CN107129680A - A kind of ferroso-ferric oxide/polypyrrole/polyaniline nano compound and preparation method thereof - Google Patents
A kind of ferroso-ferric oxide/polypyrrole/polyaniline nano compound and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of ferroso-ferric oxide/polypyrrole/polyaniline nano compound and preparation method thereof.Ferroso-ferric oxide/polypyrrole/polyaniline nano compound, including ferroso-ferric oxide sandwich layer, the polypyrrole layer for being wrapped in ferroso-ferric oxide sandwich layer periphery and the polyaniline for being wrapped in polypyrrole layer periphery.Ferroso-ferric oxide (Fe of the present invention3O4)/polypyrrole (PPy)/polyaniline (PANI) nano-complex has superior microwave absorption capacity, while being also better than the same period existing similar compound；Large-scale conductive network is established due to introducing inside multilayer conductive high polymer, system, resistivity declines to a great extent, and the cladding between different medium introduces interfacial polarization, improves impedance matching, and these factors have all greatly reinforced the wave-absorbing effect of system.
Description
Technical field
The present invention relates to a kind of ferroso-ferric oxide/polypyrrole/polyaniline nano compound and preparation method thereof, belong to suction ripple
Material Field.
Background technology
Microwave absorbing material attracts increasing concern in recent years, they precision instrument, military stealth technology and
Key player is all play in electromangnetic spectrum.The absorbing material of excellent performance usually requires have wide absorption, strong decay, matter
The characteristics of measuring light and thickness of thin, this requires material while having high magnetic loss or high dielectric loss, good impedance matching, and
Every electromagnetic parameter meets loss theory on the premise of light weight.However, these features are difficult while appearing on a kind of material：
Impedance matching is influenceed by electrical property and magnetic property simultaneously, and the mechanism influenceed is sufficiently complex so that hindered by adjustment of electro-magnetic parameters
Anti- matching is highly difficult；High magnetic loss generally requires to introduce metal composite so that density of material significantly increases；Good suction ripple effect
Fruit is often also required to thicker thickness.These problems cause homogenous material or simple blended complex can not almost be met will
Ask, it is necessary to there is specific structure according to loss Theoretical Design and add according to demand required component material adjust whole system
Electromagnetic parameter is to achieve the goal.
Magnetic nano-particle, such as Fe3O4, have been widely used in field of microwave absorption and have been proved to have well
Magnetic loss property.But due to its absorption band width and quality is too big, suffers from many limitations in use.
The content of the invention
In order to solve the defect such as absorption band width in the prior art, a kind of ferroso-ferric oxide/polypyrrole of present invention offer/poly-
Aniline nano compound and preparation method thereof.
In order to solve the above technical problems, the technical solution adopted in the present invention is as follows：
A kind of ferroso-ferric oxide/polypyrrole/polyaniline nano compound, including ferroso-ferric oxide sandwich layer, it is wrapped in four oxygen
Change the polypyrrole layer of three-iron sandwich layer periphery and be wrapped in the polyaniline of polypyrrole layer periphery.
The application ferroso-ferric oxide (Fe3O4)/polypyrrole (PPy)/polyaniline (PANI) nano-complex has superior micro-
Ripple absorbability, while being also better than the same period existing similar compound.By characterizing, due to introducing multilayer conductive high polymer, body
System is internal to establish large-scale conductive network, and resistivity declines to a great extent, and the cladding between different medium introduces interfacial polarization, improves
Impedance matching, these factors have all greatly reinforced the wave-absorbing effect of system.
In order to which the particle diameter for being further ensured that ferroso-ferric oxide in wave-absorbing effect, ferroso-ferric oxide sandwich layer is 15 ± 3nm.
The preparation method of above-mentioned ferroso-ferric oxide/polypyrrole/polyaniline nano compound, Fe is prepared by coprecipitation3O4
Nano-particle, with Fe3O4The cladding that in-situ polymerization completes polypyrrole is carried out as nucleation site, the parcel of polyaniline is finally completed.
Stronger attraction ensure that polyaniline in Fe between the carbonyl group and polyaniline conjugated chain of polypyrrole3O4/PPy
The attachment of double base composite surface.
