CN102061144A - Composite superfine fiber wave-absorbing material and preparation method thereof - Google Patents
Composite superfine fiber wave-absorbing material and preparation method thereof Download PDFInfo
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- CN102061144A CN102061144A CN2010105818314A CN201010581831A CN102061144A CN 102061144 A CN102061144 A CN 102061144A CN 2010105818314 A CN2010105818314 A CN 2010105818314A CN 201010581831 A CN201010581831 A CN 201010581831A CN 102061144 A CN102061144 A CN 102061144A
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Abstract
The invention relates to a composite superfine fiber wave-absorbing material and a preparation method thereof, relating to the technical field of preparing Fe3O4 through a sol-gel method, the technical field of preparing Fe3O4/polyaniline composite nanoparticles through the situ polymerization method, the technical field of preparing the superfine fiber wave-absorbing material through an electrostatic spinning method and other technical fields. In the method in the invention, the principles of the sol-gel method and situ combination are adopted and the situ polymerization chemical reaction of FeSO4.7H2O, FeCl3, ammonium persulfate and other raw materials is utilized to prepare Fe3O4/polyaniline composite particles with good dispersibility; and then the electrostatic spinning technology is adopted and the drum process is used to receive the obtained superfine fiber wave-absorbing material. In the method in the invention, the defects that the polyaniline is difficult to dissolve, the magnetic loss of the common wave-absorbing material is difficult to control, and the like are overcome. The prepared superfine fiber wave-absorbing material in the invention has high the advantages of strength and machinability, small fiber diameter and uniform distribution and can be widely used in various fields such as electronic screening, military camouflage and civil aviation and the like.
Description
Technical field
The present invention relates to a kind of preparation method of composite superfine fiber wave-absorbing material, be specifically related to sol-gal process and prepare Fe
3O
4, situ aggregation method prepares Fe
3O
4/ polyaniline nano compound particle, and use electrospinning process to prepare the technical fields such as superfine fibre absorbing material.
Background technology
Microwave absorbing material is meant a class material that can effectively absorb incident electromagnetic wave and make its scatter attenuation, its various different loss mechanism by material changes into heat energy or other form of energy with incident electromagnetic wave and reaches and absorb the hertzian wave purpose, for for the research and development of absorbing material be the focus of studying both at home and abroad always.Wherein, have and discover that steel fiber has good conductivity, with low dielectric matrix compound tenses such as resin, rubber, lower content can obtain dielectric real part and all very high absorbing material of imaginary part, and the electromagnetic loss mechanism of steel fiber matrix material mainly is eddy-current loss, electric dipole vibration loss, dielectric loss and ohmic loss etc.It is fine that human Stainless Steel Fibres such as Hochberg are done the shielding material shield effectiveness that conductive filler material makes, and is the superfine Stainless Steel Fibre of 7 μ m with diameter, and loading level accounts for 6% of quality, and its effectiveness of shielding (SE) value can reach 40dB.But the shortcoming of steel fiber is the problems such as winding fractures that easily produce in moulding process.Carbon fiber, silicon carbide fiber etc. are compared with steel fiber has that density is little, chemical stability good, the advantage of good moldability, though conductive capability is not as the metal height, can by its surface being carried out the conductivity that technology such as modification, doping improve fiber.People such as Tzeng find, method by electroless plating is plated to carbon fiber surface with nickel and does conductive filler material, is filled in the ABS resin, and resistivity reaches 73 Ω cm, the shielding material that processability is good, fibrous texture absorbing material have become the main developing direction that absorbing material is used.
Conductive polymers and nano inoganic particle are carried out compound gaining a special interest, gained composite material concurrent electroconductibility and magnetic, the advantage of having gathered conductive polymers and nano inoganic particle, simultaneously, polymkeric substance coats nano inoganic particle, has prevented the shortcoming that nanoparticle is reunited owing to its high surfactivity.
But above-mentioned research does not all relate to the nano inoganic particle tri-iron tetroxide (Fe that the present invention proposes
3O
4The preparation method of)/polyaniline composite superfine fiber wave-absorbing material.
Summary of the invention
The purpose of this invention is to provide a kind of novel method for preparing composite superfine fiber wave-absorbing material, utilize sol-gal process to prepare Fe
3O
4, situ aggregation method prepares Fe
3O
4/ polyaniline nano compound particle uses electrospinning process to prepare the superfine fibre absorbing material at last.
