CN107325787A - A kind of hollow carbon nano-particle and the absorbing material prepared by it - Google Patents
A kind of hollow carbon nano-particle and the absorbing material prepared by it Download PDFInfo
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- CN107325787A CN107325787A CN201710541808.4A CN201710541808A CN107325787A CN 107325787 A CN107325787 A CN 107325787A CN 201710541808 A CN201710541808 A CN 201710541808A CN 107325787 A CN107325787 A CN 107325787A
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Abstract
The absorbing material prepared the invention provides a kind of hollow carbon nano-particle and by it.The preparation method of hollow carbon nano-particle includes：Aniline, pyrroles, nonionic surfactant and water are mixed, the first solution is obtained；Added after ammonium persulfate solution is carried out into ice bath in the first solution, obtain the second solution；Suction filtration, washing, freeze-drying, obtain head product after second solution is reacted；Head product is subjected to carbonization treatment, hollow carbon nano-particle is obtained.The preparation method of absorbing material includes：Graphene, hollow carbon nano-particle and polypropylene are added into banburying in torque rheometer, mixture is obtained；Mixture is subjected to hot pressing, cold pressing, absorbing material is obtained.The technical scheme that the present invention is provided is using graphene and hollow carbon nano-particle as suction ripple medium, polypropylene is carrier, obtained absorbing material can not only reach effective absorption to electromagnetic wave, while being also integrated with the series of advantages such as the small, endurance of polypropylene material density.
Description
Technical field
The absorbing material prepared the present invention relates to a kind of hollow carbon nano-particle and by it, belongs to macromolecule composite wood
Expect technical field.
Background technology
Absorbing material refers to absorb, the electromagnetic wave for the incidence that decays, and by its incident electromagnetic energy into thermal dissipation
The material for falling or making electromagnetic wave to be disappeared by interference, is a kind of important functional material, in electronic product, stealth technology, microwave
Communication, microwave dark room, anti-electromagnetic-radiation and prevent from being widely used in terms of electromagnetic pollution.Therefore, to inhaling ripple material
The exploitation of material is most important.
In recent years, the demand to absorbing material constantly increases, and the effect of electromagnetic wave absorbent material and status are increasingly protruded,
The magnetic density of material such as traditional ferrite is larger, is easily oxidized, therefore exploitation high-performance composite wave-suction material is significant.
Electromagnetic-wave absorbent is prepared using graphene mainly pass through oxidation-reduction method, chemical vapor deposition in the prior art
The methods such as method (CVD), but this method presence can not realize the shortcomings of volume production or preparation process produce a large amount of pollutants, nothing
Method reaches the requirement of green non-pollution, and can not industrially realize volume production.
Therefore it provides a kind of simple and easy to apply, green non-pollution, and can the method for preparing absorbing material of industrial production turn into
This area technical problem urgently to be resolved hurrily.
The content of the invention
In order to solve the above technical problems, it is an object of the invention to provide a kind of hollow carbon nano-particle and its preparation side
Method；Its unique hollow structure of the hollow carbon nano-particle that the present invention is provided can cause the electromagnetic wave of incidence to be formed in cavity
Multipath reflection, can greatly lift the absorbing property of absorbing material.
Present invention also offers a kind of absorbing material prepared by above-mentioned hollow carbon nano-particle.
To reach above-mentioned purpose, the invention provides a kind of preparation method of hollow carbon nano-particle, it includes following step
Suddenly：
Aniline, pyrroles, nonionic surfactant and water are mixed, the first solution is obtained；
Added after ammonium persulfate solution is carried out into ice bath in first solution, obtain the second solution；
Second solution is reacted into 8-16h at 0-5 DEG C, suction filtration, washing, freeze-drying is then carried out, obtains primiparity
Thing；
The head product is subjected to carbonization treatment, hollow carbon nano-particle is obtained.The shape of the hollow carbon nano-particle
It is substantially spherical in shape, therefore hollow Nano carbon balls can also be referred to as.