In order to further improve impedance matching, coprecipitation prepares Fe3O4The method of nano-particle is：Protected in nitrogen
Under the conditions of, frerrous chloride and iron chloride are dissolved under water, stirring condition and are heated to 50 ± 5 DEG C, is adjusted Ph to 11 with ammoniacal liquor, so
Continue to stir 1 ± 0.1h under conditions of 50 ± 5 DEG C afterwards, be cooled to room temperature, dipping magnetic inclination analysis separation and Extraction product is washed, dried, i.e.,
Obtain Fe3O4Nano-particle.
In order to be further ensured that wave-absorbing effect, it is preferable that frerrous chloride is FeCl2·4H2O, iron chloride is FeCl3·6H2O,
The mass ratio of frerrous chloride and iron chloride is 1：(2.5-3)；Mixing speed is 600-800rpm；Wash to be each with water and ethanol
Washing five times.The quality consumption of water is 20-30 times of iron chloride and chlorination weight of iron sum；Dry is under conditions of 60 ± 5 DEG C
Dry 8 ± 0.2h.
In order to further improve wave-absorbing effect, with Fe3O4The cladding that in-situ polymerization completes polypyrrole is carried out as nucleation site
Method be：By Fe3O4Nano-particle and FeCl3·6H2O is dissolved in water, after 3 ± 0.2h of stirring under conditions of 25 ± 5 DEG C, plus
Enter neopelex solution and pyrrole monomer, 12 ± 1h, dipping magnetic inclination analysis separation and Extraction production are stirred under conditions of 25 ± 5 DEG C
Thing, washs, dries, obtain Fe3O4/PPy nano-complexes.
In order to further improve impedance matching, Fe3O4Nano-particle and FeCl3·6H2O mass ratio is 1：(18±3)；
The quality consumption of water is Fe3O4Nano-particle and FeCl3·6H212-18 times of O mass sums；Mixing speed is 500-
700rpm；The mass concentration of neopelex solution is 5-7wt%, neopelex solution and pyrrole monomer
Volume ratio be 64-68；The volume ratio of water and neopelex solution is 7-8；Dry is under conditions of 60 ± 5 DEG C
Dry 4 ± 0.2h.
In order to further improve wave-absorbing effect, the method for polyaniline parcel is：By Fe3O4/ PPy nano-complexes are dispersed in
In hydrochloric acid, 1 ± 0.1h of ultrasonic agitation is subsequently added under aniline monomer, ice bath and stirred after 1 ± 0.1h, adds ammonium persulfate, stirring
24 ± 1h is reacted, dipping magnetic inclination analysis separating-purifying is washed until filtrate is colourless with deionized water and ethanol, dries, produce four oxidations three
Iron/polypyrrole/polyaniline nano compound.
The concentration of above-mentioned hydrochloric acid is 0.1mol/L, and the volume ratio of hydrochloric acid and aniline is 320-340；Fe3O4/ PPy is nano combined
The mass ratio of thing and ammonium persulfate is 2-2.5；The consumption of hydrochloric acid is every gram of Fe3O4/ PPy nano-complexes 240-260ml；Dry
To dry 4 ± 0.2h under conditions of 60 ± 5 DEG C.
The NM technology of the present invention is with reference to prior art.
Ferroso-ferric oxide (Fe of the present invention3O4)/polypyrrole (PPy)/polyaniline (PANI) nano-complex has superior micro-
Ripple absorbability, while being also better than the same period existing similar compound；Set up due to introducing inside multilayer conductive high polymer, system
Large-scale conductive network is played, resistivity declines to a great extent, the cladding between different medium introduces interfacial polarization, improves impedance
Match somebody with somebody, these factors have all greatly reinforced the wave-absorbing effect of system, absorption band is wide and light weight.
