CN104311852B - A kind of method and apparatus for preparing vertical ordered carbon nanotube/polyaniline composite film - Google Patents
A kind of method and apparatus for preparing vertical ordered carbon nanotube/polyaniline composite film Download PDFInfo
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- CN104311852B CN104311852B CN201410581837.XA CN201410581837A CN104311852B CN 104311852 B CN104311852 B CN 104311852B CN 201410581837 A CN201410581837 A CN 201410581837A CN 104311852 B CN104311852 B CN 104311852B
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Abstract
The present invention provides a kind of method for preparing vertical ordered carbon nanotube/polyaniline composite film, it is characterised in that comprise the following steps：Prepare mix moisture dispersion liquid step, CNT after acidification is configured to CNT aqueous dispersions, it is reconfigured at polyaniline nano fiber aqueous dispersions, then CNT aqueous dispersions and polyaniline nano fiber aqueous dispersions are mixed, ultrasonic 4h, mechanical agitation 30min, obtains mix moisture dispersion liquid；Suction filtration and electric field synergistic prepare carbon nano-tube/poly aniline composite membrane step, mix moisture dispersion liquid is poured into suction filtration electric field arrangement, apply the voltage perpendicular to filter paper, the voltage is 100~250V, regulation suction filtration power is 180W, apply the synergy of electric field and suction filtration to mix moisture dispersion liquid, suction filtration continues applied voltage 24h after terminating, then filter paper is taken out, naturally carbon nano-tube/poly aniline composite membrane is obtained after drying, wherein, CNT and the mass ratio of polyaniline nano fiber are 5 in mix moisture dispersion liquid:1.
Description
Technical field
The present invention relates to the preparation of material, and in particular to a kind of use suction method and electric field method coordinate system are standby vertical orderly
The method and apparatus of carbon nano-tube/poly aniline composite membrane.
Background technology
The structure of CNT (CNTs) assigns its excellent mechanics, electricity and thermal property.With CNTs as base material
CNTs/ composite membrane of polymer has been widely studied, and the addition of CNTs causes that composite membrane has high intensity, high conductivity and high
Heat endurance, has huge application prospect in fields such as structural material, electronic device, biological medicine and electrochemistry.At present,
CNTs/ composite membrane of polymer is broadly divided into two kinds, and one group is the composite membrane prepared with CNTs and polymer simple blend, is prepared
Method is simpler, and CNTs is disorderly arranged in the polymer；Another kind is vertical CNTs/ composite membrane of polymer in order, i.e. CNTs hangs down
Directly in film surface ordered arrangement.The ordered arrangement of CNTs causes that composite membrane has anisotropy, electrical property and mechanical performance,
Gas-selectively separates the aspects such as filter membrane and shows good application potential.
Polyaniline (PANi) is a kind of conducting functional materials with conjugated structure, be easy to get with raw material, prepare it is simple,
Conductance is high and the advantages of strong heat endurance, in the neck such as electrode material, selective membrane material, electromagnetic shielding material and anti-corrosion material
Domain is widely used.PANi is combined with CNTs, the CNTs/PANi composite membrane of polymer for preparing has excellent physics
Performance.
It is that CNTs is polymerized in PANi to prepare CNTs/PANi composite membrane of polymer and be particularly the key of vertical orderly composite membrane
Dispersed and vertical ordered arrangement in thing.CNTs methods of vertical ordered arrangement in PANi polymer are allow to be to hang down
Polymer is packed into the CNTs of straight array, it is also possible to induce CNTs orientations in the polymer.The CNTs of orthogonal array growth
(as prepared using chemical vapour deposition technique) degree of order is high, but pipe is too small with ligament, and later stage polymer is difficult to be filled into
In tube gap, and the CNTs array areas prepared are smaller, expensive.Using external force field induction CNTs orientations in the polymer
The composite membrane of more practicality can be prepared, these external force fields are including high-intensity magnetic field, electric field, the mechanical field of force etc..High-intensity magnetic field method can
The CNTs arrays of high-sequential, but the magnetic field intensity needed in preparation process up to 25T or so are prepared, experiment condition is harsh.
