CN105887234A - Preparation method of high-conductivity polypyrrole nano-fibers - Google Patents
Preparation method of high-conductivity polypyrrole nano-fibers Download PDFInfo
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- CN105887234A CN105887234A CN201410783356.7A CN201410783356A CN105887234A CN 105887234 A CN105887234 A CN 105887234A CN 201410783356 A CN201410783356 A CN 201410783356A CN 105887234 A CN105887234 A CN 105887234A
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Abstract
The invention relates to a preparation method of high-conductivity polypyrrole nano-fibers. Aiming at the disadvantages at the present that polypyrrole is difficult to dissolve, is difficult to machine and is not suitable for applying and the like, the method changes a polypyrrole chemical oxidization polymerization behavior and a polypyrrole nano-fiber assembling behavior by adopting critical micelle concentration of a special template agent in a solution and utilizing content of different acids and oxidants, so as to synthesize polypyrrole with a nano-fiber-shaped microscopic structure; and nano-fiber conductive powder with a special shape and a controllable long-diameter ratio is prepared and can be widely applied to sensors, conductive coatings, antistatic agents and the like.
Description
Technical field
The present invention relates to the preparation method of a kind of high connductivity polypyrrole nanofibers, belong to electrochemistry and photoelectricity skill
Art field.
Background introduction
Polypyrrole (PPy) as one of typical conducting polymer, have conductivity height, Heat stability is good,
The advantage of strong, the nontoxic and easy preparation of oxidative resistance, is widely used in battery, sensor, antistatic coating and half
Conducting electrons device.But, big π key-like the polypyrrole macromolecule become has the strongest chain rigidity, and
Intermolecular and molecular memory, at strong interaction of hydrogen bond, causes that polypyrrole is insoluble not to be melted, and this results in poly-
Pyrroles's difficulty processing, poor mechanical property, and can not biodegradation, this just limit its development with application.
In recent years, there is the conducting polymer of specific morphology, such as nanosphere, nano wire, nanotube, nanometer
Rod and nanofiber, receive much concern due to the performance of its uniqueness；And filamentous polypyrrole is due to its unique shape
Looks, compare that other patterns have higher electric conductivity, electro-chemical activity is higher, mechanical property is more excellent, in tree
Fat is more likely formed the reticulated conductive path contacted with each other, is obviously improved the electric property of coating, and can improve
The performances such as the mechanics of coating, thermodynamics, the polypyrrole therefore studying special appearance has great importance
Summary of the invention
Present invention aims to the deficiencies in the prior art, it is provided that a kind of high connductivity polypyrrole nanofibers
Preparation method, the method is for current polypyrrole indissoluble infusibility, it is difficult to processing, be unfavorable for application, utilize
The design synthesis of soft template agent has a polypyrrole of Nanowire shape microstructure, and preparation specific morphology, draw ratio can
Control receive fine conductive powder body, it can be widely applied to sensor, conductive coating, antistatic additive etc..
The technical scheme is that
Template agent and pyrrole monomer are dissolved in solvent orange 2 A, form blend solution, and regulate solution temperature and be
-20-50℃；Oxidant is dissolved in solvent B, forms oxidizing agent solution；It is added drop-wise to be blended by oxidizing agent solution again
In solution, after stirring reaction completely, after terminating reaction by solvent C, carry out washing, be centrifuged, dry,
Obtaining electrical conductivity eventually is 0.1-10S/cm-1, a diameter of 50-60nm, draw ratio be 200-500 a kind of structure,
The high connductivity polypyrrole nanofibers that draw ratio is controlled；
Wherein said template agent be Dodecyl trimethyl ammonium chloride, Tetradecyl Trimethyl Ammonium Bromide, 16
At least one in alkyl trimethyl ammonium bromide or didodecyldimethylammbromide bromide；
Wherein said solution A is at least one in water, acetonitrile or acetonitrile/water mixed solution；
Wherein said oxidant is Ammonium persulfate., potassium peroxydisulfate, hydrogen peroxide, trivalent iron salt or hydrogen peroxide/bivalence
At least one in iron salt；
Wherein said solvent B is water or concentration is in the hydrochloric acid of 0.1-2mol/L, glacial acetic acid or camphorsulfonic acid
At least one；
Wherein said solvent C is at least one in methanol, ethanol or isopropanol；
Wherein pyrrole monomer and oxidant mol ratio are (10-0.5): 1；
Wherein template agent consumption is (5-20) CMC (i.e. critical micelle concentration)；
Wherein detergent is ethanol/water mixed solvent, and volume ratio is (10-0.1): 1；Centrifugation rate is
3000-8000r/min, centrifugation time is 5-30min；Washing and centrifuge cycle 3-5 time.
Beneficial effects of the present invention: use soft mode version to form the microstructure of specific morphology at solution, use not
Change polypyrrole chemical oxidising polymerisation behavior and polypyrrole with acid, oxygenate content and receive the assembly behavior of fibre, from
And make the final polypyrrole microstructure arrived, draw ratio controlled, and there is higher electrical conductivity.
Detailed description of the invention
Following embodiment is in order to be more fully described the present invention program, but the invention is not limited in example institute
The scheme described.