In the above-mentioned methods, it is preferable that the aniline, pyrroles, the ratio of nonionic surfactant and water are 0.76mL:
0.58mL:(0.04-0.16)g:120mL。
In a detailed embodiment, when aniline, pyrroles, nonionic surfactant and water being mixed, aniline plus
Enter amount for 0.76mL, the addition of pyrroles is 0.58mL, and the addition of nonionic surfactant is (0.04-0.16) g, water
Addition is 120mL.
In the above-mentioned methods, it is preferable that the nonionic surfactant is the triton x-100 (triton x-100
Also referred to as emulsifying agent TX-100, its English entitled Triton X-100).
In the above-mentioned methods, it is preferable that when mixing aniline, pyrroles, nonionic surfactant and water, the water is to go
Ionized water.
In the above-mentioned methods, it is preferable that this method to first solution also including being stirred, the step of ultrasonic and ice bath
Suddenly；It is highly preferred that when carrying out ice bath to first solution, the temperature of the ice bath is 0-5 DEG C, the time of the ice bath is
30-50min。
In the above-mentioned methods, it is preferable that the ammonium persulfate solution is dissolved in after deionized water by ammonium persulfate to be obtained,
Wherein, the ratio of the ammonium persulfate and the water is 3.8g:30mL.
In the above-mentioned methods, it is preferable that when ammonium persulfate solution is carried out into ice bath, the temperature of the ice bath is 0-5 DEG C, institute
The time for stating ice bath is 30-50min.
In the above-mentioned methods, it is preferable that the washing includes procedure below：By second alcohol and water according to volume ratio be 1:(3-
5) proportions are into ethanol solution；Reacted solution is washed using the ethanol solution.
In the above-mentioned methods, the temperature of the freeze-drying is general at subzero 50 DEG C or so.
In the above-mentioned methods, it is preferable that the temperature of the carbonization treatment is 700-900 DEG C；It is highly preferred that at the carbonization
The atmosphere of reason is nitrogen or argon gas；It is further preferred that when carrying out carbonization treatment, it is 3 DEG C/min to control heating rate.
Present invention also offers a kind of hollow carbon nano-particle prepared by the above method.
To reach above-mentioned purpose, present invention also offers a kind of preparation method of absorbing material, this method includes following step
Suddenly：
Graphene, hollow carbon nano-particle and polypropylene are added in torque rheometer, in banburying 10- at 190-220 DEG C
20min, obtains mixture；
By the mixture under conditions of 190-220 DEG C, 15-20MPa hot pressing 5-10min, then in room temperature, 20-
5-8min is cold-pressed under conditions of 25MPa, absorbing material is obtained.The absorbing material is graphene, hollow carbon nano-particle and poly- third
The compound of alkene.
The technical scheme that the present invention is provided is using polypropylene as carrier, and graphene and hollow carbon nanomaterial are situated between effectively to inhale ripple
Matter prepares absorbing material.Wherein, on the one hand the addition of hollow carbon nano-particle can reduce the quality of compound, the opposing party
Its unique hollow structure of face can make the electromagnetic wave of incidence form multipath reflection in cavity, on the basis of graphene greatly
Ground lifts the absorbing property of compound；In addition, being used as carrier using polypropylene so that the absorbing material prepared is not only integrated with
Polypropylene material density is small, endurance, resistant to chemical etching, stress crack resistant and the advantages of be easy to processing and forming, and also functions to
The effect of the high value added utilization of the polypropylene material produced to refinery.
In the above-mentioned methods, the banburying is one of major function of the torque rheometer.
In the above-mentioned methods, it is preferable that the graphene, hollow carbon nano-particle are with the polyacrylic mass ratio
1:(4-6):19.The mass fraction of graphene, which crosses conference, causes absorbing material electric conductivity very good, increases the reflection to electromagnetic wave,
So as to be unfavorable for absorbing；It is too small, the absorption loss scarce capacity of absorbing material can be caused, it is impossible to realize to incident electromagnetic wave
Effectively absorb, this mass ratio provided using the present invention, the mass fraction of graphene powder can be made to control optimum
In the range of, so as to ensure the assimilation effect to electromagnetic wave；In addition, the quality control of hollow carbon nano-particle is that this ratio can be with
Greatly lift the absorbing property of material.