Electric field method is that CNTs occurs polarization phenomena in the presence of electric field force, dipole moment is produced, so that CNTs can be along electric field
The direction of power reaches ordered arrangement, but the more difficult acquisition film-form CNTs/ composite membrane of polymer of electric field method.Mechanical field of force induction takes
To such as suction method, it is possible to use Vacuum filtration device, directly by CNTs and PANi nanofibers mixed dispersion liquid in shearing masterpiece
With lower suction filtration into film, its preparation method is easy, but the CNTs degrees of order are poor in the composite membrane for obtaining.
The content of the invention
Carried out the present invention be directed to above mentioned problem, it is therefore intended that one kind is provided and prepares vertical ordered carbon nanotube/polyphenyl
The method and apparatus of amine composite membrane, make arrangement of the CNT in polyaniline vertical orderly and dispersed.
The present invention to achieve the above object, employs following technical scheme：
<Scheme one>
The present invention provides a kind of method for preparing vertical ordered carbon nanotube/polyaniline composite film, it is characterised in that including
Following steps：Mix moisture dispersion liquid step is prepared, acidification is carried out to CNT, the CNT after acidification is matched somebody with somebody
CNT aqueous dispersions are set to, polyaniline nano fiber is then configured to polyaniline nano fiber aqueous dispersions, then will
CNT aqueous dispersions and polyaniline nano fiber aqueous dispersions mix, ultrasonic 4h, then mechanical agitation 30min, are mixed
Aqueous dispersions；Suction filtration and electric field synergistic prepare carbon nano-tube/poly aniline composite membrane step, by mix moisture dispersion liquid pour into suction filtration-
Electric field arrangement, applies the voltage perpendicular to filter paper on the filter paper of the suction filtration-electric field arrangement, and the voltage is 100~250V, regulation
The suction filtration power of suction filtration-electric field arrangement is 180W, the synergy of electric field and suction filtration is applied to mix moisture dispersion liquid, in suction filtration knot
Continue applied voltage 24h after beam, then take out filter paper, the carbon nano-tube/poly benzene deposited on filter paper is obtained after drying naturally
Amine composite membrane, wherein, CNT and the mass ratio of polyaniline nano fiber are 5 in mix moisture dispersion liquid:1.
Further, the method for preparing vertical ordered carbon nanotube/polyaniline composite film that the present invention is provided, can also have
Such feature：Wherein, the concentration of CNT aqueous dispersions be 0.23mg/mL, polyaniline nano fiber aqueous dispersions it is dense
It is 0.15mg/mL to spend.
In addition, the method for preparing vertical ordered carbon nanotube/polyaniline composite film that the present invention is provided, can also have this
The feature of sample：Wherein, the voltage for applying on filter paper is 250V.
<Scheme two>
The present invention also provides a kind of suction filtration-electric field arrangement, for passing through<Scheme one>Any one of method by carbon
The mix moisture dispersion liquid of nanotube and polyaniline is prepared into vertical ordered carbon nanotube/polyaniline composite film, it is characterised in that bag
Include：Body, the body is for hollow structure and upper end is provided with opening, mix moisture dispersion liquid is entered body by opening；Funnel,
Entrance is connected with the lower end of body, and outlet is downward；Liquid storage bottle, is connected positioned at funnel lower section and with the outlet of funnel；Vavuum pump,
It is connected with liquid storage bottle, for providing negative pressure to liquid storage bottle；Core, is fixed on intrinsic middle part；Filter paper, is fixed on core
Upper surface, for carrying CNT and polyaniline；Two electrodes, are fixed in body, respectively positioned at the top of filter paper with
Side, forms the electric field perpendicular to filter paper, allows CNT to be orientated on polyaniline；AC power, the two of the AC power
Pole is connected by wire with an electrode respectively, and electric current is provided to form electric field to electrode, wherein, body is polymethylacrylic acid
What methyl esters was made, the distance of each electrode to filter paper can adjust.
Further, suction filtration-electric field arrangement provided by the present invention, can also have the feature that：Wherein, electrode is aluminium
Electrode.
Further, suction filtration-electric field arrangement provided by the present invention, can also have the feature that：Each electrode to filter
The distance of paper is equal, and the distance is 9~30cm.