For achieving the above object, the technical solution used in the present invention is prepared the ultra-fine fibre absorbing material for utilizing in-situ polymerization and electrospinning process, and concrete steps are as follows:
(1) nanometer Fe
3O
4Preparation, with a certain amount of FeSO
47H
2The O aqueous solution and FeCl
3The aqueous solution mix at 2: 1 with volume ratio, toward wherein adding an amount of polyethylene glycol, be warming up to 70 ℃ after supersonic oscillations mix, toward wherein dripping concentrated ammonia liquor, continue reaction after being adjusted to PH=9 behind the strong agitation number minute, magnetic separates supernatant liquor, with Fe
3O
4Particle uses the distilled water cyclic washing for several times, and carries out drying.
(2) Fe
3O
4The preparation of/PANI compound particle took by weighing a certain amount of CTAB, mixed being placed in the there-necked flask with n-butanol according to mass ratio 1: 1, toward wherein adding a certain amount of water-soluble solution, got above-mentioned an amount of Fe after the logical nitrogen protection
3O
4Particle joins in the solution, sonic oscillation certain hour under the room temperature.Aniline joined the lucifuge processing machine stirs behind the above-mentioned solution.Drip HCl and regulate PH=4.Progressively drip ammonium persulfate solution after subsequently system temperature being controlled at 0 ℃, obtain blackish green emulsion breaking, with for several times vacuum drying of distilled water washing, obtain Fe
3O
4/ doping attitude PANI nano core-shell material
(3) preparation of Fe3O4/PANI and polyacrylonitrile composite superfine fiber wave-absorbing material takes by weighing a certain amount of PANI/Fe
3O
4Among the nanoparticle dissolution DMF, treat stirring and dissolving after, get an amount of PAN and join in the solution, with the mixed solution magnetic agitation.Get pack into the syringe of the standard capacity of being with syringe needle of mixing solutions, the positive potential that the electrostatic spinning mixing solutions is used is added in syringe needle, uses the cylinder that is covered by aluminium foil as receiving trap.Collect the nanofiber on the aluminium foil, dry under chamber state, make residual DMF volatilization.
Owing to adopted technique scheme, the present invention to have following advantage and effect:
(1) the present invention has both overcome PANI because molecular weight is low owing to adopted PANI and polyacrylonitrile to carry out conjugate spinning, and the shortcoming that is difficult to spinning makes that again the ultra-fine fibre absorbing material of preparing has the good mechanical performance, helps industrial applications.
(2) the use collosol and gel of the present invention's proposition and the preparation method of in-situ polymerization so that each reaction raw materials takes full advantage of, have both saved cost, again so that whole preparation process is easy to control.
Figure of description
Fig. 1 composite ultrafine fiber absorbing material absorbing property curve
Fig. 2 composite ultrafine fiber scanning electron microscope image
Embodiment
Example 1
FeSO with 0.3mol/l
47H
2The FeCl of the O aqueous solution and 0.4mol/L
3The aqueous solution mix at 2: 1 with volume ratio, place the there-necked flask of logical nitrogen, toward wherein adding an amount of polyethylene glycol, after mixing, supersonic oscillations are warming up to 70 ℃, behind the strong agitation number minute toward wherein dripping concentrated ammonia liquor, continue reaction 1h after being adjusted to PH=9, magnetic separates supernatant liquor, with Fe
3O
4Particle uses the distilled water cyclic washing for several times, 40 ℃ of lower vacuum drying 24h.Take by weighing a certain amount of CTAB, mix being placed in the there-necked flask according to mass ratio 1: 1 with n-butanol, toward wherein adding the water-soluble solution of 40ml, get above-mentioned an amount of Fe after the logical nitrogen protection
3O
4Particle joins in the solution, sonic oscillation 2h under the room temperature; 2ml aniline joined the lucifuge processing machine stirs 1h behind the mentioned solution, drip HCl and regulate PH=4.Progressively drip ammonium persulfate solution after subsequently system temperature being controlled at 0 ℃, dropwise in the 30min.Keep reaction temperature at 0～5 ℃ of reaction 20h, obtain blackish green emulsion breaking, with for several times vacuum drying of distilled water washing 24h, obtain Fe
3O
4/ doping attitude PANI nano core-shell material.Use electrostatic spinning to carry out spinning.