In the above-mentioned methods, it is preferable that in internal mixing pass, the rotating speed of the torque rheometer is 30-50r/min.Adopt
It is able to ensure that graphene and hollow carbon nano-particle are uniformly dispersed in polypropylene with this rotating speed, rotating speed can in practical operation
To be adjusted according to temperature, when temperature is higher, the viscosity of mixture is smaller, and now rotating speed can be relatively smaller.
In the above-mentioned methods, it is preferable that the graphene is prepared by ball-milling method, it is powder morphology；It is more excellent
Selection of land, during using ball-milling method, the time for controlling ball milling is 48-96h.
Present invention research finds that the defect and crystallinity of graphene have important shadow to the assimilation effect of final absorbing material
Ring, the defect of graphene is few, crystallinity is high-leveled and difficult with preferably electromagnetic wave absorption, and Ball-milling Time is less than 48h, the graphite prepared
Alkene product defects is few, crystallinity is high, it is impossible to obtain desired technique effect, and the Ball-milling Time provided using the present invention can not only
Enough ensure to obtain the graphene product that defect is more, crystallinity is low, graphene powder is obtained in polypropylene material preferably
Dispersion effect, and can effectively strengthen absorbability of the graphene to electromagnetic wave.
In the above-mentioned methods, it is preferable that the preparation process of the ball-milling method is as follows：
The metal ball of graphite raw material and ball milling is placed in ball grinder and carries out ball milling, Ball-milling Time is 48-96h, is obtained
Graphene powder.
In the above-mentioned methods, it is preferable that the graphite raw material includes crystalline flake graphite and/or expanded graphite.
In the above-mentioned methods, it is preferable that the instrument that the hot pressing and the cold pressing are used is vulcanizing press.
In a detailed embodiment, this method comprises the following steps：
The metal ball of graphite raw material and ball milling is placed in ball grinder and carries out ball milling, Ball-milling Time is 48-96h, is obtained
Graphene powder；Wherein, the graphite raw material includes crystalline flake graphite and/or expanded graphite；
By graphene, hollow carbon nano-particle and polypropylene according to mass ratio be 1:4:19 ratio adds torque rheology
In instrument, at 190 DEG C, banburying 10-20min under conditions of 30-50r/min obtains mixture；
By the mixture under conditions of 190-220 DEG C, 15-20MPa hot pressing 5-10min, then then at room temperature, 20-
5min is cold-pressed under conditions of 25MPa, absorbing material is obtained.
Present invention also offers a kind of absorbing material prepared by the above method, the absorbing material be graphene, in
Empty carbon nano-particle and polyacrylic compound.
Beneficial effects of the present invention：
1) the hollow carbon nano particle diameter that the technical scheme that provides of the present invention is prepared is uniform and hollow pattern substantially,
The quality of compound on the one hand can be reduced using it as ripple medium is inhaled, on the other hand its unique hollow structure can make incidence
Electromagnetic wave multipath reflection is formed in cavity, the absorbing property of compound is greatly lifted on the basis of graphene；
2) technical scheme that the present invention is provided prepares graphene powder using ball-milling method, by controlling Ball-milling Time to obtain
Preferable graphene powder (defect is more, crystallinity is low), improves the assimilation effect to electromagnetic wave；In addition, ball-milling method can be real
The industrial volume production of existing graphene powder；
3) absorbing material that the technical scheme that the present invention is provided is prepared can not only reach effective suction to electromagnetic wave
Receive, but also be integrated with small polypropylene material density, endurance, resistant to chemical etching, stress crack resistant and be easy to processing and forming etc.
Advantage；In addition, the utilization added value of polypropylene product is greatly improved；
4) technical scheme that the present invention is provided can be by controlling the size of mould to prepare the absorbing material of arbitrary dimension.
Brief description of the drawings
Fig. 1 is the transmission electron microscope picture for the hollow carbon nano-particle that embodiment 1 is provided；
Fig. 2 is the TEM figures of graphene powder in embodiment 2；
Fig. 3 is the Raman spectrogram of graphene powder in embodiment 2；
Fig. 4 be embodiment 2 in absorbing material 2-18GHz reflection loss figure；
Fig. 5 be comparative example 1 in absorbing material 2-18GHz reflection loss figure.