The effect of invention and effect
According to the method and apparatus for preparing carbon nano-tube/poly aniline composite membrane provided by the present invention, because in suction filtration-electricity
The mix moisture dispersion liquid of CNT and polyaniline is added in field device, and applies the electric field perpendicular to filter paper direction so that filter
CNT and polyaniline on paper are subject to the collective effect of suction filtration effect and electric field, therefore prepare carbon using the method and device
Nanotube/polyaniline composite film, can not only be such that CNT is evenly dispersed in polyaniline, form orthogonal array, moreover it is possible to
Enough make CNT that the degree of order very high is obtained in the presence of electric field.The method is simple to operate, with low cost.
Brief description of the drawings
Fig. 1 is the structural representation of suction filtration-electric field arrangement of the invention；
Fig. 2 is the section SEM image of CNTs/PANi composite membranes prepared by embodiment two；
Fig. 3 is the section SEM image of CNTs/PANi composite membranes prepared by embodiment three；
Fig. 4 is the section SEM image of CNTs/PANi composite membranes prepared by example IV；
Fig. 5 is the section SEM image of CNTs/PANi composite membranes prepared by embodiment five；And
Fig. 6 is the section SEM image of CNTs/PANi composite membranes prepared by comparative example.
Specific embodiment
Below in conjunction with accompanying drawing, the method and apparatus for preparing carbon nano-tube/poly aniline composite membrane provided by the present invention are made
Elaborate.
<Embodiment one>
Fig. 1 is the structural representation of suction filtration-electric field arrangement of the invention.
As shown in figure 1, the present invention provide suction filtration-electric field arrangement 10 include body 11, funnel 12, core 13, cushion block 14,
Filter paper 15, aluminium electrode 16, aluminium electrode 17, AC power 18, wire 19, wire 20, liquid storage bottle (not shown) and vacuum
Pump (not shown).
Body 11 is hollow structure, is obtained by polymethyl methacrylate.The upper end of body 11 is provided with opening, makes CNT
Mix moisture dispersion liquid 21 with polyaniline enters body 11 by opening.
Funnel 12 is connected to the lower end of body 11, is connected with body 11, with downward outlet.
Core 13 is arranged on the middle part in body 11.
Cushion block 14 is fixed on the middle part in body 11, for installing core 13.
Filter paper 15 is fixed on the upper surface of core 13, for being held during carbon nano-tube/poly aniline composite membrane is prepared
Carry CNT and polyaniline nano fiber.
Aluminium electrode 16 and aluminium electrode 17 are located inside body 11, are separately positioned on above and below filter paper 15, are formed and hung down
Directly in the electric field of filter paper 15.Aluminium electrode 16 is equal with the distance of aluminium electrode 17 to filter paper 15, can be adjusted in the range of 9~30cm
Section.
AC power 18 is arranged on outside body 11, respectively by wire 19 and wire 20 and aluminium electrode 16 and aluminium electrode 17
It is connected.
Liquid storage bottle (not shown) is located at the lower section of funnel 12, and the outlet with funnel 12 is connected, is used during suction filtration
In the water that storage is pumped out from body 11.
Vavuum pump (not shown) is connected with liquid storage bottle (not shown), and negative pressure is provided to liquid storage bottle, so that will
Water in body 11 is pumped in liquid storage bottle.
<Embodiment two>
Using<Embodiment one>In suction filtration-electric field arrangement 10 prepare carbon nano-tube/poly aniline composite membrane, preparation method
Comprise the following steps：
Step one, prepares mix moisture dispersion liquid.
Acidification is carried out to CNT (CNTs) first, the method for acidification can refer to document J.Liu,
A.G.Rinzler,H.Dai.Fullerene pipes[J].Science,1998,280,1253-1256.In the present embodiment,
A diameter of 1~the 2nm of single wall CNTs after acidification, length is about 1 μm.Then polyaniline is prepared using chemical oxidative polymerization
(PANi) nanofiber, preparation method such as document H.D.Tran, Y.Wang, J.M.D ' Arcy, et al.Toward an
understanding of the formation of conducting polymer nanofibers[J].ACS NANO,
2008,2(9):Described in 1841-1848.In the present embodiment, the diameter of the PANi nanofibers for being prepared using the above method is about
40nm, length is about 300nm.
