CN102627834A - Preparation method of chitosan modification barium ferrite filling multi-walled carbon nanotube/poly 3-methylthiophene composite wave-absorbing material - Google Patents
Preparation method of chitosan modification barium ferrite filling multi-walled carbon nanotube/poly 3-methylthiophene composite wave-absorbing material Download PDFInfo
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Abstract
The invention provides a preparation method of a chitosan modification barium ferrite filling multi-walled carbon nanotube/poly 3-methylthiophene composite wave-absorbing material. The method utilizes a carbon nanotube as a raw material, after the carbon nanotube is filled with barium ferrite, chitosan is coated on the carbon nanotube for modification, and then the carbon nanotube is composited with poly 3-methylthiophene to obtain the novel wave-absorbing material integrating magnetic loss, electrical loss and carbon nanotube wave absorption. Requirements for being thin, light, wide and strong of the wave-absorbing material are met. Therefore, the composite wave-absorbing material has wide application prospect in aspects of microwave absorption, electromagnetic radiation resistance and the like.
Description
Technical field
The invention belongs to the electromagnetic wave absorbent material preparation field, particularly a kind of conduction loss, magnetic loss and carbon nanotube of integrating inhaled the multi-walled carbon nano-tubes that the chitosan-modified GP 500 of ripple fills/the gather preparation method of 3 methyl thiophene composite wave-suction material.
Background technology
Electromagnetic wave absorbent material (Electromagnetic Wave Absorbing Materials) is meant the incident electromagnetic wave that can absorb and decay, and converts electromagnetic energy to heat energy and with its one type of material that dissipates or hertzian wave is disappeared because of interference.In broad terms, it comprises anti-electromagnetic interference (EMI) and microwave absorbing material (RAM), even comprises the wide spectrum from sound wave to the infra-red absorption material, and its range of application is also in continuous expansion.Classify from loss mechanism, absorbing material can be divided into resistor-type, dielectric type and magneticmedium type 3 big classes, and wherein, the resistor-type loss also can cover in the dielectric loss and go.
In numerous absorbing materials, ferrite and metal-powder absorption agent have good absorbing property and lower cost, but that its shortcoming is a density is too big, are difficult for preparing the absorbing material of light weight.Polythiophene base conducting polymer is as microwave absorption, and is main because have the electrical loss characteristic, rather than has the magnetic loss characteristic, and obtain the ideal wave-absorbing effect also must have the magnetic loss characteristic.Along with the progress of science and technology, more and more deep to the research of carbon nanotube, it receives much concern in suction ripple field.Because the carbon nanotube yardstick is much smaller than infrared rays and radar wave wavelength, so nanoparticle material is strong than conventional material to the absorptivity of infrared and microwave.Along with reducing of size; Nanoparticle material has the high-specific surface area than big 3 ~ 4 one magnitude of conventional coarse dispersion material; Along with the rising of surface atom ratio, lattice defect increase, dangling bonds increase, form the interface polarization of electrode easily, high specific surface area can cause multiple scattering again.In addition, the part carbon nanotube has special spirane structure and chirality, and this all causes carbon nanotube to have high absorbing property.Therefore, as the prepared absorbing material of absorption agent, have characteristics such as inhaling ripple bandwidth, controlled and compatible good, light weight, thin thickness with carbon nanotube, its shortcoming is that the magnetic permeability of carbon nanotube is lower.
Therefore; If carbon nanotube is effectively combined with magnetic substance; Compound with conduction high polymer again; Be expected to obtain integrating the novel wave-absorbing material that magnetic loss, conduction loss and carbon nanotube are inhaled ripple, satisfy the requirement of absorbing material " thin, light, wide, strong ", extremely application prospects is arranged at aspects such as microwave absorbing and environment protection healths.