Embodiment 1
In 500mL there-necked flask, 3mmol cetyl trimethylammonium bromide CTAB is dissolved in
In 150mL deionized water, 30min is stirred at room temperature；15mmol pyrrole monomer is added in CTAB solution,
After being stirred vigorously 1h, it is cooled to 0 DEG C in advance；Drip in dropping 7.5mmol ammonium persulfate aqueous solution 50mL, 30min
Complete, 0 DEG C of reaction 24h；Add 100mL methanol and terminate reaction.With ethanol and water mixed solution (volume ratio 1: 2)
Washing, 4000r/min is centrifuged 30min, and circulation is washed, is centrifuged until centrifugal upper liquid is water white transparency,
Black powdery microgranule, 50 DEG C are dried under vacuum to constant weight, and obtaining electrical conductivity is 2.67S/cm-1, a diameter of 50 nanometers,
Draw ratio be 400 polypyrrole receive fibre.
Embodiment 2
In 500mL there-necked flask, double for 5mmol Dodecyl trimethyl ammonium chloride DDAB are dissolved in
In 150mL acetonitrile/deionized water (volume ratio 1: 1), 20min is stirred at room temperature；15mmol pyrroles is single
Body is added in DDAB solution, after being stirred vigorously 0.6h, is heated to 30 DEG C；Dropping 30mmol ferric chloride
Hydrochloric acid solution (concentration is 0.1mol/L) 50mL, drips off in 30min, 30 DEG C of reaction 24h；Add 50mL
Isopropanol terminates reaction.Washing with ethanol and water mixed solution (volume ratio 2: 1), 5000r/min is centrifuged 20min,
Circulation is washed, is centrifuged until centrifugal upper liquid is water white transparency, obtains black powdery microgranule, 40 DEG C of vacuum drying
To constant weight, obtaining electrical conductivity is 1.55S/cm-1, a diameter of 60 nanometers, draw ratio be 300 polypyrrole receive fibre.
Embodiment 3
In 500mL there-necked flask, 4mmol Tetradecyl Trimethyl Ammonium Bromide TTAB is dissolved in
In 150mL acetonitrile, 30min is stirred at room temperature；15mmol pyrrole monomer is added in TTAB solution, acutely
After stirring 1.5h, it is cooled to-5 DEG C in advance；Dropping 15mmol ferrous sulfate/hydrogen peroxide-camphorsulfonic acid solution (concentration
For 0.2mol/L) 50mL, drip off in 30min ,-5 DEG C of reaction 24h；Add 75mL ethanol and terminate reaction.
Washing with ethanol and water mixed solution (volume ratio 1: 1), 6000r/min is centrifuged 10min, circulation washing, from
The heart, until centrifugal upper liquid is water white transparency, obtains black powdery microgranule, and 45 DEG C are dried under vacuum to constant weight, obtain electric
Conductance is 2.07S/cm-1, a diameter of 55 nanometers, draw ratio be 500 polypyrrole receive fibre.
Claims (2)
1. a preparation method for high connductivity polypyrrole nanofibers, its characterization step is:
Template agent and pyrrole monomer are dissolved in solvent orange 2 A, form blend solution, and regulate solution temperature and be-20-50 DEG C；Oxidant is dissolved in solvent B, forms oxidizing agent solution；Again oxidizing agent solution is added drop-wise in blend solution, after stirring reaction completely, after terminating reaction by solvent C, carries out washing, be centrifuged, dry, finally give the high connductivity polypyrrole nanofibers that structure, draw ratio are controlled；
Wherein said template agent is at least one in Dodecyl trimethyl ammonium chloride, Tetradecyl Trimethyl Ammonium Bromide, cetyl trimethylammonium bromide or didodecyldimethylammbromide bromide；
Wherein said solution A is at least one in water, acetonitrile or acetonitrile/water mixed solution；
Wherein said oxidant is at least one in Ammonium persulfate., potassium peroxydisulfate, hydrogen peroxide, trivalent iron salt or hydrogen peroxide/divalent iron salt；
Wherein said solvent B is water or concentration is at least one in the hydrochloric acid of 0.1-2mol/L, glacial acetic acid or camphorsulfonic acid；
Wherein said solvent C is at least one in methanol, ethanol or isopropanol；
Wherein pyrrole monomer and oxidant mol ratio are (10-0.5): 1；
Wherein template agent consumption is (5-20) CMC (i.e. critical micelle concentration)；
Wherein detergent is ethanol/water mixed solvent, and volume ratio is (10-0.1): 1；Centrifugation rate is 3000-8000r/min, and centrifugation time is 10-30min；Washing and centrifuge cycle 3-5 time.
2. the polypyrrole of the preparation method gained of a kind of high connductivity polypyrrole nanofibers as described in right 1 receives fibre, it is characterised in that: electrical conductivity is 0.1-10S/cm-1, a diameter of 50-60nm, draw ratio is 200-500.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410783356.7A CN105887234A (en) | 2014-12-15 | 2014-12-15 | Preparation method of high-conductivity polypyrrole nano-fibers |
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| CN201410783356.7A CN105887234A (en) | 2014-12-15 | 2014-12-15 | Preparation method of high-conductivity polypyrrole nano-fibers |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108565040A (en) * | 2018-05-04 | 2018-09-21 | 芜湖天科生物科技有限公司 | A kind of whisker type battery conductive material and preparation method thereof |
| CN109879267A (en) * | 2019-03-14 | 2019-06-14 | 中山大学 | A kind of preparation method of nanoporous carbon materials |
-
2014
- 2014-12-15 CN CN201410783356.7A patent/CN105887234A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 张国标等: ""纳米纤状聚吡咯导电涂料的制备与性能研究"", 《涂料工业》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108565040A (en) * | 2018-05-04 | 2018-09-21 | 芜湖天科生物科技有限公司 | A kind of whisker type battery conductive material and preparation method thereof |
| CN109879267A (en) * | 2019-03-14 | 2019-06-14 | 中山大学 | A kind of preparation method of nanoporous carbon materials |
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Application publication date: 20160824 |