-coated polyimide hybrid aerogel/phase-change material composite film.
Fig. 1 (a) shows that the polyimide hybrid aerogel film has high porosity, uniform pore size and thick pore walls, provides a powerful support frame for filling the phase-change material, and simultaneously shows that graphene sheets can be uniformly dispersed on the pore walls. Fig. 1 (b) shows that the prepared polyimide hybrid aerogel/phase change material composite membrane is impregnated with sufficient polyethylene glycol, and has no any gap with an aerogel framework, and fig. 1 (c) shows that polypyrrole as a surface coating layer can more effectively inhibit the leakage of the phase change material, thereby ensuring better infrared stealth practical application.
After the polypyrrole coated polyimide hybrid aerogel phase change composite film prepared in example 3 is tested by a differential scanning calorimeter, a heat flow-temperature curve is shown in fig. 2.
Integration is carried out on the curve in figure 2 to obtain that the melting enthalpy and the crystallization enthalpy of the polyimide hybrid aerogel/phase-change material composite membrane are respectively 154.4J/g and 151.8J/g, the composite membrane has good latent heat storage-release performance, and the high heat storage capacity is enough for practical application of infrared stealth and thermal camouflage.
Example 4
The present example is different from example 3 in that the mass of graphene is 0.24g, and other technical details are the same as those of example 3.
Example 5
The present example is different from example 3 in that the mass of graphene is 0.18g, and other technical details are the same as those of example 3.
Example 6
The present example is different from example 3 in that the mass of graphene is 0.12g, and other technical details are the same as those of example 3.
Example 7
The present example is different from example 3 in that the mass of graphene is 0.06g, and other technical details are the same as those of example 3.
Comparative example 1: polypyrrole-coated polyimide aerogel phase-change composite film without graphene
The present example is different from example 3 in that the mass of graphene is 0g, and other technical details are the same as those of example 3.
Comparative example 2: polyimide hybrid aerogel/phase change composite film without added graphene and without polypyrrole coating
(1) Taking 6.12g of diaminodiphenyl ether and 0.39g of UiO-66-NH 2 Adding 100.0mL of N, N-dimethylacetamide solvent into the particles, stirring for 30min, adding 6.87g of pyromellitic dianhydride in batches, vigorously stirring in an ice-water bath for 3h to obtain a polyamide acid solution containing metal organic framework material hybridization, wherein the solid content of polyamide acid in the solution is 10wt%, then slowly dropwise adding 21.9mL of triethylamine into a flask, stirring for 5h to obtain a polyamide acid salt solution containing metal organic framework material hybridization, then precipitating in acetone, filtering, washing to obtain precipitate filaments, and finally drying in a vacuum oven at 65 ℃ for 24h to obtain the polyamide acid solid containing metal organic framework hybridization.
Wherein, uiO-66-NH 2 The preparation of the granules was carried out as in example 1.
(2) Adding 3.0g of metal organic framework hybridized polyamic acid salt solid into a triethylamine dispersion solution, wherein 1.0mL of triethylamine and 44.9mL of deionized water are uniformly mixed to obtain the triethylamine dispersion solution. Stirring at room temperature for 6h, coating to form a film, randomly freezing and drying for 16h at-80 ℃ and under the vacuum pressure of 5.0Pa to obtain the polyimide hybrid aerogel film, and then performing high-temperature thermal imidization in a nitrogen environment to obtain the polyimide hybrid aerogel film.
(3) And (3) immersing the polyimide hybrid aerogel film containing graphene obtained in the step (2) into molten polyethylene glycol in a vacuum oven at 100 ℃ for 5 hours to obtain a target product.
Comparative example 3: polyimide aerogel/phase-change material composite film without graphene, metal organic frame and polypyrrole coating
(1) Adding 6.12g of diaminodiphenyl ether into 100.0mL of N, N-dimethylacetamide solvent, stirring for 30min, adding 6.87g of pyromellitic dianhydride in batches, stirring vigorously in an ice-water bath for 3h to obtain a polyamic acid solution, wherein the solid content of polyamic acid in the solution is 10wt%, slowly dropwise adding 21.9mL of triethylamine into a flask, stirring for 5h to obtain a polyamic acid salt solution hybridized with a metal-organic framework material, precipitating in acetone, filtering, washing to obtain a precipitate filament, and finally drying in a vacuum oven at 65 ℃ for 24h to obtain a polyamic acid salt solid.
(2) 3.0g of polyamic acid salt solid was added to the dispersion solution of triethylamine, wherein 1.0mL of triethylamine and 44.9mL of deionized water were mixed uniformly to obtain the dispersion solution of triethylamine. Stirring for 6h at room temperature, coating to form a film, randomly freezing and drying for 16h at-80 ℃ and under the vacuum pressure of 5.0Pa to obtain a polyimide-containing aerogel film, and then performing high-temperature thermal imidization in a nitrogen environment to finally obtain the polyimide aerogel film.
