CN106916255A - A kind of preparation method of novel C e PPy/PMMA nano core-shell composite conducting materials - Google Patents
A kind of preparation method of novel C e PPy/PMMA nano core-shell composite conducting materials Download PDFInfo
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- CN106916255A CN106916255A CN201710226274.6A CN201710226274A CN106916255A CN 106916255 A CN106916255 A CN 106916255A CN 201710226274 A CN201710226274 A CN 201710226274A CN 106916255 A CN106916255 A CN 106916255A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/0605—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms
- C08G73/0611—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms with only one nitrogen atom in the ring, e.g. polypyrroles
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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- H01G11/30—Electrodes characterised by their material
- H01G11/48—Conductive polymers
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- H—ELECTRICITY
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- H01M4/02—Electrodes composed of, or comprising, active material
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Abstract
The invention discloses a kind of preparation method of novel C e PPy/PMMA nano core-shell composite conducting materials, with Ben-zylphenol Polyoxyethyl Ether emulsifying agent, pyrroles, n-butanol, the raw materials such as MMA pass through the operational means such as ultrasonic wave, magnetic agitation and prepare novel C e PPy/PMMA nano core-shell composites.
Description
Technical field
The present invention relates to a kind of preparation method of novel C e-PPy/PMMA nano core-shell composite conducting materials, belong to Material Field.
Background technology
In conducting polymer family, with π, often the PPy of structure has synthesis letter compared with other conducting polymers altogether
Singly, the advantages of environmental stability is good, electrical conductivity is high, causes the extensive concern of people.At present, researcher has found PPy
Have tempting at aspects such as gas sensor, solar cell, ultracapacitor, secondary cell, anticorrosive paint and photoelectric devices
Application prospect.It is in water and nearly all organic but its dissolubility of the PPy of chemical synthesis or electrochemistry formated is all very poor
All it is difficult to dissolve in solvent, machinability is poor, dispersion domestic animal is poor, and these defects seriously limit the large-scale application of PPy.Solve this
The effective method of of one problem is that PPy is combined with thermoplastic polymer.Cairns et al. deposits PPy by PS microballoons
Method synthesized PS/PPy compound particles, and find that the PPy prepared by the method is discontinuous particle, grain on PS surfaces
Footpath is about in 20 ~ 30 nm.Wang et al. PPy shells in PSS surfaces successful polymerization, and find the PSS molecules of sulfonation layer not
Have completely with PS copolymerization, part PSS molecules are through PPy shells so that the water dispersible of gained composite is greatly improved.Xu
Et al. PS/PPy nano core-shell composites have been synthesized by microemulsion method, and find to be configured using polymerisable surfactant
The colloidal stability and electrical conductivity of the PS/PPy composites prepared by microemulsion system are superior to using non-polymeric surface-active
Agent.Jiang et al. is prepared by the use of cruel (PMMA) Core-shell Composite Particles of the poly- methacrylate first of PPy/ as conductive filler
PMMA transparent membranes, research finds that PMMA shells improve the compatibility of complex conductive fillerses and PMMA matrixes, so as to improve
Dispersiveness of the PPy conductive fillers in PMMA.And I have invented a kind of system of novel C e-PPy/PMMA nano core-shell composites
Preparation Method, improvement is made that in prior synthesizing method, and introduces rare element improves property, the Ce-PPy/PMMA for obtaining
Nano core-shell composite dissolving property electric conductivity is all good.
The content of the invention
For the problem that above-mentioned prior art is present, the present invention provides a kind of novel C e-PPy/PMMA nano core-shells and is combined
The preparation method of conductive material.