The CNTs after acidification is taken, the CNTs aqueous dispersions that concentration is 0.23mg/mL are configured to, PANi nanofibers are taken
It is configured to the PANi nanofiber aqueous dispersions that concentration is 0.15mg/mL.By CNTs aqueous dispersions and PANi nanofiber moisture
Dispersion liquid mixes, and is configured to mixed liquor, and makes the mass ratio of CNTs and PANi nanofibers in mixed liquor be 5:1, CNTs and PANi
The gross mass of nanofiber is about 20mg.
By the ultrasonically treated 4h of above-mentioned mixed liquor, then mechanical agitation 30min, it is well mixed CNTs and PANi nanofibers,
Obtain mix moisture dispersion liquid.
Step 2, suction filtration and electric field synergistic prepare carbon nano-tube/poly aniline composite membrane.
Take the 300mL mix moisture dispersion liquids that step one obtains to pour into the body 11 of suction filtration-electric field arrangement 10, exchange is set
The voltage of power supply 18 is 250V, and regulation aluminium electrode 16 and aluminium electrode 17 are 9mm, the suction filtration work(of vavuum pump to the distance of filter paper 15
Rate is 180W.Vavuum pump and AC power 18 are opened, suction filtration is carried out to mix moisture dispersion liquid in the presence of electric field.Suction filtration terminates
After close vavuum pump, AC power 18 continues on 24h, is then shut off AC power 18, takes out filter paper 15, dries naturally.
Vavuum pump provides negative pressure to liquid storage bottle, and the water in mix moisture dispersion liquid in body 11 is pumped into liquid storage bottle, CNTs
It is deposited in the presence of suction filtration on filter paper 15 with PANi nanofibers.In the common of the suction force perpendicular to filter paper 15 and electric field
Under effect, CNTs along direction of an electric field it is vertical it is orderly and dispersed be arranged on PANi nanofibers, obtained after drying
CNTs/PANi composite membranes.
After preparing CNTs/PANi composite membranes, the method embedded using epoxy prepares the profile scanning Electronic Speculum of composite membrane
(SEM) sample, step is as follows：First, 30g epoxies are taken, curing agent 4-4- diaminodiphenyl-methanes (curing agent quality point is added
30%) number about, adds a certain amount of acetone and fully dissolves mixture, is uniformly dispersed, and obtains embedding medium.Take a small amount of above-mentioned
Embedding medium fully embeds CNTs/PANi composite membranes, the precuring 1h at 60 DEG C, then solidifies 3h at 80 DEG C, obtains CNTs/
The epoxy resin embedding sample of PANi composite membranes.Then the brittle failure in liquid nitrogen by above-mentioned embedded samples, the metal spraying on sample section,
Obtain the section SEM samples of CNTs/PANi composite membranes.
Fig. 2 is the section SEM image of CNTs/PANi composite membranes prepared by embodiment two.
As shown in Fig. 2 the thickness of CNTs/PANi composite membranes manufactured in the present embodiment is about 20 μm, and in composite membrane
CNTs forms orthogonal array along perpendicular to the direction of composite film surface, and distributes very evenly.
<Embodiment three>
In the present embodiment, the step of preparing CNTs/PANi composite membranes is identical with embodiment two, but by the He of aluminium electrode 16
Aluminium electrode 17 is adjusted to 12mm to the distance of filter paper 15.
Fig. 3 is the section SEM image of CNTs/PANi composite membranes prepared by embodiment three；
As shown in figure 3, the thickness of CNTs/PANi composite membranes manufactured in the present embodiment is about 20 μm, CNTs is uniformly dispersed
In composite film surface, but compared with embodiment two, CNTs decreases in the degree of order arranged perpendicular to composite film surface.
<Example IV>
In the present embodiment, the step of preparing CNTs/PANi composite membranes is identical with embodiment two, keeps mixing water dispersion
The mass ratio 5 of CNTs and PANi nanofibers in liquid:1 is constant, makes the total of CNTs and PANi nanofibers in mix moisture dispersion liquid
Quality is 10mg, and the voltage that AC power 18 is adjusted during step 2 prepares composite membrane is 200V.
Fig. 4 is the section SEM image of CNTs/PANi composite membranes prepared by example IV.
As shown in figure 4, the thickness of CNTs/PANi composite membranes manufactured in the present embodiment is about 10 μm, CNTs exists in composite membrane
Arrangement on the direction of composite membrane is more in disorder, and the degree of order is substantially reduced.
