CN103680996B - A kind of Polypyrrole/graphitetype type carbon nitride nanocomposite and preparation method thereof - Google Patents
A kind of Polypyrrole/graphitetype type carbon nitride nanocomposite and preparation method thereof Download PDFInfo
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- CN103680996B CN103680996B CN201310695379.8A CN201310695379A CN103680996B CN 103680996 B CN103680996 B CN 103680996B CN 201310695379 A CN201310695379 A CN 201310695379A CN 103680996 B CN103680996 B CN 103680996B
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Abstract
The invention discloses a kind of Polypyrrole/graphitetype type carbon nitride nanocomposite and preparation method thereof, belong to composite and preparing technical field.Technical process is as follows：Graphite type carbon nitride is dispersed in water; 0 °C of lower nitrogen protection is stirred 30 minutes; obtain graphite type carbon nitride dispersion liquid; pyrroles is added dropwise in graphite type carbon nitride dispersion liquid, mixed solution is obtained, 0 °C of lower nitrogen protection is stirred 30 minutes; the initiator solution configured is added dropwise in above-mentioned mixed solution again; 0 °C of lower nitrogen protects stirring reaction 10 hours, and products therefrom is washed for several times, and Polypyrrole/graphitetype type carbon nitride nanocomposite is obtained after vacuum drying.With low cost, it is easy to mass produce the advantage of the invention is that preparation technology is simple, nano composite material prepared by the present invention has a good electric conductivity, redox reversible and with higher electric charge carrying capacity.
Description
Technical field
The invention belongs to composite and preparing technical field, it is related to a kind of nano composite material and its preparation side
Method, is a kind of Polypyrrole/graphitetype type carbon nitride nanocomposite and preparation method thereof specifically.
Background technology
Graphite type carbon nitride is the reserves most abundant C on the earth, N element composition, because its structure is similar to graphite, interlayer
With C3N4Or C6N7Ring group is between layers with weak van der Waals interaction, its powerful C-N covalent bond ensures its ring around
Under border have height heat endurance and chemical stability, medium energy gap, special optics, photoelectrochemical property and
With simplification is prepared, current study hotspot is become.At present, both at home and abroad on g-C3N4Research be concentrated mainly on and change
Property photocatalysis performance in terms of, but to g-C3N4Conduction and chemical property in terms of research it is less.Theoretical calculation shows g-C3N4Tool
There is relatively low energy gap.
Polypyrrole has good electric conductivity and environmental stability, and synthesis technique is simple, the advantages of compared with low energy gap width.Mesh
Before, study hotspot is concentrated mainly on an inorganic compound and polypyrrole be combined in terms of preparing advanced composite material (ACM).Such as PPy/
MnO2Composite have higher specific capacitance can as ultracapacitor electrode material（A. Bahloul, B.
Nessark, E. Briot, H. Groult, A. Mauger, C. M.Juilen. Polypyrrole-covered
MnO2 as electrode material for supercapacitor[J]. Power Sources, 2013, 240:
267-272）, PPy/TiO2The amount of composite absorption methylene blue is 5.5 times of 3.6 times and PPy of PPy/P25（J. J.
Li, J. G. Feng, W. Yan. Excellent adsorption and desorption characteristics
of polypyrrole/TiO2 composite for Methylene Blue[J]. Appl. Surf. Sci., 2013,
279: 400-408）.However, on polypyrrole/graphite type carbon nitride（PPy/g-C3N4）The preparation of nano composite material and its lead
The report of electricity/Electrochemical Properties is seldom.
The content of the invention
It is an object of the invention to provide a kind of Polypyrrole/graphitetype type carbon nitride nanocomposite and preparation method thereof,
Make the preparation technology of Polypyrrole/graphitetype type carbon nitride nanocomposite it is simple, with satisfactory electrical conductivity, redox reversible
With electric charge carrying capacity.
In order to solve the above technical problems, the concrete technical scheme that the present invention is used is as follows：
A kind of Polypyrrole/graphitetype type carbon nitride nanocomposite, it is characterised in that：The composite is by graphite mould nitrogen
Change carbon and polypyrrole to be formed after compound；The polypyrrole is a diameter of 200~300nm sub-micron is spherical, and dispersed deposition exists
The surface of graphite type carbon nitride or intercalation are in the layer of graphite type carbon nitride.