To achieve these goals, the technical solution adopted by the present invention is:A kind of novel C e-PPy/PMMA nano core-shells are answered
The preparation method of condensation material.Comprise the following steps:
Step 1, infrared treatment 2h is carried out to Ben-zylphenol Polyoxyethyl Ether emulsifying agent first;
Step 2 and then base phenol polyethenoxy ether emulsifying agent is transferred in there-necked flask, while adding deionized water, also pyrrole
Cough up, at room temperature magnetic agitation reaction 3h;
Step 3 and then hydrogen peroxide is added drop-wise to wherein, is added dropwise with per minute 20 drop speed, magnetic agitation 3h is obtained when being added dropwise
Latax;
After step 4, dropwise addition stirring terminate, methyl alcohol is added to be demulsified, products therefrom is centrifuged, deionized water washing;
Step 5, centrifugation, after washing terminates, products therefrom are transferred to 12h to constant weight are dried in vacuum drying chamber, obtain nanometer
Level ppy;
Step 6, obtained nanoscale ppy is transferred in there-necked flask, is subsequently adding MMA, and deionized water, then carried out
Ultrasonication 2h;
Step 7 and then cerous nitrate is added, be warmed up to 50 DEG C, while opening magnetic agitation oil bath reaction 4h;
Step 8, it is then transferred into the reactor of polytetrafluoroethylene (PTFE), carries out Hydrothermal Synthesiss, is put into air dry oven 150
DEG C, react 8h under 0.2kpa;
After step 9, reaction terminate, deionized water washing is carried out to product, then separated in centrifuge, be then transferred to
120 DEG C of dryings finally give novel C e-PPy/PMMA nano core-shell composites to the general 12h of constant weight in vacuum drying chamber.
Beneficial effect:A kind of preparation method of novel C e-PPy/PMMA nano core-shell composite conducting materials of the present invention, should
Method is simple to operate, and raw material is relatively easily obtained, and is acted synergistically by the proportioning of the selection consumption of different material and further enhanced
The generation of active group, process carries out micro emulsion method synthesis ppy using emulsifying agent is added in preparation process, also helps and obtains
Nanosized product, is finally carrying out the formation that Hydrothermal Synthesiss are conducive to product with ptfe autoclave, is also beneficial to improve
Electric conductivity and its dispersiveness.Wherein embodiment 1 is produced to Ben-zylphenol Polyoxyethyl Ether emulsifying agent, cerous nitrate mass ratio 20:3
Sample.Ben-zylphenol Polyoxyethyl Ether emulsifying agent 2g, cerous nitrate 0.3g, pyrroles 1.2g, hydrogen peroxide 8g, deionized water 200ml,
MMA1.8g, methyl alcohol 120ml.And embodiment 2 is produced to Ben-zylphenol Polyoxyethyl Ether emulsifying agent, cerous nitrate mass ratio 45:8
Sample.Ben-zylphenol Polyoxyethyl Ether emulsifying agent 4.5g, cerous nitrate 0.8g, other raw material dosages, operating procedure is with embodiment 1 one
Sample.Its electrical conductivity of novel C e-PPy/PMMA nano core-shells composite obtained in the two embodiments, dispersiveness is best in water.
Specific embodiment
Embodiment 1 is produced to Ben-zylphenol Polyoxyethyl Ether emulsifying agent, cerous nitrate mass ratio 20:3 sample.Benzylphenol polyoxy second
Alkene ether emulsifying agent 2g, cerous nitrate 0.3g, pyrroles 1.2g, hydrogen peroxide 8g, deionized water 200ml, MMA1.8g, methyl alcohol 120ml
Step 1, infrared treatment 2h is carried out to 2g Ben-zylphenol Polyoxyethyl Ethers emulsifying agent first;
Step 2 and then base phenol polyethenoxy ether emulsifying agent is transferred in there-necked flask, while 100ml deionized waters are added, also
There is 1.2g pyrroles, at room temperature magnetic agitation reaction 3h;
Step 3 and then 8g hydrogen peroxide is added drop-wise to wherein, is added dropwise with per minute 20 drop speed, magnetic agitation 3h is obtained when being added dropwise
To latax;
After step 4, dropwise addition stirring terminate, 120ml methyl alcohol is added to be demulsified, products therefrom is centrifuged, deionized water
Washing;
Step 5, centrifugation, after washing terminates, products therefrom are transferred to 12h to constant weight are dried in vacuum drying chamber, obtain nanometer
Level ppy;
Step 6, obtained nanoscale ppy is transferred in there-necked flask, is subsequently adding 1.2gMMA, and 100ml deionizations
Water, then carries out ultrasonication 2h;
Step 7 and then 0.3g cerous nitrates are added, be warmed up to 50 DEG C, while opening magnetic agitation oil bath reaction 4h;
Step 8, it is then transferred into the reactor of polytetrafluoroethylene (PTFE), carries out Hydrothermal Synthesiss, is put into air dry oven 150
DEG C, react 8h under 0.2kpa;
After step 9, reaction terminate, deionized water washing is carried out to product, then separated in centrifuge, be then transferred to
120 DEG C of dryings finally give novel C e-PPy/PMMA nano core-shell composites to the general 12h of constant weight in vacuum drying chamber.
