CN110256847A - Polyaniline/carbon foam composite preparation method with controllable absorbing property - Google Patents
Polyaniline/carbon foam composite preparation method with controllable absorbing property Download PDFInfo
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- CN110256847A CN110256847A CN201910526617.XA CN201910526617A CN110256847A CN 110256847 A CN110256847 A CN 110256847A CN 201910526617 A CN201910526617 A CN 201910526617A CN 110256847 A CN110256847 A CN 110256847A
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- carbon foam
- polyaniline
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- dispersion liquid
- absorbing property
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- 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
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
Abstract
The present invention relates to polyaniline/carbon foam composite preparation methods with controllable absorbing property, impregnate in the concentrated sulfuric acid after melamine foamed plastic is calcined, are dried to obtain carbon foam；In water by Bronsted acid, disperse oxidant, dispersion liquid A is obtained；Aniline is dispersed in water to obtain aniline dispersion liquid, is redispersed in mixture of ice and water, dispersion liquid B is obtained；Carbon foam is fully absorbed and is put into dispersion liquid A after dispersion liquid B, is stirred under ice/water mixture, foam is filtered out, polyaniline/carbon foam composite is prepared in vacuum freeze drying again after pre-cooled jelly processing.Compared with prior art, the present invention has very superior suctions intensity of wave and wider suctions wavestrip wide, and it possesses good elasticity and can make composite foam by external force application deformation occurs so that its absorbing property be adjusted.
Description
Technical field
The present invention relates to a kind of preparation methods of absorbing material, more particularly, to a kind of polyphenyl with controllable absorbing property
Amine/carbon foam composite preparation method.
Background technique
Carbon foam has specific pore structure, and wherein most aperture interconnects, and this special structure makes it have
The excellent performances such as biggish specific surface area, light weight, thermal stability be good, high thermal conductivity and electric conductivity.In addition, the performance of carbon foam
It also will receive the influence of composite properties contained therein other than being determined by pore structure size, therefore compared with the carbon materials of other forms
There is more wide application for material.Carbon foam is applied in absorbing material preparation field at present, there is preparation methods
Complexity, and inhale the lesser disadvantage of intensity of wave.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide one kind to have controllable suction wave
Polyaniline/carbon foam composite preparation method of performance is prepared by a kind of easy means and adjusts tool by stress
There is adjustable height to inhale intensity of wave and inhales the wide composite foam of wavestrip.
The purpose of the present invention can be achieved through the following technical solutions:
Polyaniline/carbon foam composite preparation method with controllable absorbing property, comprising:
Clean melamine foamed plastic is cooled to room temperature after calcination processing, taking-up, which is placed in the concentrated sulfuric acid, impregnates, then uses
Deionized water is washed repeatedly to neutrality, obtains carbon foam through being dried；
Bronsted acid, oxidant is fully dispersed in water, obtain dispersion liquid A；
Aniline is dispersed in water to obtain aniline dispersion liquid, which is redispersed in mixture of ice and water, is divided
Dispersion liquid B；
It is put into dispersion liquid A after carbon foam is fully absorbed dispersion liquid B, is stirred under ice/water mixture, filter out foam simultaneously
With deionized water and ethanol washing until washing lotion is transparent, vacuum freeze drying again after pre-cooled jelly processing, be prepared polyaniline/
Carbon foam composite.
The melamine foamed plastic handles 1-5h in 500-950 DEG C of temperature lower calcination.The too low resulting production of calcination temperature
Object surface carbonation is uneven；The excessively high then foam of temperature is easy excessively carbonization, and matter is crisp and follows the string, and cannot achieve stress regulation and control,
And resistance attenuating reduces dielectric loss and also weakens absorbing property.
Preferred 800-900 DEG C of the melamine foamed plastic calcination processing temperature, time preferred 90-120min.In the calcining
Resulting carbon foam had both maintained three-dimensional network skeleton structure within the scope of temperature range, it may have good elasticity can pass through
Stress regulation and control deformation degree is realized to realize the adjusting to absorbing property, while surface is uniform carburized, improves it to electromagnetic wave
Dielectric loss ability, facilitate the promotion of its absorbing property.