Brief description of the drawings
Fig. 1 is the gained nano-complex XRD diffraction maximums of embodiment 1:a:Fe3O4, b:Fe3O4/ PPy, c:Fe3O4/PPy/
PANI；
Fig. 2 is the FT-IR spectrograms of the gained nano-complex of embodiment 1:a:Fe3O4, b:Fe3O4/ PPy, c:Fe3O4/
PPy/PANI；
Fig. 3 is the TEM image of the gained nano-complex of embodiment 1：a:Fe3O4/ PPy, b:Fe3O4/PPy/PANI；
Fig. 4 changes for the real part (a figures) of the gained nano-complex complex dielectric permittivity of embodiment 1 with imaginary part (b figures) with frequency
Graph of a relation；
Fig. 5 changes for the real part (a figures) of the gained nano-complex complex permeability of embodiment 1 with imaginary part (b figures) with frequency
Graph of a relation；
Fig. 6 is the gained Fe of embodiment 13O4、Fe3O4/ PPy and Fe3O4/ PPy/PANI tan δε(a figures) and tan δμ(b figures)
Variation diagram；
Fig. 7 is the gained Fe of embodiment 13O4, Fe3O4/ PPy and Fe3O4/PPy/PANIC0The curve changed with frequency；
Fig. 8 is the microwave absorption curve (20wt%, 2.6mm) of 1 three kinds of nano-complexes of embodiment；
Embodiment
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention
Content is not limited solely to the following examples.
Embodiment 1
Ferroso-ferric oxide/polypyrrole/polyaniline nano compound, including ferroso-ferric oxide sandwich layer, it is wrapped in four oxidations three
The polypyrrole layer of iron core layer periphery and the polyaniline for being wrapped in polypyrrole layer periphery.
The preparation method of above-mentioned Fe 3 O/polypyrrole/polyaniline nano compound includes：
1) synthesis of Fe3O4 nano-particles
Fe is prepared by coprecipitation3O4Nano-particle：40ml deionized waters, nitrogen deoxygenation are added in three-necked flask
20min, by 0.43gFeCl24H2O and 1.18g FeCl3·6H2O adds three-necked flask, and 700rpm is stirred and heated to 50
DEG C, about 4.5ml ammoniacal liquor (26wt%), regulation Ph values to 11, solution rapid blackening, magnetic Nano after ammoniacal liquor is added is added dropwise
Particle is generated, and reaction continues to stir 1h at 50 DEG C, and room temperature, dipping magnetic inclination analysis (10 × 10 × 4cm3,1.4T) separation are cooled to afterwards
Product is extracted, is washed with deionized water and ethanol five times, 60 DEG C of dry 8h in vacuum drying chamber, the Fe that particle diameter is 15nm is obtained3O4
Nano-particle.
2)Fe3O4The synthesis of/PPy nano-complexes
The one pot process process is completed in tri- mouthfuls of round bottom beakers of a 250ml, 0.5g Fe3O4Nano-particle and
9.0gFeCl3·6H2O is added in 150ml deionized waters, and 600rpm stirrings 3h causes Fe3+ ions pass through homo-ion at 25 DEG C
Effect is gathered in nano grain surface.Afterwards by 20mlC18H29NaSO3Solution (5.85wt%) and 0.3mL PPy monomers add anti-
Liquid is answered, 12h is stirred at room temperature.(10 × 10 × 4cm3,1.4T) separation and Extraction product is analysed in dipping magnetic inclination, is washed with deionized water and ethanol
Five times, 60 DEG C of dry 4h in vacuum drying chamber.
3)Fe3O4The synthesis of/PPy/PANI nano-complexes
0.4g Fe3O4/ PPy nano-complexes are dispersed in 100ml0.1M HCl, ultrasonic agitation 1h；It is subsequently added into
1h is stirred under 0.3ml aniline monomers, ice bath；Add 0.9g ammonium persulfates, stirring reaction 24h；End-product dipping magnetic inclination analysis separation is carried
Pure, deionized water and ethanol are repeatedly washed until filtrate is colourless, and 60 DEG C of dry 4h, obtain four oxidations three in vacuum drying chamber
Iron/polypyrrole/polyaniline nano compound.