According to a kind of preparation method of described Polypyrrole/graphitetype type carbon nitride nanocomposite, it is characterised in that bag
Include following steps：
Step one, the graphite phase carbon nitride of refinement is dispersed in the reactor containing decentralized medium, magnetic agitation 30 minutes,
It is prepared into graphite type carbon nitride dispersion liquid；
Step 2, pyrroles is added dropwise in the graphite type carbon nitride dispersion liquid, and magnetic agitation must mix molten for 30 minutes
Liquid one；
Under the conditions of step 3, nitrogen protection magnetic agitation, the oxidizing agent solution prepared is added dropwise to the mixing
Mixed solution two is obtained in solution one；
Step 4, the mixed solution two sustained response 10 hours, products therefrom under the conditions of nitrogen protection magnetic agitation
Vacuum drying after 6 times is washed with absolute ethyl alcohol and produces target product i.e. Polypyrrole/graphitetype type carbon nitride nanocomposite
Graphite type carbon nitride dispersion liquid is, using water as solvent, graphite type carbon nitride to be dispersed in water in the step one.
The step one to four is reacted under the conditions of 0 °C.
Oxidizing agent solution in the step 3 is persulfate.
The persulfate initiator system of ammonium persulfate.
The present invention has beneficial effect.Graphite type carbon nitride and polypyrrole are subjected to compound preparation first a kind of nano combined
Material, with good electric conductivity, redox reversible and with higher electric charge carrying capacity, described is nano combined
Material electric conductivity is 1.3 times of pure PPy；Oxidation wave of the nano composite material on cyclic voltammetry curve and reduction crest height of wave
Approximately equal, symmetry is good, and display redox reversible is good；The specific capacitance of the nano composite material is pure PPy
(5.86 Fg-1) 2.6 times.The graphite type carbon nitride of the present invention is because with good heat endurance, chemical stability, oxidation is gone back
Former invertibity, the advantages of preparing simplification, low raw-material cost, and with potential application value.Polypyrrole has excellent
Electric conductivity and mouldability, are a small number of conducting polymers that can polymerize in water again.The two is combined by the present invention, can not only carry
The electric conductivity of high polypyrrole, redox reversible, electric charge carrying capacity, are also effectively improved graphite type carbon nitride in organic substrate
On dispersiveness and mouldability.
Brief description of the drawings
Fig. 1 is scanning electron microscope diagram of the invention.
Fig. 2 is cyclic voltammetry curve figure of the invention.
Fig. 3 is X-ray diffractogram of the invention.
The infrared spectrum collection of illustrative plates of Fig. 4 present invention.
Embodiment
Below in conjunction with instantiation the present invention is furture elucidated content, but these embodiments are not intended to limit the guarantor of the present invention
Protect scope.
Embodiment 1
1g graphite type carbon nitrides are added in the three neck round bottom flask equipped with 25ml deionized waters, nitrogen protection magnetic agitation
30min, is disperseed, and the backward dispersion liquid adds 1g pyrrolo-es and stirs 30min at 0 °C, then by oxidant 10mlAPS solution
（Containing APS3.4g）Above-mentioned mixed liquor is added dropwise, in reacting 10h under 0 °C.Products therefrom is cleaned repeatedly with deionized water, 60 °C
Lower vacuum drying 24h can obtain Polypyrrole/graphitetype type carbon nitride nanocomposite.
Fig. 1 is the SEM of the Polypyrrole/graphitetype type carbon nitride nanocomposite prepared by embodiment 1
Figure, polypyrrole particle is deposited on graphite type carbon nitride surface as can be seen from Figure or intercalation is in g-C3N4Piece interlayer；Institute
The cyclic voltammetry curve figure for the Polypyrrole/graphitetype type carbon nitride nanocomposite prepared is as shown in Fig. 2 as can be seen from Figure
There are a pair of redox peaks in curve, and the peak height approximately equal of oxidation wave reduction wave, symmetry is good, illustrates the composite oxygen
Change reduction invertibity preferably, the material electric conductivity is that pure PPy 1.3 times of specific capacitances are pure PPy (5.86 Fg-1) 2.6 times.
Embodiment 2
0.2539g graphite type carbon nitrides are added in the three neck round bottom flask equipped with 25ml deionized waters, nitrogen protection magnetic
Power stirs 30min, is disperseed, and the backward dispersion liquid adds 1g pyrrolo-es and stirs 30min at 0 °C, then by oxidant
10mlAPS solution（Containing APS3.4g）Above-mentioned mixed liquor is added dropwise, in reacting 10h under 0 °C.Products therefrom is anti-with deionized water
Multiple to clean, vacuum drying 24h can obtain Polypyrrole/graphitetype type carbon nitride nanocomposite under 60 °C.
The X-ray diffractogram of prepared Polypyrrole/graphitetype type carbon nitride nanocomposite is as shown in figure 3, from figure
In can be seen that positioned at the peak of 2 θ=24.2 ° be PPy weaker characteristic diffraction peak, the characteristic diffraction peak positioned at 2 θ=27.4 ° belongs to pure
Graphite type carbon nitride characteristic diffraction peak, may be stacked by conjugated double bond and caused.And the characteristic peak positioned at 2 θ=13.0 ° is not obvious, this
It is probably that the amount of pure graphite type carbon nitride causes very little.