Summary of the invention
The purpose of this invention is to provide the multi-walled carbon nano-tubes that a kind of chitosan-modified GP 500 fills/gather the preparation method of 3 methyl thiophene composite wave-suction material, this matrix material can be used as the absorption of low frequency microwave.The objective of the invention is to realize like this, its preparation method is:
(1) GP 500 is filled the preparation of multi-walled carbon nano-tubes
Under the room temperature, put into Erlenmeyer flask to the 1.0g multi-walled carbon nano-tubes, add 40mL iron nitrate saturated solution and 20mL nitrate of baryta saturated solution, under the whisking appliance of 800 rev/mins rotating speeds stirs; Dropwise add concentrated nitric acid 15mL and vitriol oil 5mL, after ultrasonic dispersing is even, interacted 10 days, after filtration, the vacuum-drying; Put into quartz boat, the tubular type of packing into atmosphere furnace feeds nitrogen, 2 liters/minute of gas flows; Heat-up rate is 3 ℃/minute, is warming up to 700 ℃, keeps 2h; After naturally cooling to room temperature, filter once more after being about 7 with deionized water rinsing to pH, vacuum-drying obtains the multi-walled carbon nano-tubes that GP 500 is filled.
(2) chitosan-modified GP 500 is filled the preparation of multi-walled carbon nano-tubes
It is 2 dilute acetic acid solution that the chitosan of 1.0g is dissolved in the pH value, is stirred to abundant dissolving; Take by weighing the multi-walled carbon nano-tubes that the 1.0g GP 500 is filled then, with mixed solution ultra-sonic dispersion 2h, magnetic agitation 1h; In dispersion system, drip weak ammonia again, make in the compound system pH value, behind the heating mixing solutions to 60 ℃ greater than 10; Adding 0.05g massfraction is 6% LUTARALDEHYDE; Crosslinking reaction 1.5h, centrifugal collection, dilute acetic acid washes back 50 ℃ of vacuum-drying 24h and obtains the multi-walled carbon nano-tubes that chitosan-modified GP 500 is filled.
(3) gather the preparation of 3 methyl thiophene
Under the room temperature condition, with the anhydrous FeCl of 0.25mol
3Join in the there-necked flask that contains the 100mL chloroformic solution, stir about 30min obtains the muddy liquid of sap green, will contain the monomeric 25mL chloroformic solution of 10mL3-thiotolene and dropwise splash in the there-necked flask stirring reaction 10h.After reaction finishes, with the solvent evaporate to dryness, pour the HCl solution of 1mol/L under the room temperature, stirring at room 12h, suction filtration, distilled water wash 2 ~ 3 times is colourless to filtrating, 50 ℃ of vacuum-drying 24h obtain gathering 3 methyl thiophene.
(4) chitosan-modified GP 500 is filled multi-walled carbon nano-tubes/the gather preparation of 3 methyl thiophene composite wave-suction material
The multi-walled carbon nano-tubes massfraction 20% ~ 40% of filling according to chitosan-modified GP 500 with gather 3 methyl thiophene and mix, grinding obtains the multi-walled carbon nano-tubes of chitosan-modified GP 500 filling/gather 3 methyl thiophene composite wave-suction material.
Major advantage of the present invention: the one, filled with barium ferrite in carbon nanotube; Make it have magnetic; Again with gather that the 3 methyl thiophene conduction high polymer is compound to obtain integrating the novel wave-absorbing material that magnetic loss, conduction loss and carbon nanotube are inhaled ripple, at aspects such as microwave absorbing and environment protection healths extremely application prospects is arranged; The 2nd, make the multi-walled carbon nano-tubes that GP 500 fills after, through the chitosan coating decoration, make its group's bunch minimizing, with to gather 3 methyl thiophene compound more abundant.
Embodiment
Further specify the present invention below in conjunction with embodiment.
The present invention provides the multi-walled carbon nano-tubes that a kind of chitosan-modified GP 500 fills/the gather preparation method of 3 methyl thiophene composite wave-suction material.Be to be raw material with the carbon nanotube, inner filled with barium ferrite is after the chitosan coating decoration, last again with gather that 3 methyl thiophene is compound to make a kind of novel wave-absorbing material that magnetic loss, electrical loss and carbon nanotube are inhaled ripple that integrates.