Characterize and test
X-ray diffractometer model is D8A Advance, BRUKER, and FTIS model is
Nicolet6700, ESEM and constituent analysis use field emission scanning electron microscope, model FE-SEM, Ultra55,
CarlZeiss, energy dispersive spectrometry model is EDS, X-MAX 50, Oxford Instrument.Sample for inhaling ripple test
Using paraffin as base material, nano-complex accounts for mass fraction 20wt%, using vector network analyzer test 2-18GHz it
Between electromagnetic parameter, thus evaluate its absorbing property, vector network analyzer model Agilent N5242A.
As a result with discussion
Fig. 1 illustrates pure Fe3O4Nano-particle (Fig. 2 a) Fe3O4/ PPy (Fig. 2 b) and Fe3O4/ PPy/PANI (Fig. 2 c), by
It is that the atom center of area is stood that the peak at (220) marked out in figure, (311), (400), (422), (511), and (440) place, which can be inferred that,
Square Fe3O4.It can be seen that increasing with clad, the XRD peaks of nano-complex do not have obvious change, illustrate conductive polymer
Deposition of the son on magnetic-particle surface does not have an impact nanometer Fe3O4The crystal formation of itself.
In order to confirm the presence of polypyrrole and polyaniline in the composite, table is carried out to product with FTIR spectrum figure
Levy.As shown in Figure 2, Fe3O4Particle only has two main absworption peaks, respectively in 585cm-1And 3424cm-1Place, respectively from
The Fe-O keys and-OH groups of nano grain surface.After polypyrrole completes cladding, the absworption peak of pyrroles appears in Fe3O4/ PPy's
In spectrogram (Fig. 2 b), 1544cm-1Place is the stretching vibration of C-C on pyrrole ring, 1046cm-1And 1446cm-1Peak from C-N's
Stretching vibration, 1296cm-1And 1166cm-1The peak at place is 1/4C H in plane vibration, and 1/4CH out-of-plane vibration peak is in 784cm-1And 895cm-1Place.This shows polypyrrole among binary nano complex.For Fe3O4/ PPy/PANI ternary nanos are answered
Compound, 1298cm-1The peak at place demonstrates the presence of C-N stretching vibrations on polyaniline, 798cm-1The absorption band at place comes from C-H faces
Outside sweep is vibrated, and may infer that polyaniline is present among the ternary complex.
Compound is observed to determine its pattern with projection electron microscope (TEM), as shown in figure 3, darker regions are Fe3O4
Nano particle, and the part of grey is the clad of polypyrrole and polyaniline, it can be seen that Fe3O4Particle diameter it is probably left in 15nm
The right side, (Fig. 3 a) is coated with by polypyrrole, has been carried out in polyaniline after one layer of new cladding, the part of conducting polymer is significantly thicker
(Fig. 3 b).
The electromagnetic property of nano-complex
The electromagnetic property of material can pass through its complex dielectric permittivity ε in the range of 2-18GHzr=ε 'r+ε″rAnd complex permeability
μr=μ 'r+μ″rTo be characterized, real part of permittivity (ε ') and magnetic conductivity real part (μ ') r represent the storage energy to electromagnetic energy
Power, and imaginary part of dielectric constant (ε ") and magnetic conductivity imaginary part (μ ") represent the ability for decaying to electromagnetic energy and being lost.
It is the graph of a relation that the real part of material complex dielectric permittivity and imaginary part change with frequency, Fe in Fig. 43O4Dielectric constant it is real
Portion has almost no change with imaginary part in the range of 2-18GHz, Fe3O4/ PPy and Fe3O4/ PPy/PANI ε 'rWith ε "rWith frequency
Raise and decline, this point is to Fe3O4/ PPy is especially apparent, and this should be due to that, as frequency is raised, polarization intensity and frequency are not
Caused by matching.Fe3O4/ PPy high ε ' represents its high electrode intensity and high conductivity, and this 2 points reinforcement is derived from
The introducing of polyaniline forms a big conducting networks.And its clad is blocked up after polyaniline is introduced, with Fe3O4/ PPy phases
Polarization intensity and dielectric constant than ternary complex is all relatively low.