Embodiment 2 is produced to Ben-zylphenol Polyoxyethyl Ether emulsifying agent, cerous nitrate mass ratio 45:8 sample.Benzylphenol polyoxy second
Alkene ether emulsifying agent 4.5g, cerous nitrate 0.8g, other raw material dosages, operating procedure is as embodiment 1.
Embodiment 3 is produced to Ben-zylphenol Polyoxyethyl Ether emulsifying agent, cerous nitrate mass ratio 21:3 sample.Benzylphenol polyoxy
Vinethene emulsifying agent 2.1g, cerous nitrate 0.3g, other raw material dosages, operating procedure is as embodiment 1.
Embodiment 4 is produced to Ben-zylphenol Polyoxyethyl Ether emulsifying agent, cerous nitrate mass ratio 22:3 sample.Benzylphenol polyoxy second
Alkene ether emulsifying agent 2.2g, cerous nitrate 0.3g, operating procedure is as embodiment 1.
Embodiment 5 is produced to Ben-zylphenol Polyoxyethyl Ether emulsifying agent, cerous nitrate mass ratio 23:3 sample.Benzylphenol polyoxy second
Alkene ether emulsifying agent 2.3g, cerous nitrate 0.3g, other raw material dosages, operating procedure is as embodiment 1.
Embodiment 6 is produced to Ben-zylphenol Polyoxyethyl Ether emulsifying agent, cerous nitrate mass ratio 24:3 sample.Benzylphenol polyoxy second
Alkene ether emulsifying agent 2.4g, cerous nitrate 0.3g, other raw material dosages, operating procedure is as embodiment 1.
Embodiment 7 is produced to Ben-zylphenol Polyoxyethyl Ether emulsifying agent, cerous nitrate mass ratio 25:3 sample.Benzylphenol polyoxy second
Alkene ether emulsifying agent 2.5g, cerous nitrate 0.3g, other raw material dosages, operating procedure is as embodiment 1.
Embodiment 8 is produced to Ben-zylphenol Polyoxyethyl Ether emulsifying agent, cerous nitrate mass ratio 26:3 sample.Benzylphenol polyoxy second
Alkene ether emulsifying agent 2.6g, cerous nitrate 0.3g, other raw material dosages, operating procedure is as embodiment 1.
Embodiment 9 is produced to Ben-zylphenol Polyoxyethyl Ether emulsifying agent, cerous nitrate mass ratio 27:3 sample.Benzylphenol polyoxy second
Alkene ether emulsifying agent 2.7g, cerous nitrate 0.3g, other raw material dosages, operating procedure is as embodiment 1.
Embodiment 10 is produced to Ben-zylphenol Polyoxyethyl Ether emulsifying agent, cerous nitrate mass ratio 19:3 sample.Benzylphenol polyoxy
Vinethene emulsifying agent 19g, cerous nitrate 0.3g, other raw material dosages, operating procedure is as embodiment 1.