The Bronsted acid includes hydrochloric acid, p-methyl benzenesulfonic acid or salicylic acid, the oxidant include ammonium persulfate, iron chloride or
Potassium bichromate.These Bronsted acid sources are wide at low cost and can effectively be doped to aniline monomer, so as to so that polyphenyl
Amine has good electric conductivity, is conducive to the dielectric loss of promotion system, to enhance absorbing property.
The molar ratio of the Bronsted acid and the oxidant is 0.01-0.8:0.02-0.1, the concentration of Bronsted acid in water
For 0.1-8mol/L.
In water, ultrasonic power 100-1000W, the time controls in 10- for the Bronsted acid, oxidant ultrasonic disperse
45min.Compared to dispersing modes such as mechanical stirrings, ultrasonic disperse is to mix from microcosmic (molecular level) angle to liquid material
It closes, can more effectively disperse and refine component drop, Bronsted acid and oxidant drop is allow to mix finer and smoother abundant.
The aniline forms the aniline dispersion liquid that concentration is 0.01-5mol/L through ultrasonic disperse, then through ultrasonic disperse in ice
In aqueous mixtures, ultrasonic power 100-1000W, the time is controlled in 1-12min.
It is that 200-2000rpm carries out magnetic agitation 1-6h that the carbon foam controls mixing speed in ice/water mixture.
In -10--90 DEG C of at a temperature of precooling 1-24h when precooling processing；The vacuum freeze drying is true
In vacuum freecing-dry machine, -8--60 DEG C, vacuum degree 1-15pa, freeze-drying 1-36h.
Polyaniline/the carbon foam composite being prepared has very superior suction intensity of wave and wider suction wavestrip
Width, and it possesses good elasticity and can be applied by external force and make composite foam deformation occurs to adjust to its absorbing property
Section prepares polyaniline/carbon foam composite with controllable absorbing property, and protection electronic device is in required work frequency
It can run well within the scope of rate without by Electromagnetic Interference.The present invention prepares to obtain controllable absorbing material, helps to expand and inhale
Application of the wave material in fields such as electromagnetic shielding, high-grade, precision and advanced defence and militaries.Polyaniline/carbon foam composite prepared by the present invention
Show bubble can be used for preparing controllable absorbing material field.
Compared with prior art, the present invention carries out on the basis of flexible carbon foam three-dimensional porous network structure with polyaniline
It is compound, be conducive to the dielectric loss and impedance matching performance that improve material, enhance its absorbing property.Meanwhile by applying to it
The mode of its deformation degree of different stress changes so to inhale intensity of wave and effectively inhale wavestrip it is wide regulate and control, further realize
By the controllable polyaniline/carbon foam composite of stress.This controllable absorbing property is to widen its practical application area with important
Meaning has the advantage that
One, the present invention makes carbon foam obtained by melamine foamed plastic surface carbonation not only have three using high-temperature calcination
Dimension reticular structure can increase electromagnetic wave in internal reflection to increase the loss to electromagnetic wave, while reduce sheet resistance
Be conducive to improve its dielectric loss ability and be conducive to polyaniline in the polymerization original position on its surface.
Two, the present invention can using polyaniline/carbon foam composite wave reflection loss of simple situ aggregation method preparation
Regulated and controled between -69.76~-20.49dB, is effectively inhaling that wavestrip is wide to be regulated and controled between 3.10-6.25GHz, with
The foam wave-suction material of existing method synthesis is compared, and light and its absorbing property is adjustable.
Three, polyaniline/carbon foam composite prepared by the present invention can be applicable to controllable absorbing material field.
Detailed description of the invention
Fig. 1 is the absorbing property figure under polyaniline/carbon foam composite undeformed；
Fig. 2 is polyaniline/carbon foam composite deformation 15% absorbing property figure；
Fig. 3 is polyaniline/carbon foam composite deformation 30% absorbing property figure；
Fig. 4 is polyaniline/carbon foam composite deformation 45% absorbing property figure.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection scope.