It is the complex permeability variation diagram of nano-complex in Fig. 5.Generally speaking, as frequency is raised, magnetic conductivity is in decline
Trend, this point is especially apparent for magnetic conductivity imaginary part.Can clearly it see from figure, in more than 9GHz frequency range
Magnetic conductivity imaginary part substantially no longer changes, and fluctuation within a narrow range within the specific limits.
The absorbing property of nano-complex
Fig. 6 illustrates Fe3O4, Fe3O4/ PPy and Fe3O4Dielectric loss (the tan δ of tri- kinds of nano-complexes of/PPy/PANIε)
With electromagnetic consumable (tan δμ), both losses are to influence the dominant loss of Absorbing Materials, can be divided with loss angle tangent
Do not represent：tanδε=ε "/ε ' and tan δμ=μ "/μ '.The raising of material electromagnetic wave absorption effect is mostly come to its compatibility matching
The regulation of property.From the figure, it can be seen that with simple Fe3O4Magnetic particle is compared, and adds dielectric loss after conduction high polymer
It is significantly increased, this has benefited from the interfacial polarization that magnetic-particle and conduction high polymer clad are formed, Fe3O4/ PPy Tan δε
In the range of 2-18GHz 1.20 are increased to from 0.80, and Fe3O4/ PPy/PANI drops to 0.40 by 0.70 within the range.Three
Magnetic loss all drastically decline in the range of 2-8GHz, and tended to be steady after 8GHz, a small range is floated.Absorbing property exists
Outside high dielectric loss and high magnetic loss, in addition it is also necessary to which emphasis considers the matching degree between complex dielectric permittivity and complex permeability, without
It is that simple a certain loss higher position can be with.After addition conduction high polymer is adjusted, two losses of compound all have certain journey
The raising of degree.
It can see from Fig. 4, Fig. 5, magnetic conductivity imaginary part and magnetic loss all tend to assimilation peace on 8-9GHz position
Surely, thus infer that the system there may be eddy-current loss, C can be expressed as0：
C0=μ " (μ ')-2f-1=2 π μ0σd2
Wherein, σ and d represent electrical conductivity and material thickness, μ respectively0Represent space permeability.If C0As frequency changes
Acutely lifting, does not illustrate that eddy-current loss is main magnetic loss within the range.As shown in fig. 7, C0In 2-8GHz scopes
Inside drastically decline, and had almost no change in the range of 8-18GHz, illustrated in these systems, be vortexed and damage in the range of 8-18GHz
Consumption is the leading loss in magnetic loss.And in low-frequency range, magnetic loss is made up of other mechanism, including natural resonance, magnetic hysteresis
Loss and magnetic domain resonance etc..
The reflection loss (RL) of material can be by measured relative complex dielectric permittivity and complex permeability according to transmission line
Theory is calculated：
Wherein ZinRepresent normalized impedance matching, Z0It is the characteristic matching of free space, ε0And μ0It is free space respectively
Dielectric constant and magnetic conductivity, c are the lighies velocity in vacuum, and d is the thickness of wave-absorber, and f is wave frequency.When RL is less than -10dB
When, it is believed that 90% electromagnetic wave energy is all absorbed, the scope less than -10dB is also considered as effective Absorber Bandwidth.
Fig. 8 illustrates Fe3O4, Fe3O4/ PPy and Fe3O4/ PPy/PANI accounts for the reflection loss of 20wt% mineral wax mixture
Curve, material thickness is 2.6mm.Although the introducing of polypyrrole substantially increases the dielectric loss ability of system, Fe3O4/PPy
Wave-absorbing effect than simple Fe3O4Particle is also weak, because its impedance matching is too poor, it is impossible to the assimilation effect reached.And
Fe3O4/ PPy/PANI wave-absorbing effect is very good, and the most strong absworption peak RL at 10.1GHz reaches -40.2dB, while absorption band
Width reaches 10.7GHz (6.7to 17.4GHz).The introducing that the rapidly lifting of the wave-absorbing effect comes from multilayer conductive high polymer makes
The resistance for the system of obtaining declines, and has large-scale conductive network generation, while polypyrrole and polyaniline improve multiple Jie of system
Electric constant and the loss mechanisms for introducing interfacial polarization, have greatly reinforced dielectric loss, in addition the eddy-current loss between 8-18GHz
Effect is also apparent from.By Fe3O4/ PPy/PANI and other existing Fe3O4Done pair with the wave-absorbing effect of conduction high polymer composite
Than (table 1), hence it is evident that the material has most fast effective Absorber Bandwidth and maximum maximum absorption peak, illustrate that there is application well
Prospect.
