CN106783197A - Pyrolysis porous carbon graphene composite materials of a kind of ZIF 8 and its preparation method and application - Google Patents
Pyrolysis porous carbon graphene composite materials of a kind of ZIF 8 and its preparation method and application Download PDFInfo
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- 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
- H01G11/22—Electrodes
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- 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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Abstract
The present invention relates to pyrolysis porous carbon graphene composite materials of a kind of ZIF 8 and its preparation method and application, the structure of the composite is：Graphene is wrapped in ZIF 8 and is pyrolyzed porous carbon surface.Preparation method includes：Zinc nitrate hexahydrate and 2 methylimidazoles are mixed, is dissolved in solvent, stand 1~2h, obtain milk shape solution, be centrifuged, washing, vacuum drying obtains the crystal of ZIF 8；The crystal of ZIF 8 is mixed with potassium citrate, is ground, high temperature cabonization, pickling, dried, obtained final product.Preparation method of the invention is simple, low cost, the pyrolysis porous carbon graphene composite materials of ZIF 8 for obtaining have the advantages that stable chemical nature, capacitive character be good, specific surface area is high, take full advantage of multi-stage porous and three-dimensional conductive framework improves chemical property, its specific capacitance has reached 300F/g under the current density of 1A/g, is a kind of high performance electrode material of preferable ultracapacitor.
Description
Technical field
The invention belongs to technical field of nano material, more particularly to a kind of ZIF-8 pyrolysis porous carbon-graphene composite material
And its preparation method and application.
Background technology
Zeolite imidazole ester skeleton structure has excellent physical and chemical performance, such as porosity and specific surface area higher, good
Good chemical stability etc..These special natures make it be widely used in electrochemical field.
In the prior art, pure ZIF-8 pyrolysis porous carbon is obtained by after ZIF-8 crystal direct carbonizations；But, pure ZIF-8
Pyrolysis porous carbon relative distribution, the electrode material specific capacity for being used as ultracapacitor is low, again forthright difference.
Graphene is a kind of two dimensional crystal being made up of carbon atom.Pure grapheme material is two-dimentional large pore material.Make at present
The method of standby Graphene is for directly by the method such as organic carbon and graphene oxide reduction, Graphene is large pore material, easy shape
Reticulate structure；But, often specific capacity is relatively low as electrode material for pure Graphene, again forthright difference, and energy density is low.
The content of the invention
The technical problems to be solved by the invention be to provide a kind of ZIF-8 pyrolysis porous carbon-graphene composite material and its
Preparation method and application, the method prepares ZIF-8 crystal by chemical synthesis, then by grinding ZIF-8 crystal and citric acid
Potassium is well mixed, and Graphene is wrapped in ZIF-8 and is pyrolyzed porous carbon surface by high temperature cabonization, obtains the ZIF- of electrochemical performance
8 pyrolysis porous carbon-graphene composite materials, preparation process environmental protection, process is simple, preparation cost are cheap.
ZIF-8 pyrolysis porous carbons prepared by the present invention are obtained by the carbonization of ZIF-8 crystal high-temperatures, and the raw material sources of Graphene are
Potassium citrate.Graphene is pyrolyzed porous carbon phase and is combined by the present invention with ZIF-8, substantially increases the chemical property of material.
A kind of ZIF-8 of the invention is pyrolyzed porous carbon-graphene composite material, and the structure of the composite is：Graphite
Alkene is wrapped in ZIF-8 and is pyrolyzed porous carbon surface.
The preparing raw material of the composite includes：Zinc nitrate hexahydrate, 2-methylimidazole, methyl alcohol, potassium citrate etc..
A kind of ZIF-8 of the invention is pyrolyzed the preparation method of porous carbon-graphene composite material, including：
(1) zinc nitrate hexahydrate and 2-methylimidazole are mixed, is dissolved in solvent, stand 1~2h, obtain milk shape molten
Liquid, centrifugation, washing, vacuum drying obtains ZIF-8 crystal；
(2) in mass ratio it is 1 by the ZIF-8 crystal in step (1) and potassium citrate：5~1：40 mixing, grinding is obtained
Homogeneous white powder, high temperature cabonization, pickling is dried, and obtains ZIF-8 pyrolysis porous carbon-graphene composite materials；Wherein, it is high
Temperature carbonization condition be：800 DEG C of insulation 2h.
