CN107903394B - High polymer/graphene@magnetic nano-particle foamed composite synthetic method - Google Patents
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Abstract
High polymer/graphene@magnetic nano-particle foamed composite synthetic method, is related to polyimides.1) graphene solution is prepared；2) diaminodiphenyl ether powder is added in the graphene solution of step 1) preparation and is mixed, obtain solution A；3) pyromellitic acid anhydride powder is added in the mixed solution A of step 2) preparation and is 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 plate, then is placed on using water to be dried in the flocculation basin of flocculant after flocculation；Resulting material 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, strong operability, favorable reproducibility, yield is up to 95%.
Description
Technical field
The present invention relates to polyimides, more particularly, to high polymer/graphene@magnetic nano-particle foamed composite
Synthetic method.
Background technique
Polyimides has excellent mechanical performance, and some polyimides kinds do not dissolve in organic solvent, stablizes to diluted acid
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 is huge either as structural material or as functional material because of its outstanding feature in terms of performance and synthesis
Application prospect adequately recognized, be known as " expert solved the problems, such as ", and thinks " just not without polyimides
Have the microelectric technique of today ".This foaming structure existing research that polyimides high polymer and graphene are 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.
Summary of the invention
It is relatively simple that the purpose of the present invention is to provide processing steps, and foaming structure synthesizes more uniform and high polymer/stone
The synthetic method of black alkene@magnetic nano-particle foamed composite.
The present invention the following steps are included:
1) graphene solution is prepared；
In step 1), the specific method for preparing graphene solution can are as follows: 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 is mixed, obtain solution A；
3) pyromellitic acid anhydride (PMDA) powder is added in the mixed solution A of step 2) preparation and is condensed, obtain solution B；
In step 3), in the mixed solution A that pyromellitic acid anhydride (PMDA) powder is added to step 2) preparation
Condensation can will be added 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 can be selected from one of metal, metal oxide, alloy etc..
5) solution C for obtaining step 4) is poured on plate, then is placed on using water as in the flocculation basin of flocculant, after flocculation
Drying；
In step 5), glass plate etc. is can be used in the plate；The temperature of the drying can be 60 DEG C.
The resulting material of the present invention is structurally characterized in that the high polymer with obvious foaming structure/graphene@magnetic Nano
Particle (metal, metal oxide, alloy) composite material, and show in electro-magnetic wave absorption the property of comparative superiority.
Of the invention has the prominent advantages that:
1) novel high polymer/graphene magnetic nano-particle (metal, metal oxidation is prepared using solution polycondensation
Object, alloy) foamed composite, this material is on microwave absorption with potential application prospect；
2) operation of the present invention is simple, and strong operability, favorable reproducibility, yield is up to 95%.
3) present invention can be prepared on a large scale, and realizes commercialization, has potential application in practical applications.
4) high temperature resistant of the present invention, has potential application in terms of aerospace.
Detailed description of the invention
Fig. 1 is high polymer/graphene scanning electron microscope (SEM) figure of foaming structure.
Fig. 2 is high polymer/graphene infrared spectrum 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 range is in 2~18GHz.
Fig. 7 is high polymer/graphene@FeCoNi scanning electron microscope (SEM) figure of foaming structure.
Fig. 8 is high polymer/corresponding X-ray powder diffraction figure of graphene@FeCoNi of foaming structure.
Fig. 9 is that high polymer/graphene@FeCoNi of foaming structure corresponds to the microwave absorption curve of different-thickness.In Fig. 9
In, test frequency range is in 2~18GHz.
It is high polymer/graphene@Co scanning electron microscope (SEM) figure of foaming structure corresponding to Figure 10.
It is high polymer/graphene@Co ray powder diffraction pattern of foaming structure corresponding to Figure 11.
Specific 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 weigh the ODA and PMDA that equimolar amounts is added, 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 weigh the ODA and PMDA that equimolar amounts is added, and mechanical stirring 5h is added a certain amount of later
Metal oxide is (with Fe3O4For), 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, it is placed on 16h in 60 DEG C of baking oven.
As seen from Figure 1 with a process for preparing foaming structures.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. nanoparticles foaming structure.X-ray powder diffraction figure in Fig. 5 it 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 there is no 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 lamellar spacing according to analogue data
For 2mm, it is lower than -10dB absorption band range, reaches 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 weigh the ODA and PMDA that equimolar amounts is added, and mechanical stirring 7h is added a certain amount of later
Metal alloy (by taking FeCoNi as an example) continues to stir 5h, and 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, it is placed on 12h in 60 DEG C of baking oven.
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 is it 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 lamellar spacing according to analogue data
2.5mm is lower than -10dB absorption band range, 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 weigh the ODA and PMDA that equimolar amounts is added, mechanical stirring 10h, are added later 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 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@graphene and magnetic metal alloy nanoparticles foaming structure are prepared for.Figure 11
X-ray powder diffraction figure it 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. high polymer/graphene@magnetic nano-particle foamed composite synthetic method, it is characterised in that including following step
It is rapid:
1) graphene solution is prepared；
2) diaminodiphenyl ether (ODA) powder is added in the graphene solution of step 1) preparation and is mixed, obtain solution A；
3) pyromellitic acid anhydride (PMDA) powder is added in the mixed solution A of step 2) preparation and is 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 plate, then is placed on using water to be dried in the flocculation basin of flocculant after flocculation
It is dry.
2. high polymer as described in claim 1/graphene@magnetic nano-particle foamed composite synthetic method, feature
It is in step 1), the graphene solution for preparing method particularly includes: graphene is added to n,N-Dimethylformamide
In solution, ultrasonic mixing obtains graphene solution.
3. high polymer as described in claim 1/graphene@magnetic nano-particle foamed composite synthetic method, feature
Be in step 3), it is described will pyromellitic acid anhydride powder be added step 2) preparation 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. high polymer as described in claim 1/graphene@magnetic nano-particle foamed composite synthetic method, feature
It is in step 4), the magnetic nano-particle is selected from one of metal, metal oxide, alloy.
5. high polymer as described in claim 1/graphene@magnetic nano-particle foamed composite synthetic method, feature
It is in step 5), the plate uses glass plate.
6. high polymer as described in claim 1/graphene@magnetic nano-particle foamed composite synthetic method, feature
It is in step 5), the temperature of the drying is 60 DEG C.
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