The Fe of table 13O4/ PPy/PANI and existing Fe3O4Conduction high polymer compound wave-absorbing effect is contrasted
In table, wt (%) is mass fraction, is usually to do electromagnetism test after wave absorbing agent is mixed with paraffin to calculate suction ripple
Performance, the mass fraction refers to wave absorbing agent mass fraction shared in the mixed system with paraffin, close in wave-absorbing effect
In the case of, numerical value is the smaller the better；MWCNT multilayer carbon nanotubes；CIP carbonyl irons；Graphene graphenes；microspheres
Microballoon；Polypyrrole polypyrroles；Carbon CNTs.
Embodiment 2-6
According to the preparation method and step of embodiment 1, prepare and contain different ferroso-ferric oxide/polypyrrole/polyaniline ratios
Nano-complex, its specific formula and absorbing property are as shown in table 2.
Table 2
Data in table 2 are that thickness is Fe under the data under the conditions of 2.0mm, the thickness3O4And Fe3O4/ PPy effectively inhales
Take-up is wide by both less than 6, and absworption peak is than all Fe3O4The corresponding numerical value of/ppy/PANI ratios is low.For relative maximum absworption peak,
Absorber Bandwidth is even more important evaluation index, because -47dB and -50dB absorption efficiency difference can be ignored,
Embodiment 1 is optimal experimental group.In addition, the density of ferroso-ferric oxide is 5.17 grams/cc, low-density is being introduced
After PPy and PANI (being 1 gram/cc), the density of different ferroso-ferric oxide/polypyrrole/polyaniline nano compounds is equal
Less than 2 grams/cc.
Claims (10)
1. a kind of ferroso-ferric oxide/polypyrrole/polyaniline nano compound, it is characterised in that：Including ferroso-ferric oxide sandwich layer, bag
The polypyrrole layer for being rolled in ferroso-ferric oxide sandwich layer periphery and the polyaniline for being wrapped in polypyrrole layer periphery.
2. ferroso-ferric oxide/polypyrrole/polyaniline nano compound as claimed in claim 1, it is characterised in that：Four oxidations three
The particle diameter of ferroso-ferric oxide is 15 ± 3nm in iron core layer.
3. the preparation method of ferroso-ferric oxide/polypyrrole/polyaniline nano compound described in claim 1 or 2, its feature exists
In：Fe is prepared by coprecipitation3O4Nano-particle, with Fe3O4The bag that in-situ polymerization completes polypyrrole is carried out as nucleation site
Cover, finally complete the parcel of polyaniline.
4. method as claimed in claim 3, it is characterised in that：Coprecipitation prepares Fe3O4The method of nano-particle is：In nitrogen
Under conditions of gas shielded, frerrous chloride and iron chloride are dissolved under water, stirring condition and are heated to 50 ± 5 DEG C, Ph is adjusted with ammoniacal liquor
Then section continues to stir 1 ± 0.1h to 11 under conditions of 50 ± 5 DEG C, is cooled to room temperature, and dipping magnetic inclination analysis separation and Extraction product is washed
Wash, dry, produce Fe3O4Nano-particle.
5. method as claimed in claim 4, it is characterised in that：Frerrous chloride is FeCl2·4H2O, iron chloride is FeCl3·
6H2The mass ratio of O, frerrous chloride and iron chloride is 1：(2.5-3)；Mixing speed is 600-800rpm；Wash as with water and
Ethanol respectively washing five times.
6. method as claimed in claim 4, it is characterised in that：The quality consumption of water is iron chloride and chlorination weight of iron sum
20-30 times；Dry is that 8 ± 0.2h is dried under conditions of 60 ± 5 DEG C.