Embodiment 11 is produced to Ben-zylphenol Polyoxyethyl Ether emulsifying agent, cerous nitrate mass ratio 18:3 sample.Benzylphenol polyoxy
Vinethene emulsifying agent 1.8g, cerous nitrate 0.3g, other raw material dosages, operating procedure is as embodiment 1.
Embodiment 12 is produced to Ben-zylphenol Polyoxyethyl Ether emulsifying agent, cerous nitrate mass ratio 17:3 sample.Benzylphenol polyoxy
Vinethene emulsifying agent 1.7g, cerous nitrate 0.3g, other raw material dosages, operating procedure is as embodiment 1.
Reference examples 1 are produced to Ben-zylphenol Polyoxyethyl Ether emulsifying agent, cerous nitrate mass ratio 20:3 sample.Ben-zylphenol Polyoxyethyl Ether
Emulsifying agent 2g, cerous nitrate 0.3g, do not carry out ultrasonication, other raw material dosages, and operating procedure is as embodiment 1.
Reference examples 2 are produced to Ben-zylphenol Polyoxyethyl Ether emulsifying agent, cerous nitrate mass ratio 20:3 sample.Benzylphenol polyoxy second
Alkene ether emulsifying agent 2g, cerous nitrate 0.3g, do not carry out magnetic agitation, but mechanical agitation, other raw material dosages, operating procedure with
As embodiment 1.
Reference examples 3 are produced to Ben-zylphenol Polyoxyethyl Ether emulsifying agent, cerous nitrate mass ratio 20:3 sample.Benzylphenol polyoxy second
Alkene ether emulsifying agent 2g, cerous nitrate 0.3g, add cerous nitrate not carry out being warming up to 50 DEG C, and are to continue with room temperature reaction, other raw materials
Consumption, operating procedure is as embodiment 1.
Reference examples 4 are produced to Ben-zylphenol Polyoxyethyl Ether emulsifying agent, cerous nitrate mass ratio 20:3 sample.Benzylphenol polyoxy
Vinethene emulsifying agent 2g, cerous nitrate 0.3g, are not carried out at 150 DEG C during Hydrothermal Synthesiss under 0.2kpa, but at 200 DEG C,
Carried out under 0.2kpa, other raw material dosages, operating procedure is as embodiment 1.
Embodiment 5 is produced to Ben-zylphenol Polyoxyethyl Ether emulsifying agent, cerous nitrate mass ratio 20:3 sample.Benzylphenol polyoxy second
Alkene ether emulsifying agent 2g, cerous nitrate 0.3g, pyrroles 1.2g, hydrogen peroxide 8g, deionized water 200ml, MMA1.8g, methyl alcohol 120ml
Step 1, infrared treatment 2h is carried out to 2g Ben-zylphenol Polyoxyethyl Ethers emulsifying agent first;
Step 2 and then base phenol polyethenoxy ether emulsifying agent is transferred in there-necked flask, while 100ml deionized waters are added, also
There is 1.2g pyrroles, at room temperature magnetic agitation reaction 3h;
Step 3 and then 8g hydrogen peroxide is added drop-wise to wherein, is added dropwise with per minute 20 drop speed, magnetic agitation 3h is obtained when being added dropwise
To latax;
After step 4, dropwise addition stirring terminate, 120ml methyl alcohol is added to be demulsified, products therefrom is centrifuged, deionized water
Washing;
Step 5, centrifugation, after washing terminates, products therefrom are transferred to 12h to constant weight are dried in vacuum drying chamber, obtain nanometer
Level ppy;
Step 6, obtained nanoscale ppy is transferred in there-necked flask, is subsequently adding 1.2gMMA, and 100ml deionizations
Water, then carries out ultrasonication 2h;
Step 8, it is then transferred into the reactor of polytetrafluoroethylene (PTFE), carries out Hydrothermal Synthesiss, is put into air dry oven 150
DEG C, react 8h under 0.2kpa;
After step 9, reaction terminate, deionized water washing is carried out to product, then separated in centrifuge, be then transferred to
120 DEG C of dryings finally give PPy/PMMA nano core-shell composites to the general 12h of constant weight in vacuum drying chamber.