Embodiment 3
0.4287g graphite type carbon nitrides are added in the three neck round bottom flask equipped with 25ml deionized waters, nitrogen protection magnetic
Power stirs 30min, is disperseed, and the backward dispersion liquid adds 1g pyrrolo-es and stirs 30min at 0 °C, then by oxidant
10mlAPS solution（Containing APS3.4g）Above-mentioned mixed liquor is added dropwise, in reacting 10h under 0 °C.Products therefrom is anti-with deionized water
Multiple to clean, vacuum drying 24h can obtain Polypyrrole/graphitetype type carbon nitride nanocomposite under 60 °C.
The infrared spectrum collection of illustrative plates of gained Polypyrrole/graphitetype type carbon nitride nanocomposite is as shown in figure 4, polypyrrole/stone
The characteristic absorption peak of black type azotized carbon nano composite is similar to pure PPy, and the addition of graphite type carbon nitride makes to come from PPy
The cm of characteristic absorption peak 1549-1,1457 cm-1, 1045 cm-1Generation blue shift.
Claims (5)
1. a kind of preparation method of Polypyrrole/graphitetype type carbon nitride nanocomposite, it is characterised in that comprise the following steps：
Step one, the graphite type carbon nitride of refinement is dispersed in the reactor containing decentralized medium, magnetic agitation 30 minutes, prepared
Obtain graphite type carbon nitride dispersion liquid；
Step 2, pyrroles is added dropwise in the graphite type carbon nitride dispersion liquid, and magnetic agitation obtains mixed solution one in 30 minutes；
Under the conditions of step 3, nitrogen protection magnetic agitation, the oxidizing agent solution prepared is added dropwise to the mixed solution
Mixed solution two is obtained in one；
Step 4, the mixed solution two sustained response 10 hours, products therefrom nothing under the conditions of nitrogen protection magnetic agitation
Vacuum drying produces target product i.e. Polypyrrole/graphitetype type carbon nitride nanocomposite after water-ethanol is washed 6 times.
2. a kind of preparation method of Polypyrrole/graphitetype type carbon nitride nanocomposite according to claim 1, its feature exists
In：Graphite type carbon nitride dispersion liquid is, using water as solvent, graphite type carbon nitride to be dispersed in water in the step one.
3. a kind of preparation method of Polypyrrole/graphitetype type carbon nitride nanocomposite according to claim 1, its feature exists
In：The step one to four is reacted under the conditions of 0 °C.
4. a kind of preparation method of Polypyrrole/graphitetype type carbon nitride nanocomposite according to claim 1, its feature exists
In：Oxidizing agent solution in the step 3 is persulfate.
5. a kind of preparation method of Polypyrrole/graphitetype type carbon nitride nanocomposite according to claim 4, its feature
It is：The persulfate is ammonium persulfate.
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| CN104261383B (en) * | 2014-09-04 | 2016-08-17 | 北京宝霖华科技发展有限公司 | Quantum carbon element and preparation method thereof and facilities and equipments |
| CN106124585B (en) * | 2016-06-20 | 2018-01-16 | 济南大学 | A kind of preparation method and application based on PPy/CdS/g C3N4 photoelectricity aptamer sensors |
| CN106206070A (en) * | 2016-06-24 | 2016-12-07 | 安徽江威精密制造有限公司 | A kind of electrode material adding polypyrrole/graphite phase carbon nitride composite and preparation method thereof |
| CN106252096B (en) * | 2016-08-29 | 2018-01-23 | 东莞市共和电子有限公司 | A kind of ultracapacitor |
| CN106978595B (en) * | 2017-04-06 | 2019-05-17 | 国家纳米科学中心 | A kind of graphite type carbon nitride nanotube array photoelectrode, preparation method and the usage |
| CN108470647B (en) * | 2018-05-08 | 2019-07-23 | 上海应用技术大学 | A kind of supercapacitor combination electrode material and preparation method thereof |
| CN109585178A (en) * | 2018-12-06 | 2019-04-05 | 中国矿业大学 | The polypyrrole of supercapacitor/graphite type carbon nitride electrode material and preparation method |
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| CN102974283A (en) * | 2012-12-07 | 2013-03-20 | 同济大学 | Mesoporous graphite type carbon nitride/nitrogen doped graphene sol nanocomposite and method for preparing same |
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Non-Patent Citations (2)
| Title |
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| "Dispersed conductive polymer nanoparticles on graphitic carbon nitride for enhanced solar-driven hydrogen evolution from pure water";Yi Sui, et al.;《Nanoscale》;20130710;第5卷;9150-9155 * |
| "Tubular graphitic-C3N4: a prospective material for energy storage and green photocatalysis";Muhammad Tahir, et al.;《Journal of Materials Chemistry A》;20130912;第1卷;13949-13955 * |
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