CN107720722A - A kind of nitrogenous multi-stage porous Carbon Materials and its preparation method and application - Google Patents
A kind of nitrogenous multi-stage porous Carbon Materials and its preparation method and application Download PDFInfo
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- CN107720722A CN107720722A CN201711021226.XA CN201711021226A CN107720722A CN 107720722 A CN107720722 A CN 107720722A CN 201711021226 A CN201711021226 A CN 201711021226A CN 107720722 A CN107720722 A CN 107720722A
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- carbon materials
- porous carbon
- stage porous
- cigarette filter
- nitrogenous
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Classifications
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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
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- 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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
-
- 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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
-
- 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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/44—Raw materials therefor, e.g. resins or coal
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a kind of nitrogenous multi-stage porous Carbon Materials, using the cigarette filter of recovery as carbon matrix precursor carbon material, using urea as nitrogen source, pass through the cigarette filter to the recovery containing urea, soak in the alcohol dispersion liquid of graphene oxide, and obtained after charing process.The invention also discloses the preparation method and application of above-mentioned nitrogenous multi-stage porous Carbon Materials.The present invention is used as nitrogen source using urea so that the Carbon Materials obtained after charing process have higher nitrogen content.Because cigarette filter is made up of acetate fiber, the short texture of itself is porous, and loose structure can be obtained after charing.Graphene oxide is reduced to graphene at high temperature, thus can obtain nitrogenous and graphene multilevel hole material.Obtained Carbon Materials have high ratio surface, excellent electric conductivity, and nitrogen doped, can be applied to the electrode material of ultracapacitor.
Description
Technical field
The invention belongs to technical field of composite materials, is related to a kind of nitrogenous multi-stage porous Carbon Materials, the invention further relates to above-mentioned
The preparation method and purposes of the nitrogenous multi-stage porous Carbon Materials in side.
Background technology
At present, porous material has become study hotspot due to having the characteristics that high ratio surface.The system of porous carbon material
Preparation Method mainly includes charring, spark plug, template etc., and it is with a wide range of applications in fields such as absorption, catalysis.One
As porous material can be divided into micropore (diameter is less than 2nm) according to pore size, mesopore (diameter is more than 2nm and is less than 50nm) and
Macropore (diameter is more than 50nm).The elements such as nitrogen, boron, phosphorus are added in Carbon Materials, the chemical property of material can be effectively improved, its
Middle research is most hot be exactly nitrogen doping, the addition of nitrogen-atoms can improve the electric conductivity of Carbon Materials, while improve hole
Structure.The preparation of nitrating porous carbon material is generally divided into two methods.The first is doping nitrogen in situ, be for second by urea,
The nitrogenous material such as ammonia and melamine and Carbon Materials are handled together.The nitrogen content that the latter obtains is relatively low, so in situ
Nitrogen doped most has application prospect.
With the development of society, increasing house refuse is present in our daily life, one of which is exactly useless
Cigarette end.Recycling research at present to the cigarette end that gives up is less, and the main raw material(s) of cigarette filter is acetate fiber, and
It is loose porous, porous carbon materials can be obtained after charing, there is application prospect.
The content of the invention
It is an object of the invention to provide a kind of nitrogenous multi-stage porous Carbon Materials, one is provided for the recycling of cigarette filter
Kind new method.
The second object of the present invention is to provide the preparation method of above-mentioned nitrogenous multi-stage porous Carbon Materials.
The third object of the present invention is to provide the application of above-mentioned nitrogenous multi-stage porous Carbon Materials.
The technical solution adopted in the present invention is a kind of nitrogenous multi-stage porous Carbon Materials, using the cigarette filter of recovery as
Carbon matrix precursor carbon material, using urea as nitrogen source, by the cigarette filter to the recovery containing urea, in the second of graphene oxide
Soak in alcohol dispersion liquid, and obtained after charing process.
The features of the present invention also resides in,
The cigarette filter of recovery containing urea, by the way that the cigarette filter of recovery is urinated in concentration for 0.5~1g/ml
Soaked in the plain aqueous solution, drying obtains.
Single quality increases by 5~20mg after the alcohol dispersion liquid drying of cigarette filter immersion graphene oxide.
Second technical scheme of the present invention is a kind of preparation method of nitrogenous multi-stage porous Carbon Materials, specifically to press
Implement according to following steps：
Step 1, cigarette filter is soaked in aqueous solution of urea, dried, then disperseed in the ethanol of graphene oxide
Soaked several times in liquid；
Step 2, the cigarette filter after step 1 processing carbonize painstakingly, that is, obtain nitrogenous multi-stage porous raw material of wood-charcoal
Material.
The features of the present invention also resides in,
The mass volume ratio of cigarette filter and aqueous solution of urea is 0.01~0.05g/ml in step 1.
Drying temperature is 70~100 DEG C in step 1, and the time is 20~30min.
The alcohol dispersion liquid concentration of graphene oxide is 0.5~1g/L in step 1.