Control group 61 is produced to Ben-zylphenol Polyoxyethyl Ether emulsifying agent, cerous nitrate mass ratio 20:3 sample.Benzyl phenol polyethenoxy
Ether emulsifying agent 2g, cerous nitrate 0.3g, pyrroles 1.2g, hydrogen peroxide 8g, deionized water 200ml, MMA1.8g, methyl alcohol 120ml
Step 1, infrared treatment 2h is carried out to 2g Ben-zylphenol Polyoxyethyl Ethers emulsifying agent first;
Step 2 and then base phenol polyethenoxy ether emulsifying agent is transferred in there-necked flask, while 100ml deionized waters are added, also
There is 1.2g pyrroles, at room temperature magnetic agitation reaction 3h;
Step 3 and then 8g hydrogen peroxide is added drop-wise to wherein, is added dropwise with per minute 20 drop speed, magnetic agitation 3h is obtained when being added dropwise
To latax;
After step 4, dropwise addition stirring terminate, 120ml methyl alcohol is added to be demulsified, products therefrom is centrifuged, deionized water
Washing;
Step 5, centrifugation, after washing terminates, products therefrom are transferred to 12h to constant weight are dried in vacuum drying chamber, obtain nanometer
Level ppy;
Step 6, obtained nanoscale ppy is transferred in there-necked flask, is subsequently adding 1.2gMMA, and 100ml deionizations
Water, then carries out ultrasonication 2h;
Step 7 and then 0.3g cerous nitrates are added, be warmed up to 50 DEG C, while opening magnetic agitation oil bath reaction 4h;
Step 8 and then it is put into air dry oven at 150 DEG C, 8h is reacted under 0.2kpa;
After step 9, reaction terminate, deionized water washing is carried out to product, then separated in centrifuge, be then transferred to
120 DEG C of dryings finally give novel C e-PPy/PMMA nano core-shell composites to the general 12h of constant weight in vacuum drying chamber.
Test method:The present invention is surveyed using the probe resistance rate of the KDY-1 types four/sheet resistance of Guangzhou Kunder Science & Technology Co., Ltd.'s production
The novel C e-PPy/PMMA nano core-shell composites of examination instrument test synthesis, while observing dissolubility in its water.
The novel C e-PPy/PMMA nano core-shell Electrical Conductivity of Composites of table one, dispersed test result in water
Group | Electrical conductivity(S/cm) | Dispersiveness in water |
Embodiment 1 | 0.3389 | Dispersion effect is pretty good |
Embodiment 2 | 0.3295 | Dispersion effect is pretty good |
Embodiment 3 | 0.1756 | Dispersion effect is general |
Embodiment 4 | 0.1749 | Dispersion effect is general |
Embodiment 5 | 0.1868 | Dispersion effect is general |
Embodiment 6 | 0.1839 | Dispersion effect is general |
Embodiment 7 | 0.1842 | Dispersion effect is general |
Embodiment 8 | 0.1892 | Dispersion effect is general |
Embodiment 9 | 0.1731 | Dispersion effect is general |
Embodiment 10 | 0.1757 | Dispersion effect is general |
Embodiment 11 | 0.1890 | Dispersion effect is general |
Embodiment 12 | 0.1862 | Dispersion effect is general |
Reference examples 1 | 0.1396 | Dispersion effect is general |
Reference examples 2 | 0.1324 | Dispersion effect is general |
Reference examples 3 | 0.1398 | Dispersion effect is general |
Reference examples 4 | 0.1257 | Dispersion effect is general |
Reference examples 5 | 0.1273 | Dispersion effect is general |
Reference examples 6 | 0.1425 | Dispersion effect is general |
Test result indicate that:It can be found that novel C e-PPy/PMMA nano core-shells composite electricity obtained in the technique of embodiment 1,2
Conductance, dispersiveness preferably, illustrates proportioning of both techniques in raw material in water, and the operation synergy of technique is best.Contrast is real
Example 1, comparative example 1,2,3,4 are applied it can be found that not carrying out ultrasonic pretreatment, magnetic agitation is not carried out, adds cerous nitrate not carry out
50 DEG C are warming up to, and are to continue with room temperature reaction, do not carried out under 0.2kpa at 150 DEG C during Hydrothermal Synthesiss, but at 200 DEG C,
Obtained novel C e-PPy/PMMA nano core-shell Electrical Conductivity of Composites is carried out under 0.2kpa, dispersed effect is bad in water.