Embodiment
In order to which technical characteristic, purpose and beneficial effect to the present invention are more clearly understood from, now to the skill of the present invention
Art scheme carry out it is described further below, but it is not intended that to the present invention can practical range restriction.
Embodiment 1
A kind of preparation method of hollow carbon nano-particle is present embodiments provided, this method comprises the following steps：
0.76mL aniline, 0.58mL pyrroles and 0.06g nonionic surface active agent triton x-100s are added to
In 120mL deionized water, 0.5h, ultrasonic 0.5h are stirred, then ice bath 0.5h again, (this is molten to form as clear as crystal solution
Liquid is designated as the first solution)；Wherein, the temperature of ice bath is 0 DEG C.
3.8g ammonium persulfates are dissolved in 30mL deionized water ammonium persulfate solution is made, ice bath 0.5h be (ice bath
Temperature is 0 DEG C)；Then it is disposably added in above-mentioned first solution, during addition, added while stirring, mixing time is about
For 30 seconds, the second solution is obtained.
Above-mentioned second solution is reacted into 12h at 0 DEG C, reaction utilizes Vacuum filtration device after terminating, with ethanol solution (second
Alcohol：Water=1:3, volume ratio) reacted solution is cleaned, untill filtrate water white transparency, filter cake is then collected, will
The filter cake being collected into is freeze-dried 48 hours, obtains powder sample.
Powder sample obtained above is placed in horizontal tube heating furnace and carries out carbonization treatment, carburizing temperature is 800 DEG C,
Heating rate is 3 DEG C/min, and carburizing atmosphere is nitrogen or argon gas, finally obtains hollow carbon powder of nanometric particles sample.
The transmission electron microscope picture for the hollow carbon nano-particle that the present embodiment is provided is as shown in Figure 1.As can be seen from the figure：This reality
The hollow carbon nano-particle for applying example offer is substantially spherical in shape, uniform particle sizes and hollow pattern is obvious.
Embodiment 2
A kind of absorbing material is present embodiments provided, the preparation process of the absorbing material is as follows：
Prepare graphene powder
Under room temperature condition of normal pressure, the metal ball of 100g crystalline flake graphites and ball milling is put into ball grinder, ball milling 96h,
Obtain the sample that graphite flake is stripped into graphene powder.The TEM of the graphene powder is schemed as shown in Fig. 2 as can be seen from Figure
The number of plies is less, about 8 layers.The Raman spectrograms of the graphene powder are as shown in Figure 3, it can be seen that have obvious D peaks, explanation
Defect is more in graphene product.
Prepare absorbing material
The hollow carbon nano-particle and polypropylene that graphene powder obtained above, embodiment 1 are provided are according to mass ratio
For 1:4:19 ratio is added in torque rheometer, at 190 DEG C, and banburying 20min under conditions of 50r/min obtains mixture；
By said mixture on vulcanizing press at 190 DEG C, hot pressing 10min under conditions of 20MPa, then in room
5min is cold-pressed under conditions of temperature, 25MPa, absorbing material is obtained.The size of the absorbing material is up to 10cm*10cm*2mm, specifically
The size of absorbing material can be controlled in implementation process by adjusting the size of mould.
The absorbing material that the present embodiment is provided is as shown in Figure 4 in 2-18GHz reflection loss.
Embodiment 3
A kind of absorbing material is present embodiments provided, the preparation process of the absorbing material is as follows：
Prepare graphene powder
Under room temperature condition of normal pressure, the metal ball of 10g crystalline flake graphites and ball milling is put into ball grinder, ball milling 48h is obtained
The sample of graphene powder is stripped into graphite flake.
Prepare absorbing material
The hollow carbon nano-particle and polypropylene that graphene powder obtained above, embodiment 1 are provided are according to mass ratio
For 1:4:19 ratio is added in torque rheometer, at 220 DEG C, the banburying 10min (rotating speeds of banburying under conditions of 30r/min
With time and temperature into inverse correlation relation.Temperature is higher, the viscosity of mixture it is smaller, it is necessary to rotating speed and the time it is also smaller), obtain
To mixture；
By said mixture on vulcanizing press at 190 DEG C, hot pressing 8min under conditions of 15MPa, then in room temperature,
5min is cold-pressed under conditions of 20MPa, absorbing material is obtained.
