CN103680996A - Polypyrrole/graphite type carbon nitride nanocomposite and preparation method thereof - Google Patents
Polypyrrole/graphite type carbon nitride nanocomposite and preparation method thereof Download PDFInfo
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- CN103680996A CN103680996A CN201310695379.8A CN201310695379A CN103680996A CN 103680996 A CN103680996 A CN 103680996A CN 201310695379 A CN201310695379 A CN 201310695379A CN 103680996 A CN103680996 A CN 103680996A
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- polypyrrole
- graphite mould
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Abstract
The invention discloses a polypyrrole/graphite type carbon nitride nanocomposite and a preparation method of the polypyrrole/graphite type carbon nitride nanocomposite, and belongs to the technical fields of composite materials and preparation. The preparation method of the polypyrrole/graphite type carbon nitride nanocomposite comprises the following steps of dispersing graphite type carbon nitride in water, stirring the mixture for 30 minutes under nitrogen protection at the temperature of 0DEG C to obtain graphite type carbon nitride dispersion, dropwise adding pyrrole into the graphite type carbon nitride dispersion to obtain a mixed solution, stirring the mixed solution for 30 minutes under nitrogen protection at the temperature of 0DEG C, dropwise adding a prepared initiator solution into the mixed solution, carrying out stir and reaction for 10 hours under nitrogen protection at the temperature of 0DEG C to obtain a product, washing the product several times, and carrying out vacuum drying on the product to obtain the polypyrrole/graphite type carbon nitride nanocomposite. The polypyrrole/graphite type carbon nitride nanocomposite and the preparation method of the polypyrrole/graphite type carbon nitride nanocomposite have the advantages that the preparation technology is simple, the cost is low, large-scale production can be easily conducted, and the prepared polypyrrole/graphite type carbon nitride nanocomposite has good conductivity, good oxidoreduction reversibility and high electric charge containing capacity.
Description
Technical field
The invention belongs to and belong to composite material and preparing technical field, relate to a kind of nano composite material and preparation method thereof, specifically, is a kind of polypyrrole
/graphite mould azotized carbon nano composite material and preparation method thereof.
Background technology
Graphite mould carbonitride is by the abundantest C of reserves on the earth, and N element forms, because of its structure and graphite-phase seemingly, interlayer is with C
3n
4or C
6n
7ring forms, between layers with weak van der Waals interaction, its powerful C-N covalent bond guarantees that it has thermal stability and chemical stability highly under environment around, medium energy gap, special optics, photoelectrochemical property and have preparation simplification, becomes current study hotspot.At present, both at home and abroad about g-C
3n
4research mainly concentrate on modified photocatalytic aspect of performance, but to g-C
3n
4conduction and the research of chemical property aspect less.Theoretical calculating shows g-C
3n
4there is lower energy gap.
Polypyrrole has good conductivity and environmental stability, and synthesis technique is simple, compared with advantages such as low energy gap width.At present, study hotspot mainly concentrates on an inorganic compound and polypyrrole carries out the compound advanced composite material (ACM) aspect of preparing.As PPy/MnO
2composite material has electrode material (A. Bahloul, B. Nessark, E. Briot, H. Groult, A. Mauger, the C. M.Juilen. Polypyrrole-covered MnO that higher ratio electric capacity can be used as ultracapacitor
2as electrode material for supercapacitor[J]. Power Sources, 2013,240:267-272), PPy/TiO
2the amount of composite material absorption methylene blue is 3.6 times and 5.5 times of (J. J. Li, J. G. Feng, the W. Yan. Excellent adsorption and desorption characteristics of polypyrrole/TiO of PPy of PPy/P25
2composite for Methylene Blue[J]. Appl. Surf. Sci., 2013,279:400-408).Yet, about polypyrrole/graphite mould carbonitride (PPy/g-C
3n
4) preparation of nano composite material and the report of conduction/Electrochemical Properties thereof are seldom.
Summary of the invention
The object of the present invention is to provide a kind of polypyrrole
/graphite mould azotized carbon nano composite material and preparation method thereof, makes polypyrrole
/the preparation technology of graphite mould azotized carbon nano composite material is simple, have satisfactory electrical conductivity, redox reversible and electric charge carrying capacity.
In order to solve above technical problem, the concrete technical scheme that the present invention adopts is as follows:
A kind of polypyrrole
/graphite mould azotized carbon nano composite material, is characterized in that: described composite material is formed after compound by graphite mould carbonitride and polypyrrole; Described polypyrrole is that diameter is 200
~the sub-micron of 300nm is spherical, and dispersed deposition on the surface of graphite mould carbonitride or intercalation in the layer of graphite mould carbonitride.