<Embodiment five>
In the present embodiment, the step of preparing CNTs/PANi composite membranes is identical with embodiment two, but in step 2
The voltage for adjusting AC power 18 is 100V.
Fig. 5 is the section SEM image of CNTs/PANi composite membranes prepared by embodiment five.
As shown in figure 5, the thickness of CNTs/PANi composite membranes manufactured in the present embodiment is about 10 μm, voltage is reduced to 100V
Afterwards, the CNTs in CNTs/PANi composite membranes is significantly reduced in the arrangement perpendicular to composite membrane direction, and the arrangement degree of order is poor.
<Comparative example>
Step one, prepares mix moisture dispersion liquid.In this comparative example, the preparation method of mix moisture dispersion liquid is with embodiment two.
Step 2, suction method prepares CNTs/PANi composite membranes.The 300mL mix moisture dispersion liquids that step one obtains are taken to pour into
In the body 11 of suction filtration-electric field arrangement 10, the suction filtration power for setting vavuum pump is 180W.Vavuum pump is opened, mixing water is disperseed
Liquid carries out suction filtration.Suction filtration closes vavuum pump after terminating, take out filter paper 15, dries naturally, obtains CNTs/PANi composite membranes.
Fig. 6 is the section SEM image of CNTs/PANi composite membranes prepared by comparative example.
The method embedded using epoxy prepares the section SEM samples of CNTs/PANi composite membranes, shoots SEM image such as Fig. 6 institutes
Show.It can be seen that the thickness of the CNTs/PANi composite membranes of this comparative example preparation is about 20 μm.CNTs/PANi prepared by suction method is combined
CNTs is evenly distributed in film, but most of directions along parallel to composite membrane arrange, only the small part at filter paper 15
CNTs is arranged along perpendicular to the direction of composite membrane.
The effect of embodiment and effect
According to the method and apparatus for preparing CNTs/PANi composite membranes of embodiment one~five, because in suction filtration-electric field arrangement
It is middle to add the mix moisture dispersion liquid of CNT and polyaniline, and apply the electric field perpendicular to filter paper direction so that on filter paper
CNT and polyaniline are subject to the collective effect of suction filtration and electric field, therefore prepare carbon nano-tube/poly using the method and device
Aniline composite membrane, can not only be such that CNT is evenly dispersed in polyaniline, form orthogonal array, additionally it is possible to make carbon nanometer
Pipe obtains the degree of order very high in the presence of electric field.The method is simple to operate, with low cost.
Comparative example two and embodiment three are visible, the distance of two aluminium electrodes of increase to filter paper, though do not influence CNTs/
The thickness of PANi composite membranes and the dispersiveness of CNTs, but can cause the degree of order of CNTs to reduce.
Comparative example two and example IV, embodiment five are visible, and the voltage applied in two aluminium electrodes is higher, then filter
The electric field action that CNTs and PANi on paper are subject to is bigger so that CNTs/PANi composite film thickness is bigger, and in composite membrane
The degree of order of CNTs is better.
The basic explanation under present inventive concept is these are only, the protection domain being not intended to limit the present invention.
Claims (5)
1. a kind of method for preparing vertical ordered carbon nanotube/polyaniline composite film, it is characterised in that comprise the following steps：
Mix moisture dispersion liquid step is prepared, acidification is carried out to CNT, the CNT after the acidification is matched somebody with somebody
CNT aqueous dispersions are set to, polyaniline nano fiber is then configured to polyaniline nano fiber aqueous dispersions, then will
The CNT aqueous dispersions and the polyaniline nano fiber aqueous dispersions mix, ultrasonic 4h, then mechanical agitation 30min,
Obtain mix moisture dispersion liquid；
Suction filtration and electric field synergistic prepare carbon nano-tube/poly aniline composite membrane step, and the mix moisture dispersion liquid is poured into suction filtration-electricity
Field device, applies the voltage perpendicular to the filter paper on the filter paper of the suction filtration-electric field arrangement, and the voltage is 250V, regulation
The suction filtration power of the suction filtration-electric field arrangement is 180W, and the synergy of electric field and suction filtration is applied to the mix moisture dispersion liquid,
The voltage 24h is continued to after the suction filtration terminates, then the filter paper is taken out, obtained after drying naturally in the filter
The carbon nano-tube/poly aniline composite membrane deposited on paper,
Wherein, CNT described in the mix moisture dispersion liquid and the mass ratio of the polyaniline nano fiber are 5:1.