Comparative example 1
This comparative example provides a kind of absorbing material, and the preparation process of the absorbing material is as follows：
Prepare graphene powder, preparation process be the same as Example 2；
Prepare absorbing material
According to mass ratio it is 1 by graphene powder obtained above and polypropylene:9 ratio is added to torque rheometer
In, at 190 DEG C, banburying 20min under conditions of 50r/min obtains mixture；
By said mixture on vulcanizing press at 190 DEG C, hot pressing 10min under conditions of 20MPa, then in room
5min is cold-pressed under conditions of temperature, 25MPa, absorbing material is obtained, the absorbing material is graphene/polypropylene composite.The suction ripple
The size of material can control to inhale ripple material up to 10cm*10cm*2mm in specific implementation process by adjusting the size of mould
The size of material.
The absorbing material that the present embodiment is provided is as shown in Figure 5 in 2-18GHz reflection loss.
Comparative example 2
This comparative example provides a kind of absorbing material, and the preparation process of the absorbing material is as follows：
Prepare graphene powder, preparation process be the same as Example 3；
Prepare absorbing material
According to mass ratio it is 1 by graphene powder obtained above and polypropylene:19 ratio is added to torque rheometer
In, at 220 DEG C, (rotating speed of banburying and time and temperature are into inverse correlation relation by banburying 10min under conditions of 30r/min.Temperature is got over
Height, the viscosity of mixture it is smaller, it is necessary to rotating speed and the time it is also smaller), obtain mixture；
By said mixture on vulcanizing press at 190 DEG C, hot pressing 8min under conditions of 15MPa, then in room temperature,
5min is cold-pressed under conditions of 20MPa, absorbing material is obtained, the absorbing material is graphene/polypropylene composite.
From embodiment 2 provide absorbing material 2-18GHz reflection loss figure (Fig. 4) and comparative example 1 offer suction
Wave material can be seen that in 2-18GHz reflection loss figure (Fig. 5)：Embodiment 2 adds maximum suction after hollow carbon nano-particle
- 50dB or so can be promoted to from -20dB of polypropylene/graphene complex or so by receiving peak.
Claims (12)
1. a kind of preparation method of hollow carbon nano-particle, it comprises the following steps：
Aniline, pyrroles, nonionic surfactant and water are mixed, the first solution is obtained；
Added after ammonium persulfate solution is carried out into ice bath in first solution, obtain the second solution；
Second solution is reacted into 8-16h at 0-5 DEG C, suction filtration, washing, freeze-drying is then carried out, obtains head product；
The head product is subjected to carbonization treatment, hollow carbon nano-particle is obtained.
2. according to the method described in claim 1, wherein, the aniline, pyrroles, the ratio of nonionic surfactant and water are
0.76mL:0.58mL:(0.04-0.16)g:120mL；
Preferably, the nonionic surfactant is triton x-100；
It is highly preferred that when aniline, pyrroles, nonionic surfactant and water are mixed, the water is deionized water.
3. according to the method described in claim 1, wherein, this method also include first solution is stirred, ultrasound and
The step of ice bath；
Preferably, when carrying out ice bath to first solution, the temperature of the ice bath is 0-5 DEG C, and the time of the ice bath is 30-
50min。
4. according to the method described in claim 1, wherein, the ammonium persulfate solution is to be dissolved in by ammonium persulfate after deionized water
Obtain；
It is highly preferred that the ratio of the ammonium persulfate and the deionized water is 3.8g:30mL.
5. according to the method described in claim 1, wherein, by ammonium persulfate solution carry out ice bath when, the temperature of the ice bath is
0-5 DEG C, the time of the ice bath is 30-50min.
6. according to the method described in claim 1, wherein, the temperature of the carbonization treatment is 700-900 DEG C；
Preferably, the atmosphere of the carbonization treatment is nitrogen or argon gas.