Embodiment 1
(1) GP 500 is filled the preparation of multi-walled carbon nano-tubes
Under the room temperature, put into Erlenmeyer flask to the 1.0g multi-walled carbon nano-tubes, add 40mL iron nitrate saturated solution and 20mL nitrate of baryta saturated solution, under the whisking appliance of 800 rev/mins of rotating speeds stirs; Dropwise add concentrated nitric acid 15mL and vitriol oil 5mL, after ultrasonic dispersing is even, interacted 10 days, after filtration, the vacuum-drying; Put into quartz boat, the tubular type of packing into atmosphere furnace feeds nitrogen, 2 liters/minute of gas flows; Heat-up rate is 3 ℃/minute, is warming up to 700 ℃, keeps 2h; After naturally cooling to room temperature, filter once more after being about 7 with deionized water rinsing to pH, vacuum-drying obtains the multi-walled carbon nano-tubes that GP 500 is filled.
(2) chitosan-modified GP 500 is filled the preparation of multi-walled carbon nano-tubes
It is 2 dilute acetic acid solution that the chitosan of 1.0g is dissolved in the pH value, is stirred to abundant dissolving; Take by weighing the multi-walled carbon nano-tubes that the 1.0g GP 500 is filled then, with mixed solution ultra-sonic dispersion 2h, magnetic agitation 1h; In dispersion system, drip weak ammonia again, make in the compound system pH value, behind the heating mixing solutions to 60 ℃ greater than 10; Adding 0.05g massfraction is 6% LUTARALDEHYDE; Crosslinking reaction 1.5h, centrifugal collection, dilute acetic acid washes back 50 ℃ of vacuum-drying 24h and obtains the multi-walled carbon nano-tubes that chitosan-modified GP 500 is filled.
(3) gather the preparation of 3 methyl thiophene
Under the room temperature condition, with the anhydrous FeCl of 0.25mol
3Join in the there-necked flask that contains the 100mL chloroformic solution, stir about 30min obtains the muddy liquid of sap green, will contain the monomeric 25mL chloroformic solution of 10mL 3 methyl thiophene and dropwise splash in the there-necked flask stirring reaction 10h.After reaction finishes, with the solvent evaporate to dryness, pour the HCl solution of 1mol/L under the room temperature, stirring at room 12h, suction filtration, distilled water wash 2 ~ 3 times is colourless to filtrating, 50 ℃ of vacuum-drying 24h obtain gathering 3 methyl thiophene.
(4) chitosan-modified GP 500 is filled multi-walled carbon nano-tubes/the gather preparation of 3 methyl thiophene composite wave-suction material
The multi-walled carbon nano-tubes of getting the chitosan-modified GP 500 filling of 0.8g gathers 3 methyl thiophene with 3.2g and mixes; Grind fully; Obtain chitosan-modified GP 500 and fill multi-walled carbon nano-tubes/gather 3 methyl thiophene composite wave-suction material; Its absorption peak can reach 40% greater than the frequency span of-25dB, and the highest absorption peak can reach-37dB.
Embodiment 2
The preparation of the preparation of GP 500 filling multi-walled carbon nano-tubes, chitosan-modified GP 500 filling multi-walled carbon nano-tubes, the preparation that gathers 3 methyl thiophene are with embodiment 1; The multi-walled carbon nano-tubes of getting the chitosan-modified GP 500 filling of 1.0g gathers 3 methyl thiophene with 3.0g and mixes; Grind fully; Obtain chitosan-modified GP 500 and fill multi-walled carbon nano-tubes/gather 3 methyl thiophene composite wave-suction material; Its absorption peak can reach 35% greater than the frequency span of-28dB, and the highest absorption peak can reach-40dB.
Embodiment 3
The preparation that the preparation of GP 500 filling multi-walled carbon nano-tubes, chitosan-modified GP 500 are filled multi-walled carbon nano-tubes, the preparation embodiment 1 that gathers 3 methyl thiophene; The multi-walled carbon nano-tubes of getting the chitosan-modified GP 500 filling of 1.2g gathers 3 methyl thiophene with 2.8g and mixes; Grind fully; Obtain the multi-walled carbon nano-tubes that chitosan-modified GP 500 fills/gather 3 methyl thiophene composite wave-suction material; Its absorption peak can reach 30% greater than the frequency span of-30dB, and the highest absorption peak can reach-38dB.