Example 2
FeSO with 2mol/l
47H
2The FeCl of the O aqueous solution and 2.2mol/L
3The aqueous solution mix at 3: 2 with mass ratio, place the there-necked flask of logical nitrogen, toward wherein adding an amount of polyethylene glycol, after mixing, supersonic oscillations are warming up to 75 ℃, behind the strong agitation number minute toward wherein dripping concentrated ammonia liquor, continue reaction 1.2h after being adjusted to PH=9, magnetic separates supernatant liquor, with Fe
3O
4Particle uses the distilled water cyclic washing for several times, 40 ℃ of lower vacuum drying 24h.Take by weighing a certain amount of CTAB, mix being placed in the there-necked flask according to mass ratio 3: 2 with n-butanol, toward wherein adding the water-soluble solution of 80ml, get above-mentioned an amount of Fe after the logical nitrogen protection
3O
4Particle joins solution; In, sonic oscillation 2h under the room temperature.10g aniline joined the lucifuge processing machine stirs 1h behind the above-mentioned solution.Drip HCl and regulate PH=4.Progressively drip ammonium persulfate solution after subsequently system temperature being controlled at 0 ℃, dropwise in the 30min.Keep reaction temperature at 0～5 ℃ of reaction 20h, obtain blackish green emulsion breaking, with for several times vacuum drying of distilled water washing 24h, obtain Fe
3O
4/ doping attitude PANI nano core-shell material.Use electrostatic spinning to carry out spinning.
Claims (3)
1. composite superfine fiber wave-absorbing material and preparation method thereof is characterized in that preparing nanometer Fe with situ aggregation method
3O
4/ polyaniline nano compound particle is mixed into blend spinning liquid with nano-complex particle and the polyacrylonitrile that obtains then, and the method by electrostatic spinning spins the composite superfine fiber wave-absorbing material with loose structure again.
2. such as the preparation method of right 1 described a kind of composite superfine fiber wave-absorbing material, it is characterized in that sol-gal process prepares nanometer Fe
3O
4: FeSO
47H
2The O aqueous solution and FeCl
3The aqueous solution mix at 2: 1 with volume ratio, place the there-necked flask of logical nitrogen, reaction temperature is 70 ℃.PH value is 9.
3. such as the preparation method of right 1 described a kind of composite superfine fiber wave-absorbing material, it is characterized in that: take HCl as dopant acid, employing CTAB is that emulsifying agent, n-butanol are assistant for emulsifying agent, is initator microemulsion in-situ polymerization Fe at ammonium persulfate (APS)
3O
4/ polyaniline.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304304A (en) * | 2011-07-30 | 2012-01-04 | 中国科学院合肥物质科学研究院 | Preparation method of plastic coating with civil frequency-range electromagnetic compatibility function based on crosslinking and uniform dispersing system |
| CN102408562A (en) * | 2011-09-23 | 2012-04-11 | 西南交通大学 | Preparation method for polyaniline/ferroferric oxide compound with nucleus-shell structure |
| CN102493176A (en) * | 2011-11-24 | 2012-06-13 | 东华大学 | Preparation method of electromagnetic functional compound fabric |
| CN103087624A (en) * | 2013-01-31 | 2013-05-08 | 南昌航空大学 | Ultraviolet light-cured polyaniline/Fe3SO4 wave absorbing coating |
| CN104213243A (en) * | 2014-09-24 | 2014-12-17 | 西北工业大学 | Preparation method of polyaniline nanofiber with high draw ratio |
| CN104264272A (en) * | 2014-09-24 | 2015-01-07 | 西北工业大学 | Preparation method of electromagnetic nanofibers |
| CN104790067A (en) * | 2015-04-17 | 2015-07-22 | 东华大学 | Nano conductive polymer/graphene composite fiber, and preparation method and application thereof |
| CN106283397A (en) * | 2016-08-30 | 2017-01-04 | 长春理工大学 | Green emitting electromagnetism three function two-layer composite nano-fiber membrane and preparation method thereof |
| CN106811834A (en) * | 2017-01-12 | 2017-06-09 | 南开大学 | A kind of preparation method of flexible di-iron trioxide/ferroso-ferric oxide and nitrogen-doped carbon composite nano fiber |
| CN108505144A (en) * | 2018-05-10 | 2018-09-07 | 芜湖市创源新材料有限公司 | A kind of preparation method of composite regenerated cellulose fibre |
| CN108729027A (en) * | 2018-05-31 | 2018-11-02 | 浙江理工大学 | A kind of polyaniline fiber wave-absorber system and preparation method thereof |
| CN109817963A (en) * | 2019-02-18 | 2019-05-28 | 吉林大学 | Fe7Se8Nanoparticle/nitrogen-doped carbon nano-fiber composite material preparation method and applications |