7. the method as described in claim 3-6 any one, it is characterised in that：With Fe3O4Carried out as nucleation site in situ poly-
Close and complete the method for cladding of polypyrrole and be：By Fe3O4Nano-particle and FeCl3·6H2O is dissolved in water, in 25 ± 5 DEG C of condition
After 3 ± 0.2h of lower stirring, neopelex solution and pyrrole monomer are added, stir 12 under conditions of 25 ± 5 DEG C ±
1h, dipping magnetic inclination analysis separation and Extraction product, washs, dries, obtain Fe3O4/PPy nano-complexes.
8. method as claimed in claim 7, it is characterised in that：Fe3O4Nano-particle and FeCl3·6H2O mass ratio is 1：
(18±3)；The quality consumption of water is Fe3O4Nano-particle and FeCl3·6H212-18 times of O mass sums；Mixing speed is
500-700rpm；The mass concentration of neopelex solution is 5-7wt%, neopelex solution and pyrroles
The volume ratio of monomer is 64-68；The volume ratio of water and neopelex solution is 7-8；Dry as in 60 ± 5 DEG C of bar
4 ± 0.2h is dried under part.
9. method as claimed in claim 7, it is characterised in that：Polyaniline parcel method be：By Fe3O4/ PPy is nano combined
Thing is dispersed in hydrochloric acid, 1 ± 0.1h of ultrasonic agitation, is subsequently added under aniline monomer, ice bath and is stirred after 1 ± 0.1h, adds over cure
Sour ammonium, 24 ± 1h of stirring reaction, dipping magnetic inclination analysis separating-purifying is washed until filtrate is colourless with deionized water and ethanol, dries, produce
Ferroso-ferric oxide/polypyrrole/polyaniline nano compound.
10. method as claimed in claim 9, it is characterised in that：The concentration of hydrochloric acid is 0.1M, and the volume ratio of hydrochloric acid and aniline is
320-340；Fe3O4The mass ratio of/PPy nano-complexes and ammonium persulfate is 2-2.5；The consumption of hydrochloric acid is every gram of Fe3O4/PPy
Nano-complex 240-260ml；Dry is that 4 ± 0.2h is dried under conditions of 60 ± 5 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109065211A (en) * | 2018-05-30 | 2018-12-21 | 查公祥 | A kind of poly closes composite conducting additive and preparation method thereof |
| CN109608879A (en) * | 2018-11-20 | 2019-04-12 | 郑州大学 | A kind of hollow ferroso-ferric oxide microballoon@polyaniline/polyimide composite film absorbing material and preparation method |
| CN109731617A (en) * | 2018-12-13 | 2019-05-10 | 东莞理工学院 | A kind of Fe3O4/ polypyrrole/polyaniline/TiO2The preparation method of/ZnO composite material |
| CN114314679A (en) * | 2021-12-31 | 2022-04-12 | 华中科技大学 | Polypyrrole-coated ferroferric oxide nanoflower wave-absorbing material, preparation method and application |
-
2017
- 2017-05-25 CN CN201710380164.5A patent/CN107129680A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| BINGZHEN LI ET AL: "Synthesis of Fe3O4/polypyrrole/polyaniline nanocomposites by in-situ method and their electromagnetic absorbing properties", 《JOURNAL OF SAUDI CHEMICAL SOCIETY》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109065211A (en) * | 2018-05-30 | 2018-12-21 | 查公祥 | A kind of poly closes composite conducting additive and preparation method thereof |
| CN109608879A (en) * | 2018-11-20 | 2019-04-12 | 郑州大学 | A kind of hollow ferroso-ferric oxide microballoon@polyaniline/polyimide composite film absorbing material and preparation method |
| CN109731617A (en) * | 2018-12-13 | 2019-05-10 | 东莞理工学院 | A kind of Fe3O4/ polypyrrole/polyaniline/TiO2The preparation method of/ZnO composite material |
| CN114314679A (en) * | 2021-12-31 | 2022-04-12 | 华中科技大学 | Polypyrrole-coated ferroferric oxide nanoflower wave-absorbing material, preparation method and application |
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