Cigarette filter soaks 20~30 times in the alcohol dispersion liquid of graphene oxide, shelve 2 after immersion every time~
6min, then soaked next time, it is desirable to single quality increases by 5~20mg after the cigarette filter drying after step 1 processing.
Charing process temperature is 600~900 DEG C, and soaking time is 2~3h.
3rd technical scheme of the present invention is a kind of purposes of nitrogenous multi-stage porous Carbon Materials, as super electricity
The electrode material of container.
The invention has the advantages that the present invention is used as nitrogen source using urea so that the Carbon Materials tool obtained after charing process
There is higher nitrogen content.Because cigarette filter is made up of acetate fiber, the short texture of itself is porous, can be obtained after charing
To loose structure.Graphene oxide is reduced to graphene at high temperature, thus can obtain nitrogenous and graphene multi-stage porous
Material.Obtained Carbon Materials have high ratio surface, excellent electric conductivity, and nitrogen doped, can be applied to super capacitor
The electrode material of device.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of nitrogenous multi-stage porous Carbon Materials prepared by embodiment 1；
Fig. 2 is the scanning electron microscope (SEM) photograph of nitrogenous multi-stage porous Carbon Materials prepared by embodiment 2；
Fig. 3 is the scanning electron microscope (SEM) photograph of nitrogenous multi-stage porous Carbon Materials prepared by embodiment 3.
Embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
A kind of nitrogenous multi-stage porous Carbon Materials of the present invention, using the cigarette filter of recovery as carbon matrix precursor carbon material, with urine
Element is nitrogen source, by being dried after the cigarette filter of recovery is soaked in urea liquid, then in the ethanol of graphene oxide
Soaked repeatedly in dispersion liquid, finally put it into tube furnace and carbonized to obtain.
A kind of preparation method of nitrogenous multi-stage porous Carbon Materials of the present invention, specifically implements according to following steps：
Step 1, the aqueous solution that concentration is 0.5~1g/ml urea is prepared；
Step 2, it is 0.01~0.05g/ml according to the mass volume ratio of cigarette filter and urea liquid, by the perfume (or spice) of recovery
In urea liquid prepared by tobacco filters soaking step 1, soak time is 10~20min.Then it is placed 20 in an oven
~30min, temperature setting are 70~100 DEG C, then soak 30~60s, oxidation in the alcohol dispersion liquid of graphene oxide again
The alcohol dispersion liquid concentration of graphene is 0.5~1g/L.In order to which more graphene oxides can be allowed to enter in cigarette filter,
This process repeats 20~30 times, shelves 2~6min every time.After drying, the quality of single cigarette filter increases by 5~20mg.
Step 3, cigarette filter is put into tube furnace after being handled in step 2, carries out charing process, and charing process temperature is
600~900 DEG C, programming rate is that 5~10 DEG C/min soaking times are 2~3h, and nitrogenous multi-stage porous Carbon Materials are obtained after charing.
The present invention chooses urea as nitrogen source, because the Nitrogen content of urea is high, solubility is high so that obtained after charing process
Carbon Materials there is higher nitrogen content.Because cigarette filter is made up of acetate fiber, the short texture of itself is porous, charcoal
Loose structure can be obtained after change.Graphene oxide is reduced to graphene at high temperature, thus can obtain nitrogenous and graphite
The multilevel hole material of alkene.Obtained Carbon Materials have high ratio surface, excellent electric conductivity, and nitrogen doped, can apply
In the electrode material of ultracapacitor.
The present invention directly can recycle cigarette filter, and the recycling for the cigarette end that gives up is significant,
Nitrogen content is higher after directly being soaked with urea liquid.
Embodiment 1
10g urea is dissolved in 20ml deionized waters, cigarette filter is then soaked into 20min in urea liquid, is soaked
30min is placed after bubble in an oven, temperature setting is 70 DEG C.By 1mg graphene oxides in 2ml ethanol ultrasonic disperse.Then
Will in urea liquid soak after and dry cigarette filter soak 30s in the alcohol dispersion liquid of graphene oxide after take
Go out, 2min is shelved on culture dish, is then soaked again.This process is repeated 20 times.Finally place it in and charcoal is carried out in tube furnace
Change, carbonization temperature is 600 DEG C, is incubated 2h, programming rate is 5~10 DEG C/min.Nitrogenous multi-stage porous Carbon Materials are obtained after charing.
Its scanning electron microscope (SEM) photograph is as shown in figure 1, it can clearly be seen that the hole of its surface distributed, and nitrogen content highest.
Embodiment 2
15g urea is dissolved in 20ml deionized waters, cigarette filter is then soaked into 15min in urea liquid, is soaked
27min is placed after bubble in an oven, temperature setting is 80 DEG C.By 2mg graphene oxides in 2ml ethanol ultrasonic disperse.Then
Will in urea liquid soak after and dry cigarette filter soak 40s in the alcohol dispersion liquid of graphene oxide after take
Go out, 3min is shelved on culture dish, is then soaked again.This process repeats 22 times.Finally place it in and charcoal is carried out in tube furnace
Change, carbonization temperature is 900 DEG C, is incubated 3h, programming rate is 5~10 DEG C/min.Nitrogenous multi-stage porous Carbon Materials are obtained after charing.