A kind of polyaniline/carbon foam composite preparation method with controllable absorbing property proposed by the present invention, tool
Steps are as follows for body:
(1) it prepares carbon foam: clean melamine foamed plastic being calcined in resistance furnace: in 500-950 DEG C of calcining at constant temperature
Room temperature is gradually cooling to after 1-5h.Whole process carries out under nitrogen protection.Taking-up is placed in dense after foam is cooled to room temperature
1-50min is impregnated in sulfuric acid, then is washed repeatedly with deionized water to neutrality, and the dry 1- in 20-50 DEG C of vacuum drying oven
12h；
(2) it prepares dispersion liquid A: weighing Bronsted acid 0.01mol-0.8mol, 50- is added in oxidant 0.02-0.1mol
In 360ml water；Under 500W power, ultrasonic disperse 10-45min keeps Bronsted acid and oxidant fully dispersed in water, uses
For Bronsted acid to be any in hydrochloric acid, p-methyl benzenesulfonic acid or salicylic acid, oxidant is to appoint in ammonium persulfate, iron chloride or potassium bichromate
It is a kind of；
(3) prepare dispersion liquid B: the ultrasonic disperse 0.03-0.1mol aniline (An) in 10-100ml water obtains An dispersion
Liquid, by An dispersion liquid ultrasonic disperse in mixture of ice and water, ultrasonic power 300W, ultrasonic time 1-12min；
(4) it prepares polyaniline/carbon foam composite: putting into dispersion after dry carbon foam is fully absorbed dispersion liquid B
In liquid A, under ice/water mixture, magnetic agitation is carried out with the revolving speed of 200-2000r/min and continues 1-6h.After the completion, it filters out
Foam and with deionized water and ethanol washing until washing lotion is transparent.Finally, by polyaniline/carbon foam (PANI/CF) at -50 DEG C
Precooling 1-24h in low temperature refrigerator, is subsequently placed in vacuum freeze drier and is freeze-dried 1-36h, obtains polyaniline/carbon foam
Composite material.
More detailed case study on implementation below, by following case study on implementation further illustrate technical solution of the present invention with
And the technical effect that can be obtained.
Embodiment 1:
The present embodiment be a kind of polyaniline/carbon foam composite preparation method with controllable absorbing property, by with
Lower step carries out:
(1) it prepares carbon foam: clean melamine foamed plastic being calcined in resistance furnace: in 950 DEG C of calcining at constant temperature 2.5h
After be gradually cooling to room temperature.Whole process carries out under nitrogen protection.It is taken out after foam is cooled to room temperature and is placed in the concentrated sulfuric acid
Middle immersion 15min, then washed repeatedly with deionized water to neutrality, and the dry 12h in 50 DEG C of vacuum drying oven；
(2) it prepares dispersion liquid A: weighing p-methyl benzenesulfonic acid 0.02mol, ammonium persulfate 0.02mol is added in 360ml water；?
Under 500W power, ultrasonic disperse 45min keeps Bronsted acid and oxidant fully dispersed in water；
(3) prepare dispersion liquid B: the ultrasonic disperse 0.03mol aniline (An) in 10ml water obtains An dispersion liquid, by An points
Dispersion liquid ultrasonic disperse is in mixture of ice and water, ultrasonic power 300W, ultrasonic time 12min；
(4) it prepares polyaniline/carbon foam composite: putting into dispersion after dry carbon foam is fully absorbed dispersion liquid B
In liquid A, under ice/water mixture, magnetic agitation is carried out with the revolving speed of 200r/min and continues 6h.After the completion, foam is filtered out simultaneously
With deionized water and ethanol washing until washing lotion is transparent.Finally, the low temperature by polyaniline/carbon foam (PANI/CF) at -50 DEG C
Precooling 2h in refrigerator, is subsequently placed in vacuum freeze drier and is freeze-dried 36h, obtains polyaniline/carbon foam composite.
The present invention makes carbon foam obtained by melamine foamed plastic surface carbonation not only have three-dimensional using high-temperature calcination
Reticular structure, which can increase electromagnetic wave, to be had in internal reflection to increase the loss to electromagnetic wave, while reduce sheet resistance
Conducive to improving its dielectric loss ability and be conducive to that polyaniline is in situ in the polymerization on its surface, so improve loss to electromagnetic wave with
It absorbs.
Polyaniline/carbon foam composite prepared by the present invention under 3.5mm thickness, works as composite foam under test frequency
When deformation occurs effectively loss can be realized to 90% or more electromagnetic wave within the scope of 8.70-14.95GHz,
At 12.90GHz, inhales intensity of wave and reach maximum value -69.76dB；When composite foam deformation 15%, effectively inhaling wavestrip width is
9.25-15.50GHz inhaling intensity of wave reaches maximum value -61.39dB；When composite foam deformation 30%, it is wide effectively to inhale wavestrip
For 9.05-15.30GHz, inhales intensity of wave and reach maximum value -28.77dB；When composite foam deformation 45%, wavestrip is effectively inhaled
Width is 6.95-10.95GHz, inhales intensity of wave and reaches maximum value -20.49dB.