2. the method for preparing vertical ordered carbon nanotube/polyaniline composite film according to claim 1, it is characterised in that：
Wherein, the concentration of the CNT aqueous dispersions be 0.23mg/mL, the polyaniline nano fiber aqueous dispersions it is dense
It is 0.15mg/mL to spend.
3. a kind of suction filtration-electric field arrangement, for by the method described in claim 1 or 2 by the mixed of CNT and polyaniline
Heshui dispersion liquid is prepared into vertical ordered carbon nanotube/polyaniline composite film, it is characterised in that including：
Body, the body is for hollow structure and upper end is provided with opening, the mix moisture dispersion liquid is passed through the opening and enters
The body；
Funnel, entrance is connected with the lower end of the body, and outlet is downward；
Liquid storage bottle, is connected positioned at funnel lower section and with the outlet of the funnel；
Vavuum pump, is connected with the liquid storage bottle, for providing negative pressure to the liquid storage bottle；
Core, is fixed on the intrinsic middle part；
Filter paper, is fixed on the upper surface of the core, for carrying the CNT and the polyaniline；
Two electrodes, are fixed in the body, respectively above and below the filter paper, are formed perpendicular to the filter paper
Electric field, allow the CNT to be orientated on the polyaniline；
AC power, the two poles of the earth of the AC power are connected by wire with an electrode respectively, and electricity is provided to the electrode
Flow to form the electric field,
Wherein, the body is that polymethyl methacrylate is made,
Each described electrode can adjust to the distance of the filter paper.
4. suction filtration-electric field arrangement according to claim 3, it is characterised in that：
Wherein, the electrode is aluminium electrode.
5. suction filtration-the electric field arrangement according to claim 3 or 4, it is characterised in that：
Wherein, the distance of each electrode to filter paper is equal, and the distance is 9~30cm.
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| CN104787748B (en) * | 2015-04-28 | 2016-11-02 | 南京工业大学 | A kind of preparation method of orthotropic opening carbon nano-tube film |
| CN105241944B (en) * | 2015-09-25 | 2017-10-31 | 浙江大学 | The method of antibiotic in Electrochemical Detection milk based on the vertical enrichment of micella in order |
| CN107541996A (en) * | 2016-06-25 | 2018-01-05 | 董晓 | A kind of preparation method of modified carbon nano-tube electromagnetic shielding paper |
| US11583808B2 (en) | 2018-12-18 | 2023-02-21 | Dalian University Of Technology | Method of preparation of conductive polymer/carbon nanotube composite nanofiltration membrane and the use thereof |
| CN109821418B (en) * | 2019-03-29 | 2021-03-02 | 天津工业大学 | Oriented carbon nanotube-based membrane, interfacial polymerization nanofiltration membrane using same and preparation method thereof |
| CN110862470B (en) * | 2019-12-02 | 2022-08-16 | 上海深化实业有限公司 | Devolatilization method of polyvinyl chloride resin for paste |
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| CN101429336A (en) * | 2008-10-30 | 2009-05-13 | 上海应用技术学院 | Process for producing carbon nano-tube/polyaniline conductive composite material |
| CN101654555A (en) * | 2008-08-22 | 2010-02-24 | 清华大学 | Method for preparing carbon nano tube/conducting polymer composite material |
| CN102558554A (en) * | 2012-01-09 | 2012-07-11 | 上海理工大学 | Carbon nano tube reinforced polyaniline nano-fiber and preparing method thereof |
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| CN101654555A (en) * | 2008-08-22 | 2010-02-24 | 清华大学 | Method for preparing carbon nano tube/conducting polymer composite material |
| CN101429336A (en) * | 2008-10-30 | 2009-05-13 | 上海应用技术学院 | Process for producing carbon nano-tube/polyaniline conductive composite material |
| CN102558554A (en) * | 2012-01-09 | 2012-07-11 | 上海理工大学 | Carbon nano tube reinforced polyaniline nano-fiber and preparing method thereof |
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