CN107903394A - The synthetic method of high polymer/graphene@magnetic nano-particle foamed composites - Google Patents

The synthetic method of high polymer/graphene@magnetic nano-particle foamed composites Download PDF

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CN107903394A
CN107903394A CN201711140252.4A CN201711140252A CN107903394A CN 107903394 A CN107903394 A CN 107903394A CN 201711140252 A CN201711140252 A CN 201711140252A CN 107903394 A CN107903394 A CN 107903394A
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graphene
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high polymer
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CN107903394B (en
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江智渊
赵慧
郑兰荪
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Xiamen University
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    • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
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Abstract

The synthetic method of high polymer/graphene@magnetic nano-particle foamed composites, is related to polyimides.1) graphene solution is prepared；2) diaminodiphenyl ether powder is added in the graphene solution of step 1) preparation and mixed, obtain solution A；3) pyromellitic acid anhydride powder is added in the mixed solution A of step 2) preparation and be condensed, obtain solution B；4) magnetic nano-particle is added in the solution B that step 3) obtains, stirs, obtains solution C；5) solution C for obtaining step 4) is poured on tablet, then is placed on using water in the flocculation basin of flocculant, to be dried after flocculation；The material of gained is structurally characterized in that the high polymer with obvious foaming structure/graphene magnetic nano-particle composite material, and the property of comparative superiority is shown in electro-magnetic wave absorption.Easy to operate, workable, favorable reproducibility, yield is up to 95%.