Polyaniline/carbon foam composite prepared by the present invention can be applicable to controllable absorbing material field.
Embodiment 2:
The present embodiment be a kind of polyaniline/carbon foam composite preparation method with controllable absorbing property, by with
Lower step carries out:
(1) it prepares carbon foam: clean melamine foamed plastic being calcined in resistance furnace: in 950 DEG C of calcining at constant temperature 2.5h
After be gradually cooling to room temperature.Whole process carries out under nitrogen protection.It is taken out after foam is cooled to room temperature and is placed in the concentrated sulfuric acid
Middle immersion 15min, then washed repeatedly with deionized water to neutrality, and the dry 12h in 50 DEG C of vacuum drying oven；
(2) it prepares dispersion liquid A: weighing hydrochloric acid 0.3mol, ammonium persulfate 0.02mol is added in 360ml water；In 500W power
Under, ultrasonic disperse 45min keeps Bronsted acid and oxidant fully dispersed in water；
(3) prepare dispersion liquid B: the ultrasonic disperse 0.03mol aniline (An) in 10ml water obtains An dispersion liquid, by An points
Dispersion liquid ultrasonic disperse is in mixture of ice and water, ultrasonic power 300W, ultrasonic time 12min；
(4) it prepares polyaniline/carbon foam composite: putting into dispersion after dry carbon foam is fully absorbed dispersion liquid B
In liquid A, under ice/water mixture, magnetic agitation is carried out with the revolving speed of 200r/min and continues 6h.After the completion, foam is filtered out simultaneously
With deionized water and ethanol washing until washing lotion is transparent.Finally, the low temperature by polyaniline/carbon foam (PANI/CF) at -50 DEG C
Precooling 2h in refrigerator, is subsequently placed in vacuum freeze drier and is freeze-dried 36h, obtains polyaniline/carbon foam composite.
The present invention makes carbon foam obtained by melamine foamed plastic surface carbonation not only have three-dimensional using high-temperature calcination
Reticular structure, which can increase electromagnetic wave, to be had in internal reflection to increase the loss to electromagnetic wave, while reduce sheet resistance
Conducive to improving its dielectric loss ability and be conducive to that polyaniline is in situ in the polymerization on its surface, so improve loss to electromagnetic wave with
It absorbs.
Polyaniline/carbon foam composite prepared by the present invention can be in 5.6-18GHz frequency range when deformation occurs
Absorption of the interior realization to 90% electromagnetic wave, has reflection loss minimum -40.08 when with a thickness of 3.0mm at 13.78GHz.
Polyaniline/carbon foam composite prepared by the present invention can be applicable to controllable absorbing material field.
Embodiment 3:
The present embodiment be a kind of polyaniline/carbon foam composite preparation method with controllable absorbing property, by with
Lower step carries out:
(1) it prepares carbon foam: clean melamine foamed plastic being calcined in resistance furnace: in 950 DEG C of calcining at constant temperature 2.5h
After be gradually cooling to room temperature.Whole process carries out under nitrogen protection.It is taken out after foam is cooled to room temperature and is placed in the concentrated sulfuric acid
Middle immersion 15min, then washed repeatedly with deionized water to neutrality, and the dry 12h in 50 DEG C of vacuum drying oven；
(2) it prepares dispersion liquid A: weighing hydrochloric acid 0.3mol, ammonium persulfate 0.02mol is added in 360ml water；In 500W power
Under, ultrasonic disperse 45min keeps Bronsted acid and oxidant fully dispersed in water；
(3) prepare dispersion liquid B: the ultrasonic disperse 0.03mol aniline (An) in 10ml water obtains An dispersion liquid, by An points
Dispersion liquid ultrasonic disperse is in mixture of ice and water, ultrasonic power 300W, ultrasonic time 12min；
(4) it prepares polyaniline/carbon foam composite: putting into dispersion after dry carbon foam is fully absorbed dispersion liquid B
In liquid A, under ice/water mixture, magnetic agitation is carried out with the revolving speed of 200r/min and continues 6h.After the completion, foam is filtered out simultaneously
With deionized water and ethanol washing until washing lotion is transparent.Finally, the low temperature by polyaniline/carbon foam (PANI/CF) at -50 DEG C
Precooling 2h in refrigerator, is subsequently placed in vacuum freeze drier and is freeze-dried 36h, obtains polyaniline/carbon foam composite.