Control group 6 as can be seen that find carrying out the formation that Hydrothermal Synthesiss are conducive to product with ptfe autoclave,
Electric conductivity and its dispersiveness can be increased substantially.
Claims (4)
1. a kind of preparation method of novel C e-PPy/PMMA nano core-shell composite conducting materials, it is characterised in that poly- with benzylphenol
The raw materials such as oxygen vinethene emulsifying agent, pyrroles, n-butanol, MMA by ultrasonic wave, prepare new by the operational means such as magnetic agitation
Ce-PPy/PMMA nano core-shell composites.
2. a kind of preparation method of novel C e-PPy/PMMA nano core-shell composite conducting materials, it is characterised in that specially:
Step 1, infrared treatment 2h is carried out to Ben-zylphenol Polyoxyethyl Ether emulsifying agent first;
Step 2 and then base phenol polyethenoxy ether emulsifying agent is transferred in there-necked flask, while adding deionized water, also pyrrole
Cough up, at room temperature magnetic agitation reaction 3h;
Step 3 and then hydrogen peroxide is added drop-wise to wherein obtains latax;
After step 4, dropwise addition stirring terminate, methyl alcohol is added to be demulsified, products therefrom is centrifuged, deionized water washing;
Step 5, centrifugation, after washing terminates, products therefrom are transferred to 12h to constant weight are dried in vacuum drying chamber, obtain nanometer
Level ppy;
Step 6, obtained nanoscale ppy is transferred in there-necked flask, is subsequently adding MMA, and deionized water, then carried out
Ultrasonication 2h;
Step 7 and then cerous nitrate is added, be warmed up to 50 DEG C, while opening magnetic agitation oil bath reaction 4h;
Step 8 and then it is put into air dry oven at 150 DEG C, 8h is reacted under 0.2kpa;
After step 9, reaction terminate, deionized water washing is carried out to product, then separated in centrifuge, be then transferred to
120 DEG C of dryings finally give novel C e-PPy/PMMA nano core-shell composites to the general 12h of constant weight in vacuum drying chamber.
3. a kind of preparation method of Ce-PPy/PMMA nano core-shells composite conducting material according to claim 2, its feature
It is described step 8, also to include being transferred in the reactor of polytetrafluoroethylene (PTFE), carries out Hydrothermal Synthesiss.
4. a kind of preparation method of Ce-PPy/PMMA nano core-shells composite conducting material according to claim 2, its feature
It is described step 3, to be specially and be added drop-wise to wherein hydrogen peroxide, is added dropwise with per minute 20 drop speed, magnetic force is stirred when being added dropwise
Mix 3h and obtain latax.
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CN1880526A (en) * | 2005-06-13 | 2006-12-20 | 中国科学院化学研究所 | Ultra-hydrophobic conductive macromolecular nano fiber and method for preparing same and use thereof |
CN101942254A (en) * | 2010-09-29 | 2011-01-12 | 山东大学 | Aqueous conducting anti-corrosive paint containing nano core-shell structure polypyrrole |
CN102898669A (en) * | 2012-10-24 | 2013-01-30 | 西安科技大学 | Preparation method and device of conducting polypyrrole film |
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