Embodiment 4
The preparation of the preparation of GP 500 filling multi-walled carbon nano-tubes, chitosan-modified GP 500 filling multi-walled carbon nano-tubes, the preparation that gathers 3 methyl thiophene are with embodiment 1; The multi-walled carbon nano-tubes of getting the chitosan-modified GP 500 filling of 1.4g gathers 3 methyl thiophene with 2.6g and mixes; Grind fully; Obtain the multi-walled carbon nano-tubes that chitosan-modified GP 500 fills/gather 3 methyl thiophene composite wave-suction material; Its absorption peak can reach 35% greater than the frequency span of-30dB, and the highest absorption peak can reach-42dB.
Embodiment 5
The preparation of the preparation of GP 500 filling multi-walled carbon nano-tubes, chitosan-modified GP 500 filling multi-walled carbon nano-tubes, the preparation that gathers 3 methyl thiophene are with embodiment 1; The multi-walled carbon nano-tubes of getting the chitosan-modified GP 500 filling of 1.6g gathers 3 methyl thiophene with 2.4g and mixes; Grind fully; Obtain the multi-walled carbon nano-tubes that chitosan-modified GP 500 fills/gather 3 methyl thiophene composite wave-suction material; Its absorption peak can reach 35% greater than the frequency span of-28dB, and the highest absorption peak can reach-39dB.
Claims (2)
1. a chitosan-modified GP 500 is filled multi-walled carbon nano-tubes/gather the preparation method of 3 methyl thiophene composite wave-suction material, it is characterized in that the preparation method is following:
(1) GP 500 is filled the preparation of multi-walled carbon nano-tubes: under the room temperature, put into there-necked flask to the 1.0g multi-walled carbon nano-tubes, add 40mL iron nitrate saturated solution and 20mL nitrate of baryta saturated solution; Under the whisking appliance of 800 rev/mins of rotating speeds stirs, dropwise add concentrated nitric acid 15mL and vitriol oil 5mL, after ultrasonic dispersing is even; Interacted 10 days, and after filtration, the vacuum-drying, put into quartz boat; The tubular type of packing into atmosphere furnace feeds nitrogen, 2 liters/minute of gas flows; Heat-up rate is 3 ℃/minute, is warming up to 700 ℃, keeps 2h; After naturally cooling to room temperature, filter once more after being about 7 with deionized water rinsing to pH, vacuum-drying obtains the multi-walled carbon nano-tubes that GP 500 is filled;
(2) chitosan-modified GP 500 is filled the preparation of multi-walled carbon nano-tubes: it is 2 dilute acetic acid solution that the chitosan of 1.0-2.0g is dissolved in pH value, is stirred to abundant dissolving, takes by weighing the multi-walled carbon nano-tubes of 1.0g GP 500 filling then; With mixed solution ultra-sonic dispersion 2h, magnetic agitation 1h drips weak ammonia again in dispersion system; Make in the compound system pH value greater than 10; Behind the heating mixing solutions to 60 ℃, add the 0.05g massfraction and be 6% LUTARALDEHYDE, crosslinking reaction 1.5h; Centrifugal collection, dilute acetic acid are washed back 50 ℃ of vacuum-drying 24h and are obtained the multi-walled carbon nano-tubes that chitosan-modified GP 500 is filled;
(3) gather the preparation of 3 methyl thiophene: under the room temperature condition, with the anhydrous FeCl of 0.25mol
3Join in the there-necked flask that contains the 100mL chloroformic solution, stir about 30min obtains the muddy liquid of sap green; To contain the monomeric 25mL chloroformic solution of 10mL 3 methyl thiophene and dropwise splash in the there-necked flask, behind the stirring reaction 10h, under the room temperature with the solvent evaporate to dryness; Pour the HCl solution of 1mol/L into, stirring at room 12h, suction filtration; Distilled water wash 2 ~ 3 times is colourless to filtrating, and 50 ℃ of vacuum-drying 24h obtain gathering 3 methyl thiophene;
(4) chitosan-modified GP 500 is filled multi-walled carbon nano-tubes/the gather preparation of 3 methyl thiophene composite wave-suction material: the multi-walled carbon nano-tubes massfraction 20% ~ 40% of filling according to chitosan-modified GP 500 with gather 3 methyl thiophene and mix; Grind fully, obtain the multi-walled carbon nano-tubes that chitosan-modified GP 500 fills/gather 3 methyl thiophene composite wave-suction material.