The mass ratio of zinc nitrate hexahydrate, 2-methylimidazole and solvent is 1~5 in the step (1)：8~10：700~
800,
The solvent is methyl alcohol.
The condition of centrifugation is in the step (1)：8000~10000 revs/min, it is centrifuged 5~10 minutes.
Washing is that methyl alcohol or ethanol are washed 2~3 times in the step (1).
Dry temperature is 50~60 DEG C in the step (1), and vacuum is -0.1~-0.08MPa.
ZIF-8 crystal and the mass ratio of potassium citrate are 1 in the step (2)：20.
The atmosphere of step (2) the high temperature carbonisation is nitrogen and argon gas gaseous mixture or argon gas；The speed of intensification is 2
~5 DEG C/min.
The condition of pickling is the 6~8h of hydrochloric acid agitator treating of 0.5~1.0mol/L in the step (2).
The composite is applied to the electrode material field of ultracapacitor.
The present invention prepares new ZIF-8 pyrolysis porous carbon-Graphene composite woods by simple technological design
Material.The composite has following advantage：Graphene is wrapped in ZIF-8 and is pyrolyzed porous carbon surface, forms three-dimensional conductive framework.It is multiple
Condensation material is hierarchical porous structure, improves the overall specific capacity of material and forthright again.Therefore, ZIF-8 is pyrolyzed porous carbon and graphite
Alkene is effectively combined, and can reach good chemiluminescence, to prepare the composite of excellent performance.
Beneficial effect
(1) method of the present invention preparation process is simple and environmentally-friendly, easily operated, is a kind of Green Chemistry preparation method；
(2) experimental design is ingenious in the present invention, by high temperature cabonization technology, is simply and effectively wrapped in graphene sheet layer
ZIF-8 surfaces, prepare ZIF-8 pyrolysis porous carbon-graphene composite materials；
(3) the ZIF-8 pyrolysis porous carbon-graphene composite materials prepared by the present invention have specific capacitance higher, compared with
Good is forthright again, is the ideal electrode material of ultracapacitor；
(4) the ZIF-8 pyrolysis porous carbon-graphene composite materials prepared by the present invention have forthright good again, power density
Height, energy density is big, capacitive character is good, stable chemical nature, specific surface area high the advantages of, take full advantage of multi-stage porous and three-dimensional led
Electric framework improves chemical property, and its specific capacitance has reached 300F/g under the current density of 1A/g.
Brief description of the drawings
Fig. 1 is (A) ZIF-8 pyrolysis porous carbons in embodiment 1, and (B) pure graphene nano lamella, (C) ZIF-8 pyrolysis is porous
The SEM figures of carbon-graphite alkene composite；
Fig. 2 is ZIF-8 pyrolysis porous carbons in embodiment 1, and Graphene, ZIF-8 is pyrolyzed porous carbon-graphene composite material
Multiplying power figure；
Fig. 3 is ZIF-8 pyrolysis porous carbons in embodiment 1, and Graphene, ZIF-8 is pyrolyzed porous carbon-graphene composite material
Power density and energy density profile；
Fig. 4 is the SEM figures of ZIF-8 pyrolysis porous carbon-graphene composite material (ZIF-8-G-1) in embodiment 2.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content for having read instruction of the present invention, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
Embodiment 1
(1) zinc nitrate hexahydrate and 2-methylimidazole are mixed, is dissolved in methyl alcohol, zinc nitrate hexahydrate, 2- methyl miaows
Azoles is 1 with the mass ratio of methyl alcohol：8：700.
(2) by solution left standstill 1h, milk shape solution is obtained.
(3) resulting solution is centrifuged 10min under 10000 revs/min of speed, after washed three times with methyl alcohol, obtain
ZIF-8 crystal.
(4) the ZIF-8 crystal that will be obtained is dried；Wherein, dry temperature is 60 DEG C, and vacuum is -0.1MPa.
(5) the ZIF-8 crystal that will be prepared is 1 with potassium citrate in mass ratio：20 mixing, grinding obtains homogeneous white
Color powder.
(6) under nitrogen atmosphere, 5 DEG C/min is warming up to 800 DEG C to the white powder that will be obtained, and keeps 2h, and carbonization is prepared
ZIF-8 is pyrolyzed porous carbon-graphene composite material.
(7) ZIF-8 that will be prepared is pyrolyzed porous carbon-graphene composite material 0.5mol/L salt pickling 6h, dries, and obtains
ZIF-8 is pyrolyzed porous carbon-graphene composite material.