Advantages of the present invention: the present invention makes carbon foam obtained by melamine foamed plastic surface carbonation using high-temperature calcination
It not only can increase electromagnetic wave in internal reflection to increase the loss to electromagnetic wave with tridimensional network, reduce simultaneously
Sheet resistance is conducive to improve its dielectric loss ability and to be conducive to polyaniline in situ in the polymerization on its surface, and then improves to electricity
The loss and absorption of magnetic wave.
Polyaniline/carbon foam composite prepared by the present invention can be in 6.0-18GHz frequency range when deformation occurs
Absorption of the interior realization to 90% electromagnetic wave, has reflection loss minimum -47.26 when with a thickness of 4.0mm at 9.86GHz.
Polyaniline/carbon foam composite prepared by the present invention can be applicable to controllable absorbing material field.
Embodiment 4:
The present embodiment is a kind of preparation method of polyaniline nano ring with absorbing property, the present embodiment and implementation
Unlike example 3: using oxidant being iron chloride in step (2), other steps are identical.
Embodiment 5:
Embodiment is a kind of preparation method of polyaniline nano ring with absorbing property, the present embodiment and embodiment
Unlike 2: for the Bronsted acid used in step (2) for 0.6mol hydrochloric acid, other steps are identical.
Embodiment 6:
The present embodiment be a kind of polyaniline/carbon foam composite preparation method with controllable absorbing property, by with
Lower step carries out:
(1) it prepares carbon foam: clean melamine foamed plastic being calcined in resistance furnace: after 500 DEG C of calcining at constant temperature 5h
It is gradually cooling to room temperature.Whole process carries out under nitrogen protection.It takes out and is placed in the concentrated sulfuric acid after foam is cooled to room temperature
15min is impregnated, then is washed repeatedly with deionized water to neutrality, and the dry 12h in 50 DEG C of vacuum drying oven；
(2) it prepares dispersion liquid A: weighing p-methyl benzenesulfonic acid 0.01mol, iron chloride 0.05mol is added to the water, p-methyl benzenesulfonic acid
Concentration control be 0.1mol/L；Under 100W power, ultrasonic disperse 45min keeps p-methyl benzenesulfonic acid and iron chloride fully dispersed
In water；
(3) prepare dispersion liquid B: ultrasonic disperse aniline (An) in water obtains the An dispersion liquid that concentration is 0.01mol/L,
By An dispersion liquid ultrasonic disperse in mixture of ice and water, ultrasonic power 100W, ultrasonic time 12min；
(4) it prepares polyaniline/carbon foam composite: putting into dispersion after dry carbon foam is fully absorbed dispersion liquid B
In liquid A, under ice/water mixture, magnetic agitation is carried out with the revolving speed of 400r/min and continues 4h.After the completion, foam is filtered out simultaneously
With deionized water and ethanol washing until washing lotion is transparent.Finally, the low temperature by polyaniline/carbon foam (PANI/CF) at -10 DEG C
Precooling for 24 hours, is subsequently placed in vacuum freeze drier in refrigerator, and controlled at -8 DEG C, vacuum degree is 1pa freeze-drying
36h obtains polyaniline/carbon foam composite.