7. the hollow carbon nano-particle that the method described in claim any one of 1-6 is prepared.
8. a kind of preparation method of absorbing material, this method comprises the following steps：
Hollow carbon nano-particle described in graphene, claim 7 and polypropylene are added in torque rheometer, in 190-220
Banburying 10-20min at DEG C, obtains mixture；
By the mixture under conditions of 190-220 DEG C, 15-20MPa hot pressing 5-10min, then in room temperature, 20-25MPa
Under the conditions of be cold-pressed 5-8min, obtain absorbing material.
9. method according to claim 8, wherein, the graphene, the hollow carbon nano-particle with it is described polyacrylic
Mass ratio is 1:(4-6):19.
10. method according to claim 8, wherein, in internal mixing pass, the rotating speed of the torque rheometer is 30-
50r/min。
11. method according to claim 8, wherein, the graphene is prepared by ball-milling method；
When preferably, using ball-milling method, the time for controlling ball milling is 48-96h.
12. the absorbing material prepared as the method described in claim any one of 8-11.
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| CN108439369A (en) * | 2018-04-12 | 2018-08-24 | 深圳大学 | Hollow carbon nanometer micro ball of nitrogen oxygen codope and its preparation method and application |
| CN108448101A (en) * | 2018-04-12 | 2018-08-24 | 深圳大学 | Lithium sulfur battery anode material and its preparation method and application |
| CN108865061A (en) * | 2018-07-14 | 2018-11-23 | 合肥艾飞新材料有限公司 | A kind of hollow plumbago alkene microballoon and preparation method thereof |
| CN109879635A (en) * | 2019-04-15 | 2019-06-14 | 苏州安洁新材料有限公司 | A kind of ultra-thin high magnetic permeability inhales wave plate and its casting slurry and preparation method |
| CN110041886A (en) * | 2019-05-21 | 2019-07-23 | 常州威斯双联科技有限公司 | A kind of novel graphene absorbing material and preparation method |
| CN110060834A (en) * | 2019-05-16 | 2019-07-26 | 常州威斯双联科技有限公司 | Magnetically soft alloy powder inhales wave plate, preparation method, electronic component and electronic equipment |
| CN110487866A (en) * | 2019-09-19 | 2019-11-22 | 西北师范大学 | A kind of application of Porous hollow Nano carbon balls material prepared and its detect nitrite |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108439369A (en) * | 2018-04-12 | 2018-08-24 | 深圳大学 | Hollow carbon nanometer micro ball of nitrogen oxygen codope and its preparation method and application |
| CN108448101A (en) * | 2018-04-12 | 2018-08-24 | 深圳大学 | Lithium sulfur battery anode material and its preparation method and application |
| CN108865061A (en) * | 2018-07-14 | 2018-11-23 | 合肥艾飞新材料有限公司 | A kind of hollow plumbago alkene microballoon and preparation method thereof |
| CN109879635A (en) * | 2019-04-15 | 2019-06-14 | 苏州安洁新材料有限公司 | A kind of ultra-thin high magnetic permeability inhales wave plate and its casting slurry and preparation method |
| CN110060834A (en) * | 2019-05-16 | 2019-07-26 | 常州威斯双联科技有限公司 | Magnetically soft alloy powder inhales wave plate, preparation method, electronic component and electronic equipment |
| CN110060834B (en) * | 2019-05-16 | 2021-06-08 | 常州威斯双联科技有限公司 | Soft magnetic alloy powder, wave absorbing plate, preparation method of soft magnetic alloy powder, electronic component and electronic equipment |
| CN110041886A (en) * | 2019-05-21 | 2019-07-23 | 常州威斯双联科技有限公司 | A kind of novel graphene absorbing material and preparation method |
| CN110487866A (en) * | 2019-09-19 | 2019-11-22 | 西北师范大学 | A kind of application of Porous hollow Nano carbon balls material prepared and its detect nitrite |
| CN110487866B (en) * | 2019-09-19 | 2022-01-28 | 西北师范大学 | Preparation and application of porous hollow carbon nanosphere material |
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| CN107325787B (en) | 2021-01-29 |
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