Preparation-obtained ZIF-8 pyrolysis is characterized using SEM (SEM), electrochemical workstation porous
The pattern and structure of carbon-graphite alkene composite and the chemical property as electrode material for super capacitor.
SEM test results show：ZIF-8 pyrolysis porous carbon-graphene composite materials prepared in the present embodiment have
Three-dimensional structure, graphene nanometer sheet is wrapped in ZIF-8 and is pyrolyzed porous carbon surface.Referring to Fig. 1.Electrochemical results show：
ZIF-8 pyrolysis porous carbon-graphene composite materials have specific capacitance higher forthright again with preferable, and its quality specific capacitance reaches
300F/g, referring to Fig. 2；Power density higher, has reached 10000W/kg, energy density higher, 40Wh/kg, referring to figure
3.Wherein, the preparation method of ZIF-8 pyrolysis porous carbon is shown in comparative example 1.The preparation method of Graphene is shown in comparative example 2.
Embodiment 2
(1) zinc nitrate hexahydrate and 2-methylimidazole are mixed, is dissolved in methyl alcohol, zinc nitrate hexahydrate, 2- methyl miaows
Azoles is 1 with the mass ratio of methyl alcohol：8：700.
(2) by solution left standstill 1h, milk shape solution is obtained.
(3) resulting solution is centrifuged 10min under 10000 revs/min of speed, after washed three times with methyl alcohol, obtain
ZIF-8 crystal.
(4) the ZIF-8 crystal that will be obtained is dried；Wherein, dry temperature is 60 DEG C, and vacuum is -0.1MPa.
(5) the ZIF-8 crystal that will be prepared is 1 with potassium citrate in mass ratio：5 mixing, grinding obtains homogeneous white
Powder.
(6) under nitrogen atmosphere, 5 DEG C/min is warming up to 800 DEG C to the white powder that will be obtained, and keeps 2h, and carbonization is prepared
ZIF-8 is pyrolyzed porous carbon-graphene composite material.
(7) ZIF-8 that will be prepared is pyrolyzed porous carbon-graphene composite material 0.5mol/L salt pickling 6h, dries, acquisition
Composite is designated as ZIF-8-G-1.Its SEM figures are as shown in Figure 4.
Embodiment 3
(1) zinc nitrate hexahydrate and 2-methylimidazole are mixed, is dissolved in methyl alcohol, zinc nitrate hexahydrate, 2- methyl miaows
Azoles is 1 with the mass ratio of methyl alcohol：8：700.
(2) by solution left standstill 1h, milk shape solution is obtained.
(3) resulting solution is centrifuged 10min under 10000 revs/min of speed, after washed three times with methyl alcohol, obtain
ZIF-8 crystal.
(4) the ZIF-8 crystal that will be obtained is dried；Wherein, dry temperature is 60 DEG C, and vacuum is -0.1MPa.
(5) the ZIF-8 crystal that will be prepared is 1 with potassium citrate in mass ratio：40 mixing, grinding obtains homogeneous white
Color powder.
(6) under nitrogen atmosphere, 5 DEG C/min is warming up to 800 DEG C to the white powder that will be obtained, and keeps 2h, and carbonization is prepared
ZIF-8 is pyrolyzed porous carbon-graphene composite material.
(7) ZIF-8 that will be prepared is pyrolyzed porous carbon-graphene composite material 0.5mol/L salt pickling 6h, dries, acquisition
Composite is designated as ZIF-8-G-2.
Comparative example 1
(1) zinc nitrate hexahydrate and 2-methylimidazole are mixed, is dissolved in methyl alcohol, zinc nitrate hexahydrate, 2- methyl miaows
Azoles is 1 with the mass ratio of methyl alcohol：8：700.
(2) by solution left standstill 1h, milk shape solution is obtained.
(3) resulting solution is centrifuged 10min under 10000 revs/min of speed, after washed three times with methyl alcohol, obtain
ZIF-8 crystal.
(4) the ZIF-8 crystal that will be obtained is dried；Wherein, dry temperature is 60 DEG C, and vacuum is -0.1MPa.
(5) the ZIF-8 crystal grinding that will be prepared, obtains homogeneous white powder.
(6) under nitrogen atmosphere, 5 DEG C/min is warming up to 800 DEG C to the white powder that will be obtained, and keeps 2h, and carbonization is prepared
ZIF-8 is pyrolyzed porous carbon.