Embodiment 7:
The present embodiment be a kind of polyaniline/carbon foam composite preparation method with controllable absorbing property, by with
Lower step carries out:
(1) it prepares carbon foam: clean melamine foamed plastic being calcined in resistance furnace: after 800 DEG C of calcining at constant temperature 2h
It is gradually cooling to room temperature.Whole process carries out under nitrogen protection.It takes out and is placed in the concentrated sulfuric acid after foam is cooled to room temperature
15min is impregnated, then is washed repeatedly with deionized water to neutrality, and the dry 12h in 50 DEG C of vacuum drying oven；
(2) it prepares dispersion liquid A: weighing salicylic acid 1mol, potassium bichromate 0.1mol is added to the water, the concentration of p-methyl benzenesulfonic acid
Control is 1mol/L；Under 400W power, ultrasonic disperse 30min keeps salicylic acid and potassium bichromate fully dispersed in water；
(3) prepare dispersion liquid B: ultrasonic disperse aniline (An) in water obtains the An dispersion liquid that concentration is 0.1mol/L,
By An dispersion liquid ultrasonic disperse in mixture of ice and water, ultrasonic power 300W, ultrasonic time 10min；
(4) it prepares polyaniline/carbon foam composite: putting into dispersion after dry carbon foam is fully absorbed dispersion liquid B
In liquid A, under ice/water mixture, magnetic agitation is carried out with the revolving speed of 500r/min and continues 3h.After the completion, foam is filtered out simultaneously
With deionized water and ethanol washing until washing lotion is transparent.Finally, the low temperature by polyaniline/carbon foam (PANI/CF) at -20 DEG C
Precooling 18h in refrigerator, is subsequently placed in vacuum freeze drier, and controlled at -20 DEG C, vacuum degree is 5pa freeze-drying
For 24 hours, polyaniline/carbon foam composite is obtained.
Embodiment 8:
The present embodiment be a kind of polyaniline/carbon foam composite preparation method with controllable absorbing property, by with
Lower step carries out:
(1) it prepares carbon foam: clean melamine foamed plastic being calcined in resistance furnace: in 900 DEG C of calcining at constant temperature 90min
After be gradually cooling to room temperature.Whole process carries out under nitrogen protection.It is taken out after foam is cooled to room temperature and is placed in the concentrated sulfuric acid
Middle immersion 10min, then washed repeatedly with deionized water to neutrality, and dried for 24 hours in 50 DEG C of vacuum drying oven；
(2) it prepares dispersion liquid A: weighing p-methyl benzenesulfonic acid 8mol, potassium bichromate 0.1mol is added to the water, p-methyl benzenesulfonic acid
Concentration control is 8mol/L；Under 1000W power, ultrasonic disperse 10min is well dispersed in p-methyl benzenesulfonic acid and potassium bichromate
In water；
(3) prepare dispersion liquid B: ultrasonic disperse aniline (An) in water obtains the An dispersion liquid that concentration is 5mol/L, will
An dispersion liquid ultrasonic disperse is in mixture of ice and water, ultrasonic power 1000W, ultrasonic time 1min；
(4) it prepares polyaniline/carbon foam composite: putting into dispersion after dry carbon foam is fully absorbed dispersion liquid B
In liquid A, under ice/water mixture, magnetic agitation is carried out with the revolving speed of 2000r/min and continues 1h.After the completion, foam is filtered out simultaneously
With deionized water and ethanol washing until washing lotion is transparent.Finally, the low temperature by polyaniline/carbon foam (PANI/CF) at -90 DEG C
Precooling 2h in refrigerator, is subsequently placed in vacuum freeze drier, and controlled at -60 DEG C, vacuum degree is 15pa freeze-drying
1h obtains polyaniline/carbon foam composite.
Embodiment 9:
The present embodiment be a kind of polyaniline/carbon foam composite preparation method with controllable absorbing property, by with
Lower step carries out:
(1) it prepares carbon foam: clean melamine foamed plastic being calcined in resistance furnace: in 950 DEG C of calcining at constant temperature 60min
After be gradually cooling to room temperature.Whole process carries out under nitrogen protection.It is taken out after foam is cooled to room temperature and is placed in the concentrated sulfuric acid
Middle immersion 10min, then washed repeatedly with deionized water to neutrality, and dried for 24 hours in 50 DEG C of vacuum drying oven；
(2) prepare dispersion liquid A: weighing hydrochloric acid 0.5mol, potassium bichromate 0.05mol is added to the water, p-methyl benzenesulfonic acid it is dense
Degree control is 6mol/L；Under 500W power, ultrasonic disperse 30min keeps hydrochloric acid and potassium bichromate fully dispersed in water；
(3) prepare dispersion liquid B: ultrasonic disperse aniline (An) in water obtains the An dispersion liquid that concentration is 2mol/L, will
An dispersion liquid ultrasonic disperse is in mixture of ice and water, ultrasonic power 500W, ultrasonic time 5min；
(4) it prepares polyaniline/carbon foam composite: putting into dispersion after dry carbon foam is fully absorbed dispersion liquid B
In liquid A, under ice/water mixture, magnetic agitation is carried out with the revolving speed of 1000r/min and continues 3h.After the completion, foam is filtered out simultaneously
With deionized water and ethanol washing until washing lotion is transparent.Finally, the Low-temperature Ice by polyaniline/carbon foam (PANI/CF) at -60 DEG C
Precooling 6h in case, is subsequently placed in vacuum freeze drier, and controlled at -40 DEG C, vacuum degree is that 10pa is freeze-dried 5h,
Obtain polyaniline/carbon foam composite.