| CN109989130A (en) * | 2019-04-18 | 2019-07-09 | 山东大学 | A kind of flexibility ferroso-ferric oxide fiber and preparation method thereof |
| CN111358061A (en) * | 2020-04-26 | 2020-07-03 | 安徽农业大学 | Moisture-absorbing and heating uterus-warming underpants and preparation method thereof |
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| CN1096487C (en) * | 1999-07-12 | 2002-12-18 | 武汉工业大学 | nm-class composite polyphenylamine-Fe2O3 material and its preparing process |
| CN101117733A (en) * | 2007-07-27 | 2008-02-06 | 东华大学 | Radiation-absorption fibre and preparing process |
| CN101161725A (en) * | 2007-09-29 | 2008-04-16 | 复旦大学 | Polyaniline coated magnetic carbon-nano tube composite material and preparation method thereof |
-
2010
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Patent Citations (3)
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|---|---|---|---|---|
| CN1096487C (en) * | 1999-07-12 | 2002-12-18 | 武汉工业大学 | nm-class composite polyphenylamine-Fe2O3 material and its preparing process |
| CN101117733A (en) * | 2007-07-27 | 2008-02-06 | 东华大学 | Radiation-absorption fibre and preparing process |
| CN101161725A (en) * | 2007-09-29 | 2008-04-16 | 复旦大学 | Polyaniline coated magnetic carbon-nano tube composite material and preparation method thereof |
Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304304A (en) * | 2011-07-30 | 2012-01-04 | 中国科学院合肥物质科学研究院 | Preparation method of plastic coating with civil frequency-range electromagnetic compatibility function based on crosslinking and uniform dispersing system |
| CN102304304B (en) * | 2011-07-30 | 2013-04-17 | 中国科学院合肥物质科学研究院 | Preparation method of plastic coating with civil frequency-range electromagnetic compatibility function based on crosslinking and uniform dispersing system |
| CN102408562A (en) * | 2011-09-23 | 2012-04-11 | 西南交通大学 | Preparation method for polyaniline/ferroferric oxide compound with nucleus-shell structure |
| CN102408562B (en) * | 2011-09-23 | 2013-04-03 | 西南交通大学 | Preparation method for polyaniline/ferroferric oxide compound with nucleus-shell structure |
| CN102493176A (en) * | 2011-11-24 | 2012-06-13 | 东华大学 | Preparation method of electromagnetic functional compound fabric |
| CN103087624B (en) * | 2013-01-31 | 2016-05-18 | 南昌航空大学 | A kind of UV curing polyaniline/FeSO4Microwave absorbing coating and preparation method thereof |
| CN103087624A (en) * | 2013-01-31 | 2013-05-08 | 南昌航空大学 | Ultraviolet light-cured polyaniline/Fe3SO4 wave absorbing coating |
| CN104213243A (en) * | 2014-09-24 | 2014-12-17 | 西北工业大学 | Preparation method of polyaniline nanofiber with high draw ratio |
| CN104264272A (en) * | 2014-09-24 | 2015-01-07 | 西北工业大学 | Preparation method of electromagnetic nanofibers |
| CN104213243B (en) * | 2014-09-24 | 2016-05-04 | 西北工业大学 | A kind of preparation method of the polyaniline nano fiber with high length-diameter ratio |
| CN104790067A (en) * | 2015-04-17 | 2015-07-22 | 东华大学 | Nano conductive polymer/graphene composite fiber, and preparation method and application thereof |
| CN106283397A (en) * | 2016-08-30 | 2017-01-04 | 长春理工大学 | Green emitting electromagnetism three function two-layer composite nano-fiber membrane and preparation method thereof |
| CN106811834A (en) * | 2017-01-12 | 2017-06-09 | 南开大学 | A kind of preparation method of flexible di-iron trioxide/ferroso-ferric oxide and nitrogen-doped carbon composite nano fiber |
| CN106811834B (en) * | 2017-01-12 | 2019-02-05 | 南开大学 | A kind of preparation method of flexibility di-iron trioxide/ferroso-ferric oxide and nitrogen-doped carbon composite nano fiber |
| CN108505144A (en) * | 2018-05-10 | 2018-09-07 | 芜湖市创源新材料有限公司 | A kind of preparation method of composite regenerated cellulose fibre |
| CN108729027A (en) * | 2018-05-31 | 2018-11-02 | 浙江理工大学 | A kind of polyaniline fiber wave-absorber system and preparation method thereof |
| CN108729027B (en) * | 2018-05-31 | 2020-06-16 | 浙江理工大学 | Polyaniline fiber wave-absorbing system |
| CN109817963A (en) * | 2019-02-18 | 2019-05-28 | 吉林大学 | Fe7Se8Nanoparticle/nitrogen-doped carbon nano-fiber composite material preparation method and applications |
| CN109817963B (en) * | 2019-02-18 | 2021-09-21 | 吉林大学 | Fe7Se8Preparation method and application of nano particle/nitrogen-doped carbon nanofiber composite material |
| CN109989130A (en) * | 2019-04-18 | 2019-07-09 | 山东大学 | A kind of flexibility ferroso-ferric oxide fiber and preparation method thereof |
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Application publication date: 20110518 |