According to described a kind of polypyrrole
/the preparation method of graphite mould azotized carbon nano composite material, is characterized in that comprising the following steps:
Step 1, is dispersed in the graphite-phase carbonitride of refinement in the reactor containing decentralized medium, and magnetic agitation 30 minutes is prepared into graphite mould carbonitride dispersion liquid;
Step 2, dropwise adds pyrroles in described graphite mould carbonitride dispersion liquid, and magnetic agitation obtains mixed solution one for 30 minutes;
Step 3, under nitrogen protection magnetic agitation condition, is dropwise added in described mixed solution one to obtain mixed solution two by the oxidizing agent solution preparing;
Step 4, described mixed solution two sustained response 10 hours under nitrogen protection magnetic agitation condition, it is polypyrrole that products therefrom is drying to obtain target product with 6 final vacuums of absolute ethanol washing
/graphite mould azotized carbon nano composite material
In described step 1, graphite mould carbonitride dispersion liquid is to take water as solvent, and graphite mould carbonitride is dispersed in water.
Described step 1 to four is all to react under 0 ° of C condition.
Oxidizing agent solution in described step 3 is persulfate.
Described persulfate initiator system of ammonium persulfate.
the present invention has beneficial effect.First graphite mould carbonitride and polypyrrole are carried out to a kind of nano composite material of compound preparation, have good conductivity, redox reversible and have higher electric charge carrying capacity, described nano composite material conductivity is 1.3 times of pure PPy; Oxidation wave and the reduction wave peak height approximately equal of described nano composite material on cyclic voltammetry curve, symmetry is good, shows that redox reversible is good; The ratio electric capacity of this nano composite material is pure PPy (5.86 Fg
-1) 2.6 times.Graphite mould carbonitride of the present invention is because having good thermal stability, chemical stability, and redox reversible, preparation simplification, the advantage such as cost of material is cheap, and there is potential using value.Polypyrrole has good electric conductivity and mouldability, is again the conducting polymer that minority can polymerization in water.The present invention is compound by the two, not only can improve conductivity, redox reversible, the electric charge carrying capacity of polypyrrole, also effectively improves dispersiveness and the mouldability of graphite mould carbonitride on organic substrate.
Accompanying drawing explanation
Fig. 1 is scanning electron microscope diagram of the present invention.
Fig. 2 is cyclic voltammetry curve figure of the present invention.
Fig. 3 is X-ray diffractogram of the present invention.
Fig. 4 infrared spectrum collection of illustrative plates of the present invention.
Embodiment
Below in conjunction with instantiation, further illustrate content of the present invention, but these embodiment do not limit the scope of the invention.
embodiment 1
1g graphite mould carbonitride is added in three mouthfuls of round-bottomed flasks that 25ml deionized water is housed; nitrogen protection magnetic agitation 30min; disperse; backward this dispersion liquid adds 1g pyrrolo-to stir 30min at 0 ° of C; subsequently oxidant 10mlAPS solution (containing APS3.4g) is dropwise added to above-mentioned mixed liquor, under 0 ° of C, react 10h.Products therefrom cleans repeatedly with deionized water, and under 60 ° of C, vacuumize 24h can obtain polypyrrole
/graphite mould azotized carbon nano composite material.
Fig. 1 is the prepared polypyrrole of embodiment 1
/the scanning electron microscope diagram of graphite mould azotized carbon nano composite material, as can be seen from Figure polypyrrole particle be deposited on graphite mould carbonitride surface or intercalation in g-C
3n
4sheet interlayer; Prepared polypyrrole
/the cyclic voltammetry curve figure of graphite mould azotized carbon nano composite material as shown in Figure 2, there is a pair of redox peak in curve as can be seen from Figure, the peak height approximately equal of oxidation wave reduction wave, symmetry is good, illustrate that this composite material redox reversible is better, this material electric conductivity is that the 1.3 multiple proportions electric capacity of pure PPy are pure PPy (5.86 Fg
-1) 2.6 times.
embodiment 2
0.2539g graphite mould carbonitride is added in three mouthfuls of round-bottomed flasks that 25ml deionized water is housed; nitrogen protection magnetic agitation 30min; disperse; backward this dispersion liquid adds 1g pyrrolo-to stir 30min at 0 ° of C; subsequently oxidant 10mlAPS solution (containing APS3.4g) is dropwise added to above-mentioned mixed liquor, under 0 ° of C, react 10h.Products therefrom cleans repeatedly with deionized water, and under 60 ° of C, vacuumize 24h can obtain polypyrrole
/graphite mould azotized carbon nano composite material.
Prepared polypyrrole
/the X-ray diffractogram of graphite mould azotized carbon nano composite material as shown in Figure 3, the peak that is positioned at as can be seen from Figure 2 θ=24.2 ° is the weak characteristic diffraction peak of PPy, the characteristic diffraction peak that is positioned at 2 θ=27.4 °, belongs to pure graphite mould carbonitride characteristic diffraction peak, may cause by conjugated double bond is stacking.And the characteristic peak that is positioned at 2 θ=13.0 ° is not obvious, this may be that the amount of pure graphite mould carbonitride causes very little.
embodiment 3
0.4287g graphite mould carbonitride is added in three mouthfuls of round-bottomed flasks that 25ml deionized water is housed; nitrogen protection magnetic agitation 30min; disperse; backward this dispersion liquid adds 1g pyrrolo-to stir 30min at 0 ° of C; subsequently oxidant 10mlAPS solution (containing APS3.4g) is dropwise added to above-mentioned mixed liquor, under 0 ° of C, react 10h.Products therefrom cleans repeatedly with deionized water, and under 60 ° of C, vacuumize 24h can obtain polypyrrole
/graphite mould azotized carbon nano composite material.