Embodiment 10:
Using following experimental verifications effect of the invention:
One, it prepares carbon foam: clean melamine foamed plastic being calcined in resistance furnace: in 950 DEG C of calcining at constant temperature 2.5h
After be gradually cooling to room temperature.Whole process carries out under nitrogen protection.It is taken out after foam is cooled to room temperature and is placed in the concentrated sulfuric acid
Middle immersion 15min, then washed repeatedly with deionized water to neutrality, and the dry 12h in 50 DEG C of vacuum drying oven；
Two, it prepares dispersion liquid A: weighing p-methyl benzenesulfonic acid 0.02mol, ammonium persulfate 0.02mol is added in 360ml water；?
Under 500W power, ultrasonic disperse 45min keeps Bronsted acid and oxidant fully dispersed in water；
Three, prepare dispersion liquid B: the ultrasonic disperse 0.03mol aniline (An) in 10ml water obtains An dispersion liquid, by An points
Dispersion liquid ultrasonic disperse is in mixture of ice and water, ultrasonic power 300W, ultrasonic time 12min；
Four, it prepares polyaniline/carbon foam composite: putting into dispersion after dry carbon foam is fully absorbed dispersion liquid B
In liquid A, under ice/water mixture, magnetic agitation is carried out with the revolving speed of 200r/min and continues 6h.After the completion, foam is filtered out simultaneously
With deionized water and ethanol washing until washing lotion is transparent.Finally, the low temperature by polyaniline/carbon foam (PANI/CF) at -50 DEG C
Precooling 2h in refrigerator, is subsequently placed in vacuum freeze drier and is freeze-dried 36h, obtains polyaniline/carbon foam composite,
It is named as PANI/CF.
Existed using polyaniline/carbon foam composite with absorbing property that Agilent N5224A tests this experiment preparation
Electromagnetic parameter under different deformation brings suction wave loss formula into and obtains its reflection damage under different deformation degree under each thickness
Consumption, wherein Fig. 1 is PANI/CF deformation occurs lower absorbing property figure, and Fig. 2 is PANI/CF wave absorbtion in deformation 15%
It can scheme, Fig. 3 is the absorbing property figure of PANI/CF deformation 30%, and Fig. 4 is the absorbing property figure of PANI/CF deformation 45%.(in figure
0.5,1,1.5,2,2.5,3,3.5,4,4.5,5 suction wave profiles under the simulated thickness representated by corresponding number respectively)
By known to Fig. 1-Fig. 4 polyaniline/carbon foam composite wave reflection loss can for-69.76dB~-
Regulated and controled between 20.49dB, effectively inhales that wavestrip is wide to be regulated and controled between 3.10-6.25GHz.
In the description of this specification, the description of reference term " one embodiment ", " example ", " specific example " etc. means
Particular features, structures, materials, or characteristics described in conjunction with this embodiment or example are contained at least one implementation of the invention
In example or example.In the present specification, schematic expression of the above terms may not refer to the same embodiment or example.
Moreover, particular features, structures, materials, or characteristics described can be in any one or more of the embodiments or examples to close
Suitable mode combines.
The above description of the embodiments is intended to facilitate ordinary skill in the art to understand and use the invention.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, ability
Field technique personnel announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be of the invention
Within protection scope.