(7) ZIF-8 that will be prepared is pyrolyzed porous carbon 0.5mol/L salt pickling 6h, dries, and obtains final product.
Comparative example 2
(1) by potassium citrate under nitrogen atmosphere, 5 DEG C/min is warming up to 800 DEG C, keeps 2h, and graphite is prepared in carbonization
Alkene.
(2) the Graphene 0.5mol/L salt pickling 6h that will be prepared, dry, and obtain final product.
Claims (10)
1. a kind of ZIF-8 pyrolysis porous carbon-graphene composite material, it is characterised in that the structure of the composite is：Graphite
Alkene is wrapped in ZIF-8 and is pyrolyzed porous carbon surface.
2. a kind of ZIF-8 is pyrolyzed the preparation method of porous carbon-graphene composite material, including：
(1) zinc nitrate hexahydrate and 2-methylimidazole are mixed, are dissolved in solvent, stand 1~2h, obtain milk shape solution,
Centrifugation, washing, vacuum drying obtains ZIF-8 crystal；
(2) in mass ratio it is 1 by the ZIF-8 crystal in step (1) and potassium citrate：5~1：40 mixing, grinding, high temperature cabonization,
Pickling, dries, and obtains ZIF-8 pyrolysis porous carbon-graphene composite materials；Wherein, the condition of high temperature cabonization is：800 DEG C of insulations
2h。
3. a kind of ZIF-8 according to claim 2 is pyrolyzed the preparation method of porous carbon-graphene composite material, its feature
It is that the mass ratio of zinc nitrate hexahydrate, 2-methylimidazole and solvent is 1~5 in the step (1)：8~10：700~800.
4. a kind of ZIF-8 according to claim 3 is pyrolyzed the preparation method of porous carbon-graphene composite material, its feature
It is that the solvent is methyl alcohol.
5. a kind of ZIF-8 according to claim 2 is pyrolyzed the preparation method of porous carbon-graphene composite material, its feature
It is that the condition of centrifugation is in the step (1)：8000~10000 revs/min, it is centrifuged 5~10 minutes.
6. a kind of ZIF-8 according to claim 2 is pyrolyzed the preparation method of porous carbon-graphene composite material, its feature
It is that washing is methyl alcohol or ethanol in the step (1), is washed 2~3 times.
7. a kind of ZIF-8 according to claim 2 is pyrolyzed the preparation method of porous carbon-graphene composite material, its feature
It is that vacuum drying temperature is 50~60 DEG C in the step (1), vacuum is -0.1~-0.08MPa.
8. a kind of ZIF-8 according to claim 2 is pyrolyzed the preparation method of porous carbon-graphene composite material, its feature
It is that the atmosphere of step (2) the high temperature carbonisation is nitrogen and argon gas gaseous mixture or argon gas；The speed of intensification is 2~5
℃/min。
9. a kind of ZIF-8 according to claim 2 is pyrolyzed the preparation method of porous carbon-graphene composite material, its feature
It is that the condition of pickling is the 6~8h of hydrochloric acid agitator treating of 0.5~1.0mol/L in the step (2).
10. a kind of ZIF-8 as claimed in claim 1 is pyrolyzed the application of porous carbon-graphene composite material, it is characterised in that
The composite is applied to the electrode material field of ultracapacitor.
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| CN108054020A (en) * | 2017-11-22 | 2018-05-18 | 江苏大学 | A kind of preparation method and application of nitrogen-doped carbon particle/graphitized carbon nitrogen composite material |
| CN108190856A (en) * | 2018-01-25 | 2018-06-22 | 南京航空航天大学 | A kind of preparation method of Ce-N codopes two dimension porous carbon materials |
| CN108545712A (en) * | 2018-04-17 | 2018-09-18 | 东华大学 | A method of synthesizing multi-stage porous carbon material with salt template carbonization ZIF-8 |
| CN108648925A (en) * | 2018-04-17 | 2018-10-12 | 东华大学 | A kind of carbon nanotube-carbon nanosheet nano-hybrid material and its preparation and application |
| CN108806998A (en) * | 2018-07-18 | 2018-11-13 | 江苏大学 | Tri compound ZnO/ZnCo of the solvent structure based on ZIF-82O4The method and its application of/NiO |
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| CN108190856A (en) * | 2018-01-25 | 2018-06-22 | 南京航空航天大学 | A kind of preparation method of Ce-N codopes two dimension porous carbon materials |
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