2. modify GP 500 according to preparing method's prepared chitosan of claim 1 and fill multi-walled carbon nano-tubes/gather 3 methyl thiophene composite wave-suction material.
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Cited By (7)
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| CN102964571A (en) * | 2012-11-12 | 2013-03-13 | 南昌航空大学 | Preparation method of barium ferrite/carbon nanotube/poly(3-methylthiophene) composite wave-absorbing material |
| CN103632798A (en) * | 2013-12-03 | 2014-03-12 | 东华理工大学 | Method for preparing poly-3-methylthiophene coated nickel-zinc ferrite nanoparticle magnetic liquid |
| CN104086953A (en) * | 2014-06-26 | 2014-10-08 | 南昌航空大学 | Preparation method for chitosan-modified ferrite-filled multi-wall carbon nano tube/polythiophene composite wave-absorbing material |
| CN104098874A (en) * | 2014-06-26 | 2014-10-15 | 南昌航空大学 | Composite wave-absorbing material preparation method |
| CN104147643A (en) * | 2014-08-06 | 2014-11-19 | 江苏双林海洋生物药业有限公司 | Method for preparing conductive tissue engineering scaffold of chitosan and carbon nanometer tube |
| CN107057135A (en) * | 2016-12-22 | 2017-08-18 | 中北大学 | A kind of High-performance graphene/FeNixThe preparation of/natural rubber electromagnetic wave absorbent material |
| CN109438927A (en) * | 2018-11-23 | 2019-03-08 | 南昌航空大学 | A kind of chitosan-modified ferrite filling multi-walled carbon nanotube/polythiophene composite wave-suction material preparation method |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102964571A (en) * | 2012-11-12 | 2013-03-13 | 南昌航空大学 | Preparation method of barium ferrite/carbon nanotube/poly(3-methylthiophene) composite wave-absorbing material |
| CN103632798A (en) * | 2013-12-03 | 2014-03-12 | 东华理工大学 | Method for preparing poly-3-methylthiophene coated nickel-zinc ferrite nanoparticle magnetic liquid |
| CN103632798B (en) * | 2013-12-03 | 2016-02-24 | 东华理工大学 | A kind of preparation method of poly-3 methyl thiophene clad nano nickel-zinc ferrite particle magnetic liquid |
| CN104086953A (en) * | 2014-06-26 | 2014-10-08 | 南昌航空大学 | Preparation method for chitosan-modified ferrite-filled multi-wall carbon nano tube/polythiophene composite wave-absorbing material |
| CN104098874A (en) * | 2014-06-26 | 2014-10-15 | 南昌航空大学 | Composite wave-absorbing material preparation method |
| CN104086953B (en) * | 2014-06-26 | 2017-07-21 | 南昌航空大学 | A kind of chitosan-modified ferrite fills the preparation method of multi-walled carbon nanotube/polythiophene composite wave-suction material |
| CN104147643A (en) * | 2014-08-06 | 2014-11-19 | 江苏双林海洋生物药业有限公司 | Method for preparing conductive tissue engineering scaffold of chitosan and carbon nanometer tube |
| CN104147643B (en) * | 2014-08-06 | 2016-05-18 | 江苏双林海洋生物药业有限公司 | Prepare the method for chitosan-carbon nanotube conductive tissue engineering rack |
| CN107057135A (en) * | 2016-12-22 | 2017-08-18 | 中北大学 | A kind of High-performance graphene/FeNixThe preparation of/natural rubber electromagnetic wave absorbent material |
| CN109438927A (en) * | 2018-11-23 | 2019-03-08 | 南昌航空大学 | A kind of chitosan-modified ferrite filling multi-walled carbon nanotube/polythiophene composite wave-suction material preparation method |
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