Claims (10)
1. polyaniline/carbon foam composite preparation method with controllable absorbing property, which is characterized in that this method packet
It includes:
Clean melamine foamed plastic is cooled to room temperature after calcination processing, taking-up, which is placed in the concentrated sulfuric acid, impregnates, then spend from
Sub- water is washed repeatedly to neutrality, obtains carbon foam through being dried；
Bronsted acid, oxidant is fully dispersed in water, obtain dispersion liquid A；
Aniline is dispersed in water to obtain aniline dispersion liquid, which is redispersed in mixture of ice and water, dispersion liquid is obtained
B；
It is put into dispersion liquid A after carbon foam is fully absorbed dispersion liquid B, is stirred under ice/water mixture, filter out foam and spend
Until washing lotion is transparent, polyaniline/carbon bubble is prepared in vacuum freeze drying again after pre-cooled jelly processing for ionized water and ethanol washing
Foam composite material.
2. polyaniline/carbon foam composite preparation method according to claim 1 with controllable absorbing property,
It is characterized in that, the melamine foamed plastic handles 1-5h in 500-950 DEG C of temperature lower calcination.
3. polyaniline/carbon foam composite preparation side according to claim 1 or 2 with controllable absorbing property
Method, which is characterized in that preferred 800-900 DEG C of the melamine foamed plastic calcination processing temperature, time preferred 90-120min.
4. polyaniline/carbon foam composite preparation method according to claim 1 with controllable absorbing property,
It is characterized in that, the Bronsted acid includes hydrochloric acid, p-methyl benzenesulfonic acid or salicylic acid.
5. polyaniline/carbon foam composite preparation method according to claim 1 with controllable absorbing property,
It is characterized in that, the oxidant includes ammonium persulfate, iron chloride or potassium bichromate.
6. polyaniline/carbon foam composite preparation according to claim 1 or 4 or 5 with controllable absorbing property
Method, which is characterized in that the molar ratio of the Bronsted acid and the oxidant is 0.01-8:0.02-0.1, and Bronsted acid is in water
Concentration be 0.1-8mol/L.
7. polyaniline/carbon foam composite preparation according to claim 1 or 4 or 5 with controllable absorbing property
Method, which is characterized in that in water, ultrasonic power 100-1000W, the time controls for the Bronsted acid, oxidant ultrasonic disperse
In 10-45min.
8. polyaniline/carbon foam composite preparation method according to claim 1 with controllable absorbing property,
It is characterized in that, the aniline forms the aniline dispersion liquid that concentration is 0.01-5mol/L through ultrasonic disperse, then through ultrasonic disperse in ice
In aqueous mixtures, ultrasonic power 100-1000W, the time is controlled in 1-12min.
9. polyaniline/carbon foam composite preparation method according to claim 1 with controllable absorbing property,
It is characterized in that, it is that 200-2000rpm carries out magnetic agitation 1-6h that the carbon foam controls mixing speed in ice/water mixture.
10. polyaniline/carbon foam composite preparation method according to claim 1 with controllable absorbing property,
It is characterized in that, in -10--90 DEG C of at a temperature of precooling 1-24h when the precooling is handled；The vacuum freeze drying is
In vacuum freeze drier, -8--60 DEG C, vacuum degree 1-15pa, freeze-drying 1-36h.
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| CN115041144B (en) * | 2022-05-23 | 2024-05-03 | 广州大学 | Polyaniline nitrogen-doped carbon foam, preparation method and application |
| CN115041144A (en) * | 2022-05-23 | 2022-09-13 | 广州大学 | Polyaniline nitrogen-doped carbon foam, preparation method and application |
| CN115386337A (en) * | 2022-08-12 | 2022-11-25 | 许昌学院 | Chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material and preparation method thereof |
| CN115386337B (en) * | 2022-08-12 | 2023-09-08 | 许昌学院 | Chiral polyaniline/biomass derived porous carbon composite wave-absorbing material and preparation method thereof |
| CN115651606B (en) * | 2022-12-14 | 2023-09-19 | 中南大学 | Three-dimensional metal organic framework derivative/carbon foam composite wave-absorbing material and preparation method thereof |
| CN115651606A (en) * | 2022-12-14 | 2023-01-31 | 中南大学 | Three-dimensional metal organic framework derivative/carbon foam composite wave-absorbing material and preparation method thereof |
| CN116322008A (en) * | 2023-02-23 | 2023-06-23 | 之江实验室 | Hollow-structure rGO wave-absorbing material and preparation method and application thereof |
| CN116322008B (en) * | 2023-02-23 | 2023-11-10 | 之江实验室 | Hollow-structure rGO wave-absorbing material and preparation method and application thereof |
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