Description

The synthetic method of high polymer/graphene@magnetic nano-particle foamed composites
Technical field
The present invention relates to polyimides, more particularly, to high polymer/graphene@magnetic nano-particle foamed composites Synthetic method.
Background technology
Polyimides has excellent mechanical performance, some polyimides kinds do not dissolve in organic solvent, and diluted acid is stablized Polyimides has very high radiation-resistant property, and polyimides is self-extinguishing polymer, and smoke rate is low.Polyimides is as a kind of Special engineered material, has been widely used in fields such as Aeronautics and Astronautics, microelectronics, nanometer, liquid crystal, seperation film, laser.Polyamides is sub- Amine, because of its outstanding feature in terms of performance and synthesis, either as structural material or as functional material, its is huge Application prospect sufficiently recognized, be known as " expert solved the problems, such as ", and think " without polyimides just not Have the microelectric technique of today ".Polyimides high polymer has been studied with this foaming structure that graphene is formed.(Y.Li, X.L.pei, B.shen, W.T.zhai, L.H.zhang, RSC ADV.5 (2015) 24342-24351) however, at present for poly- Few, while this structure of foaming structure research that acid imide high polymer/graphene is compounded to form with magnetic nano-particle Composite material has good electric conductivity and high saturation and magnetic intensity, has good application space in terms of electro-magnetic wave absorption, has Wide application space.
The content of the invention
Relatively simple it is an object of the invention to provide processing step, foaming structure synthesizes more homogeneous and high polymer/stone The synthetic method of black alkene@magnetic nano-particle foamed composites.
The present invention comprises the following steps：
1) graphene solution is prepared；
In step 1), the specific method for preparing graphene solution can be：Graphene is added to N, N- dimethyl In formamide solution, ultrasonic mixing, obtains graphene solution.
2) diaminodiphenyl ether (ODA) powder is added in the graphene solution of step 1) preparation and mixed, obtain solution A；
3) pyromellitic acid anhydride (PMDA) powder is added in the mixed solution A of step 2) preparation and be condensed, obtain solution B；
It is described to add pyromellitic acid anhydride (PMDA) powder in mixed solution A prepared by step 2) in step 3) Condensation, will can add in the solution prepared in step 2) with the PMDA powder of diaminodiphenyl ether (ODA) equimolar amounts.
4) magnetic nano-particle is added in the solution B that step 3) obtains, stirs, obtains solution C；
In step 4), the magnetic nano-particle may be selected from one kind in metal, metal oxide, alloy etc..
5) solution C for obtaining step 4) is poured on tablet, then is placed on using water as in the flocculation basin of flocculant, after flocculation Drying；
In step 5), the tablet can use glass plate etc.；The temperature of the drying can be 60 DEG C.
The material of gained of the invention is structurally characterized in that the high polymer with obvious foaming structure/graphene@magnetic Nanos Particle (metal, metal oxide, alloy) composite material, and show in electro-magnetic wave absorption the property of comparative superiority.
The present invention's has the prominent advantages that：
1) novel high polymer/graphene magnetic nano-particle (metal, metal oxidation is prepared using solution polycondensation Thing, alloy) foamed composite, this material has potential application prospect on microwave absorption；
2) present invention is easy to operate, and workable, favorable reproducibility, yield is up to 95%.
3) present invention can be prepared on a large scale, realize commercialization, in practical applications with potential application value.
4) high temperature resistant of the present invention, has potential application value in terms of aerospace.
Brief description of the drawings
Fig. 1 is scanning electron microscope (SEM) figure of high polymer/graphene of foaming structure.
Fig. 2 is the infrared spectrum of high polymer/graphene of foaming structure.
Fig. 3 is high polymer/graphene@Fe of the foaming structure under small multiple3O4Scanning electron microscope (SEM) figure.
Fig. 4 is high polymer/graphene@Fe of the foaming structure under amplification factor3O4Scanning electron microscope (SEM) figure.
Fig. 5 is high polymer/graphene@Fe of foaming structure3O4Corresponding X-ray powder diffraction figure.
Fig. 6 is high polymer/graphene@Fe of foaming structure3O4The microwave absorption curve of corresponding different-thickness.In Fig. 6 In, test frequency scope is in 2~18GHz.
Fig. 7 is scanning electron microscope (SEM) figure of high polymer/graphene@FeCoNi of foaming structure.
Fig. 8 is high polymer/corresponding X-ray powder diffraction figures of graphene@FeCoNi of foaming structure.
Fig. 9 is that high polymer/graphene@FeCoNi of foaming structure correspond to the microwave absorption curve of different-thickness.In Fig. 9 In, test frequency scope is in 2~18GHz.
The high polymer for foaming structure/graphene@Co scanning electron microscope (SEM) figure corresponding to Figure 10.
The high polymer for foaming structure/graphene@Co ray powder diffraction patterns corresponding to Figure 11.
Embodiment
Below by embodiment combination attached drawing, the invention will be further described.
Embodiment 1
(1) in the round-bottomed flask of 100~250ml, a certain amount of redox graphene is added, measures certain volume N, N- diformazan based solvent, ultrasonic 1.5h, weighs the ODA and PMDA for adding equimolar amounts, mechanic whirl-nett reaction 8h, what is obtained is molten Liquid is poured on clean glass plate, is placed it in using water as the general 12h that in the flocculation basin of flocculant, flocculates, is placed on 60 DEG C 12h in baking oven.
(2) in the round-bottomed flask of 100-250ml, a certain amount of redox graphene is added, measures certain volume N, N- diformazan based solvent, ultrasonic 1h, weighs the ODA and PMDA for adding equimolar amounts, mechanical agitation 5h, adds a certain amount of afterwards Metal oxide is (with Fe3O4Exemplified by), continue to stir 3h, obtained solution is poured on clean glass plate, places it in Yi Shui For the general 10h that in the flocculation basin of flocculant, flocculates, 16h in 60 DEG C of baking oven is placed on.
As seen from Figure 1 with a process for preparing foaming structure.The present invention prepares polyimides as seen from Figure 2 This high polymer of acid.High polymer/graphene and magnetic metal (metal oxide, conjunction are prepared for it can be seen from Fig. 3 and Fig. 4 Gold) etc. nano-particle foaming structure.X-ray powder diffraction figure in Fig. 5 can be seen that：18.3 ° of angle of diffraction, 30.1 °, 35.5 °, 37.1 °, 43.1 °, 53.5 °, 56.9 °, 62.6 °, 70.9 ° with the Fe of body-centered cubic structure3O4:PDF#65-3107's (111), (220) are corresponding with (311), (222), (400), (422), (511), (440), (620) crystal face, and do not send out The appearance of existing other impurity peaks.Fig. 6 is the simulation drawing of microwave absorption, it can be seen that, is inhaling wave plate layer thickness according to analogue data For 2mm, less than -10dB absorption band scopes, reach the absorption broadening of 2.4GHz.
Embodiment 2
(1) in the round-bottomed flask of 100~250ml, a certain amount of redox graphene is added, measures certain volume N, N- diformazan based solvent, ultrasonic 2h, weighs the ODA and PMDA for adding equimolar amounts, mechanical agitation 7h, adds a certain amount of afterwards Metal alloy (by taking FeCoNi as an example), continues to stir 5h, obtained solution is poured on clean glass plate, places it in Yi Shui For the general 12h that in the flocculation basin of flocculant, flocculates, 12h in 60 DEG C of baking oven is placed on.
As seen from Figure 7, high polymer/graphene and magnetic nano-particle (metal, alloy, metal oxide) are prepared for Foaming structure.X-ray powder diffraction figure in Fig. 8 can be seen that：44.5 °, 51.8 °, 76.7 °, 92.7 ° of angle of diffraction and body-centered (111), (200) of the FeCoNi of cubic structure are corresponding with (220), (222), (311), crystal face, and are not found it The appearance of its impurity peaks.Fig. 9 is the simulation drawing of microwave absorption, it can be seen that, is inhaling wave plate layer thickness according to analogue data 2.5mm, less than -10dB absorption band scopes, reaches the absorption broadening of 5.9GHz.
Embodiment 3
(1) in the round-bottomed flask of 100~250ml, a certain amount of redox graphene is added, measures certain volume N, N- diformazan based solvent, ultrasonic 0.5h, weighs the ODA and PMDA for adding equimolar amounts, mechanical agitation 10h, adds afterwards certain The metal (by taking Co as an example) of amount, continues to stir 5h, and obtained solution is poured on clean glass plate, places it in using water as wadding In the flocculation basin of solidifying agent, flocculate general 10h, is placed on 18h in 60 DEG C of baking oven
As seen from Figure 10, high polymer@graphenes and magnetic metal alloy nanoparticles foaming structure are prepared for.Figure 11 X-ray powder diffraction figure can be seen that：41.7 ° of angle of diffraction, 44.8 °, 47.6 °, 75.9 ° with the metal Co of hexagonal structure: (100) of PDF#05-0727, (002), (101), (110) crystal face are corresponding, and are not found going out for other impurity peaks It is existing.