(3) And (3) immersing the polyimide aerogel film obtained in the step (2) into molten polyethylene glycol in a vacuum oven at 100 ℃ for 5 hours to obtain the polyimide aerogel/phase-change material composite film.
Test example 1:
the polypyrrole-coated polyimide hybrid aerogel/phase change material composite films prepared in examples 1 to 3 were pressed into a ring shape with a standard outer diameter, inner diameter, and thickness to fit a sample holder in an instrument, and electromagnetic parameters of the sample were measured using a transmission/reflection method using a vector network analyzer, and the microwave absorption effect of the sample was determined according to the obtained electromagnetic parameters within a certain range (4 to 18 GHz), as shown in table 1.
TABLE 1 electromagnetic microwave absorption Performance parameters of hybrid aerogel/phase change material composite membranes in examples 1-3
Figure BDA0003897998960000101
The absorption capability of a material for electromagnetic waves is generally expressed in terms of reflection loss (R) L ) Is represented by R L The higher the absolute value, the greater the ability to absorb electromagnetic waves, indicating that 90% of the electromagnetic wave energy can be absorbed when the absolute value is greater than 10 dB.
Figure BDA0003897998960000102
Figure BDA0003897998960000103
In which each represents the meaning: input impedance (Z) in ) Free space impedance (Z) 0 ) Light velocity (c), electromagnetic wave frequency (f), complex dielectric constant (epsilon), complex magnetic permeability (mu) and thickness (d) of the composite film.
As can be seen from table 1, the hybrid aerogel/phase change material composite films in examples 1 to 3 all have a good absorption effect on electromagnetic microwaves, and the hybrid aerogel/phase change material composite film in example 3 has a smaller reflection loss value and a wider effective absorption band than the hybrid aerogel/phase change material composite films in examples 1 and 2, thereby showing a better electromagnetic wave absorption effect.
Test example 2
The polypyrrole-coated polyimide hybrid aerogel phase-change composite film (S1) prepared in example 3, the polypyrrole-coated polyimide hybrid aerogel film (S2) which is not doped with graphene and is prepared in comparative example 1, the undoped graphene and polyimide hybrid aerogel/phase-change material composite film (S3) which is not coated with polypyrrole and is prepared in comparative example 2, the non-doped graphene and non-metal organic frame and the polypyrrole-coated polyimide aerogel/phase-change material composite film (S4) prepared in comparative example 3 are respectively placed on a hot stage at a constant temperature of 90 ℃, and the temperature change process thereof is recorded by using a thermal infrared camera, and the thermal infrared stealth performance test result is shown in fig. 3.
As can be seen from fig. 3, the four samples S1, S2, S3, and S4 showed a distinct color change after 1 minute and 5 minutes of heating, and rapidly changed from blue to yellow. Comparing S1 and S2, the composite film (S1) added with the hybrid filler graphene has slightly faster temperature change response, which shows that the addition of the graphene can enhance certain photothermal conversion capacity, so that the phase change material filled in the composite film can rapidly perform thermal response and phase transition on a heat source, the reaction to the background temperature is slow due to large latent heat adsorption, an additional thermal buffering effect is generated on the composite film, the surface temperature of the composite film is effectively reduced, the detection time of a thermal infrared camera is delayed, and the target and the environmental temperature are fused as far as possible. Comparing S1 with S2, S3 and S4, the temperature change difference value after 5 minutes fluctuates within the range of 2-4 ℃, and the influence of thermal infrared imaging of the composite film coated by the added graphene, the metal organic frame and the polypyrrole is small, so that the composite film has a certain temperature control effect while the better electromagnetic performance is ensured, and the composite film is very favorable for infrared stealth and thermal camouflage of a heat source for infrared detection.
The microwave absorption capacity of the composite membranes prepared in example 3 and comparative examples 1 to 3, which were measured by a vector network analyzer, is shown in fig. 4.
As can be seen from fig. 4, the composite film prepared in example 3 has a smaller minimum reflection loss value and a wider effective absorption frequency band than those of comparative examples 1 to 3, which also illustrates that the composite of the metal organic framework material, the carbon material and the resistive loss material forms multi-level dielectric and electromagnetic dissipation, improves the impedance matching characteristics of the material, enhances the electromagnetic energy dissipation capability, thereby having better microwave absorption capability and more effectively realizing electromagnetic stealth.
Test example 3
The polypyrrole-coated polyimide hybrid aerogel phase-change composite films with different graphene contents prepared in examples 3 to 7 were tested by a vector network analyzer, and the microwave absorption capacity was obtained as shown in fig. 5.