Gained polypyrrole
/the infrared spectrum collection of illustrative plates of graphite mould azotized carbon nano composite material as shown in Figure 4, polypyrrole
/the characteristic absorption peak of graphite mould azotized carbon nano composite material is similar to pure PPy, and adding of graphite mould carbonitride, makes to come from characteristic absorption peak 1549 cm of PPy
-1, 1457 cm
-1, 1045 cm
-1there is blue shift.
Claims (6)
1. a polypyrrole
/graphite mould azotized carbon nano composite material, is characterized in that: described composite material is formed after compound by graphite mould carbonitride and polypyrrole; Described polypyrrole is that diameter is 200
~the sub-micron of 300nm is spherical, and dispersed deposition on the surface of graphite mould carbonitride or intercalation in the layer of graphite mould carbonitride.
2. a kind of polypyrrole according to claim 1
/the preparation method of graphite mould azotized carbon nano composite material, is characterized in that comprising the following steps:
Step 1, is dispersed in the graphite-phase carbonitride of refinement in the reactor containing decentralized medium, and magnetic agitation 30 minutes is prepared into graphite mould carbonitride dispersion liquid;
Step 2, dropwise adds pyrroles in described graphite mould carbonitride dispersion liquid, and magnetic agitation obtains mixed solution one for 30 minutes;
Step 3, under nitrogen protection magnetic agitation condition, is dropwise added in described mixed solution one to obtain mixed solution two by the oxidizing agent solution preparing;
Step 4, described mixed solution two sustained response 10 hours under nitrogen protection magnetic agitation condition, it is polypyrrole that products therefrom is drying to obtain target product with 6 final vacuums of absolute ethanol washing
/graphite mould azotized carbon nano composite material.
3. a kind of polypyrrole as claimed in claim 2
/the preparation method of graphite mould azotized carbon nano composite material, is characterized in that: in described step 1, graphite mould carbonitride dispersion liquid is to take water as solvent, and graphite mould carbonitride is dispersed in water.
4. a kind of polypyrrole as claimed in claim 2
/the preparation method of graphite mould azotized carbon nano composite material, is characterized in that: described step 1 to four is all to react under 0 ° of C condition.
5. a kind of polypyrrole as claimed in claim 2
/the preparation method of graphite mould azotized carbon nano composite material, is characterized in that: the oxidizing agent solution in described step 3 is persulfate.
6. a kind of polypyrrole as claimed in claim 5
/the preparation method of graphite mould azotized carbon nano composite material, is characterized in that: described persulfate initiator system of ammonium persulfate.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104261383A (en) * | 2014-09-04 | 2015-01-07 | 朱光华 | Qunatum carbon, and preparation method and implementation apparatus thereof |
| CN106124585A (en) * | 2016-06-20 | 2016-11-16 | 济南大学 | A kind of preparation method and application based on PPy/CdS/g C3N4 photoelectricity aptamer sensor |
| 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 |
| CN106978595A (en) * | 2017-04-06 | 2017-07-25 | 国家纳米科学中心 | A kind of graphite type carbon nitride nanotube array photoelectrode, preparation method and the usage |
| WO2018041095A1 (en) * | 2016-08-29 | 2018-03-08 | Liu Sizhi | Supercapacitor |
| CN108470647A (en) * | 2018-05-08 | 2018-08-31 | 上海应用技术大学 | A kind of ultracapacitor PEDOT:PSS@g-C3N4Combination 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 |
Citations (1)
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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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Patent Citations (1)
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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 |
Non-Patent Citations (2)
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|---|
| MUHAMMAD TAHIR, ET AL.: ""Tubular graphitic-C3N4: a prospective material for energy storage and green photocatalysis"", 《JOURNAL OF MATERIALS CHEMISTRY A》 * |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104261383A (en) * | 2014-09-04 | 2015-01-07 | 朱光华 | Qunatum carbon, and preparation method and implementation apparatus thereof |
| CN106124585A (en) * | 2016-06-20 | 2016-11-16 | 济南大学 | A kind of preparation method and application based on PPy/CdS/g C3N4 photoelectricity aptamer sensor |
| 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 |
| WO2018041095A1 (en) * | 2016-08-29 | 2018-03-08 | Liu Sizhi | Supercapacitor |
| CN106978595A (en) * | 2017-04-06 | 2017-07-25 | 国家纳米科学中心 | A kind of graphite type carbon nitride nanotube array photoelectrode, preparation method and the usage |
| 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 |
| CN108470647A (en) * | 2018-05-08 | 2018-08-31 | 上海应用技术大学 | A kind of ultracapacitor PEDOT:PSS@g-C3N4Combination electrode material and preparation method thereof |
| 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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