Claims (6)

1. the synthetic method of high polymer/graphene@magnetic nano-particle foamed composites, it is characterised in that including following step Suddenly：
1) graphene solution is prepared；
2) diaminodiphenyl ether (ODA) powder is added in the graphene solution of step 1) preparation and mixed, obtain solution A；
3) pyromellitic acid anhydride (PMDA) powder is added in the mixed solution A of step 2) preparation and be condensed, obtain solution B；
4) magnetic nano-particle is added in the solution B that step 3) obtains, stirs, obtains solution C；
5) solution C for obtaining step 4) is poured on tablet, then is placed on using water in the flocculation basin of flocculant, to be dried after flocculation It is dry.
2. the synthetic method of high polymer as claimed in claim 1/graphene@magnetic nano-particle foamed composites, its feature Be in step 1), it is described prepare graphene solution specific method be：Graphene is added to N,N-dimethylformamide In solution, ultrasonic mixing, obtains graphene solution.
3. the synthetic method of high polymer as claimed in claim 1/graphene@magnetic nano-particle foamed composites, its feature Be in step 3), it is described will pyromellitic acid anhydride powder add step 2) prepare mixed solution A in be condensed, be by with The PMDA powder of diaminodiphenyl ether equimolar amounts is added in the solution prepared in step 2).
4. the synthetic method of high polymer as claimed in claim 1/graphene@magnetic nano-particle foamed composites, its feature It is in step 4), the one kind of the magnetic nano-particle in metal, metal oxide, alloy.
5. the synthetic method of high polymer as claimed in claim 1/graphene@magnetic nano-particle foamed composites, its feature It is in step 5), the tablet uses glass plate.
6. the synthetic method of high polymer as claimed in claim 1/graphene@magnetic nano-particle foamed composites, its feature It is in step 5), the temperature of the drying is 60 DEG C.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113527678A (en) * 2020-04-14 2021-10-22 中科院广州化学有限公司 Polyimide foam composite material and preparation method and application thereof

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US20110160372A1 (en) * 2009-12-31 2011-06-30 Cheil Industries Inc. Thermoplastic Resin Composition with EMI Shielding Properties
CN102732037A (en) * 2011-04-08 2012-10-17 中国科学院金属研究所 Graphene foam/polymer high-conductivity composite material preparation method and application thereof
CN103319892A (en) * 2013-07-12 2013-09-25 中国科学院长春应用化学研究所 Polyimide foamed composite and preparation method thereof
CN105524466A (en) * 2014-09-28 2016-04-27 中国科学院苏州纳米技术与纳米仿生研究所 Porous graphene electromagnetic wave absorbing composite material, preparation method and applications thereof
WO2017116657A1 (en) * 2015-12-28 2017-07-06 Nanotek Instruments, Inc. Graphene-Carbon Hybrid Foam

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1887038A (en) * 2003-11-25 2006-12-27 爱克工业株式会社 Electromagnetic wave shielding resin composition, ferrite-coated metal magnetic microparticle suitable for use therein and process for producing the same
US20110160372A1 (en) * 2009-12-31 2011-06-30 Cheil Industries Inc. Thermoplastic Resin Composition with EMI Shielding Properties
CN102732037A (en) * 2011-04-08 2012-10-17 中国科学院金属研究所 Graphene foam/polymer high-conductivity composite material preparation method and application thereof
CN103319892A (en) * 2013-07-12 2013-09-25 中国科学院长春应用化学研究所 Polyimide foamed composite and preparation method thereof
CN105524466A (en) * 2014-09-28 2016-04-27 中国科学院苏州纳米技术与纳米仿生研究所 Porous graphene electromagnetic wave absorbing composite material, preparation method and applications thereof
WO2017116657A1 (en) * 2015-12-28 2017-07-06 Nanotek Instruments, Inc. Graphene-Carbon Hybrid Foam

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113527678A (en) * 2020-04-14 2021-10-22 中科院广州化学有限公司 Polyimide foam composite material and preparation method and application thereof
CN113527678B (en) * 2020-04-14 2023-04-07 中科院广州化学有限公司 Polyimide foam composite material and preparation method and application thereof

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