As can be seen from fig. 5, as the content of graphene increases, the minimum reflection loss value becomes smaller, and when the content of example 3 is reached, the minimum reflection loss value can reach-56.8 dB, and the microwave absorption effect is the best.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims (10)

1. The polypyrrole-coated polyimide hybrid aerogel/phase-change material composite membrane is characterized in that the polyimide hybrid aerogel/phase-change material composite membrane takes a phase-change material as a core material, a polyimide hybrid aerogel membrane as a porous framework, and polypyrrole as a surface coating layer;
the polyimide hybrid aerogel is synthesized by taking polyamic acid salt as a matrix and taking a metal organic framework material and a carbon material as a doping filler.
2. The hybrid aerogel/phase change material composite membrane of claim 1, wherein the metal-organic framework material is the UiO series;
the carbon material is one or more of graphene, a carbon nano tube and a transition metal carbon-containing new material MXene;
the phase change material is one or more of polyethylene glycol, fatty acid and sugar alcohol.
3. The preparation method of the polypyrrole coated polyimide hybrid aerogel/phase change material composite film according to claim 1 or 2, comprising the following steps:
(1) Adding dibasic acid anhydride, diamine and aminated metal organic framework material into an organic solvent, performing polycondensation reaction to obtain a metal organic framework material hybridized polyamic acid solution, adding organic base, precipitating solid in an acetone solvent, filtering and drying to obtain metal organic framework material hybridized polyamic acid salt solid;
(2) Adding the polyamic acid salt solid hybridized by the metal organic framework material into a dispersion solution containing organic base, stirring, adding a carbon material, after stirring, carrying out freeze drying and thermal imidization treatment to obtain a polyimide hybrid aerogel membrane;
(3) Soaking the polyimide hybrid aerogel film into the molten phase-change material to obtain a polyimide hybrid aerogel/phase-change material composite film;
(4) And spraying the pyrrole solution on the surface of the polyimide hybrid aerogel/phase-change material composite membrane, and oxidizing by using an oxidant to prepare the polyimide hybrid aerogel/phase-change material composite membrane coated by polypyrrole.
4. The method for preparing the polypyrrole coated polyimide hybrid aerogel/phase change material composite film according to claim 3, wherein in step (1), the dibasic acid anhydride is one or more of pyromellitic dianhydride, biphenyltetracarboxylic dianhydride, and benzophenonetetracarboxylic dianhydride;
the diamine is one or more of diaminodiphenyl ether, 4' -diaminodiphenylmethane and p-phenylenediamine;
the organic solvent is one or more of N, N-dimethylacetamide, N-dimethylformamide and N-methylpyrrolidone.
5. The preparation method of the polypyrrole coated polyimide hybrid aerogel/phase change material composite film according to the claim 3, wherein in the step (1), the ratio of the amounts of the substances of the dibasic acid anhydride and the diamine is (1.00-1.02): 1;
the mass ratio of the total mass of the dibasic acid anhydride and the diamine to the mass of the metal organic framework is 100: (1-5).
6. The preparation method of the polypyrrole coated polyimide hybrid aerogel/phase change material composite film according to the claim 3, wherein in the step (1), the solid content of the polyamic acid in the metal organic framework material hybrid polyamic acid solution is 10-30wt%;
the organic alkali is one or more of triethanolamine, triethylamine and tripropylamine;
the mass ratio of the organic base to the substance of the polyamic acid terminal carboxyl hybridized by the metal organic framework material is (2-4) to 1.
7. The preparation method of the polypyrrole coated polyimide hybrid aerogel/phase change material composite film according to the claim 3, wherein in the step (2), the dispersant of the organic base-containing dispersion solution is deionized water or tert-butyl alcohol;
the content of the metal organic framework material hybridized polyamic acid salt solid in the organic base dispersion solution is 1-10wt%;
the mass ratio of the metal organic framework material hybridized polyamic acid salt solid to the carbon material is 100: (1-10).
8. The method for preparing a polypyrrole coated polyimide hybrid aerogel/phase change material composite film according to claim 3, wherein in step (2), the freezing method is one or more of one-way freezing, two-way freezing and random freezing;
the freeze drying temperature is-70 deg.C to-80 deg.C, the vacuum pressure is 0.5-5Pa, and the freeze drying time is 8-16h;
the temperature rise conditions of the thermal imidization treatment are as follows: keeping the temperature for 1h at 0-150 ℃; keeping the temperature at 150-300 ℃ for 2h, wherein the heating rate is 1.25 ℃/min.
9. The method for preparing the polypyrrole coated polyimide hybrid aerogel/phase change material composite film according to the claim 3, wherein in the step (4), the oxidant is ferric trichloride solution or ammonium persulfate solution;
the mass ratio of the pyrrole solution to the oxidant is (1-4): (3-12).
10. The polypyrrole coated polyimide hybrid aerogel/phase change material composite film of claim 1 or 2 is used for preparing infrared/electromagnetic stealth materials.
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