Its scanning electron microscope (SEM) photograph is as shown in Fig. 2 it can clearly be seen that the hole of its surface distributed, and nitrogen content highest.
Embodiment 3
20g urea is dissolved in 20ml deionized waters, cigarette filter is then soaked into 10min in urea liquid, is soaked
20min is placed after bubble in an oven, temperature setting is 100 DEG C.By 1.2mg graphene oxides in 2ml ethanol ultrasonic disperse.So
Afterwards will in urea liquid soak after and dry cigarette filter soak 45s in the alcohol dispersion liquid of graphene oxide after take
Go out, 4min is shelved on culture dish, is then soaked again.This process repeats 24 times.Finally place it in and charcoal is carried out in tube furnace
Change, carbonization temperature is 700 DEG C, is incubated 2.5h, programming rate is 5~10 DEG C/min.Nitrogenous multi-stage porous raw material of wood-charcoal is obtained after charing
Material.Its scanning electron microscope (SEM) photograph is as shown in figure 3, it can clearly be seen that the hole of its surface distributed, and nitrogen content highest.
Embodiment 4
12g urea is dissolved in 20ml deionized waters, cigarette filter is then soaked into 12min in urea liquid, is soaked
22min is placed after bubble in an oven, temperature setting is 95 DEG C.By 1.4mg graphene oxides in 2ml ethanol ultrasonic disperse.So
Afterwards will in urea liquid soak after and dry cigarette filter soak 50s in the alcohol dispersion liquid of graphene oxide after take
Go out, 5min is shelved on culture dish, is then soaked again.This process repeats 26 times.Finally place it in and charcoal is carried out in tube furnace
Change, carbonization temperature is 650 DEG C, is incubated 2h, programming rate is 5~10 DEG C/min.Nitrogenous multi-stage porous Carbon Materials are obtained after charing.
Embodiment 5
18g urea is dissolved in 20ml deionized waters, cigarette filter is then soaked into 18min in urea liquid, is soaked
25min is placed after bubble in an oven, temperature setting is 90 DEG C.By 1.8mg graphene oxides in 2ml ethanol ultrasonic disperse.So
Afterwards will in urea liquid soak after and dry cigarette filter soak 60s in the alcohol dispersion liquid of graphene oxide after take
Go out, 6min is shelved on culture dish, is then soaked again.This process repeats 30 times.Finally place it in and charcoal is carried out in tube furnace
Change, carbonization temperature is 800 DEG C, is incubated 2.5h, programming rate is 5~10 DEG C/min.Nitrogenous multi-stage porous raw material of wood-charcoal is obtained after charing
Material.
Claims (10)
- A kind of 1. nitrogenous multi-stage porous Carbon Materials, it is characterised in that using the cigarette filter of recovery as carbon matrix precursor carbon material, with Urea is nitrogen source, by the cigarette filter to the recovery containing urea, is soaked in the alcohol dispersion liquid of graphene oxide, and Obtained after charing process.
- 2. a kind of nitrogenous multi-stage porous Carbon Materials according to claim 1, it is characterised in that the recovery containing urea Cigarette filter, by the way that immersion, drying obtain in concentration is 0.5~1g/ml aqueous solution of urea by the cigarette filter of recovery.
- 3. a kind of nitrogenous multi-stage porous Carbon Materials according to claim 1, it is characterised in that the cigarette filter soaks oxygen After the alcohol dispersion liquid drying of graphite alkene, single quality increases by 5~20mg.
- 4. a kind of preparation method of nitrogenous multi-stage porous Carbon Materials, it is characterised in that specifically implement according to following steps：Step 1, cigarette filter is soaked in aqueous solution of urea, dried, then in the alcohol dispersion liquid of graphene oxide Immersion is several times；Step 2, the cigarette filter after step 1 processing carbonize painstakingly, that is, obtain nitrogenous multi-stage porous Carbon Materials.
- A kind of 5. preparation method of nitrogenous multi-stage porous Carbon Materials according to claim 4, it is characterised in that the step 1 The mass volume ratio of middle cigarette filter and aqueous solution of urea is 0.01~0.05g/ml.
- A kind of 6. preparation method of nitrogenous multi-stage porous Carbon Materials according to claim 4, it is characterised in that the step 1 Middle drying temperature is 70~100 DEG C, and the time is 20~30min.
- A kind of 7. preparation method of nitrogenous multi-stage porous Carbon Materials according to claim 4, it is characterised in that the step 1 The alcohol dispersion liquid concentration of middle graphene oxide is 0.5~1g/L.
- A kind of 8. preparation method of nitrogenous multi-stage porous Carbon Materials according to claim 4, it is characterised in that the cigarette mistake Filter tip soaks 20~30 times in the alcohol dispersion liquid of graphene oxide, shelves 2~6min after immersion every time, then carry out next time Immersion, it is desirable to which single quality increases by 5~20mg after the cigarette filter drying after step 1 processing.
- 9. the preparation method of a kind of nitrogenous multi-stage porous Carbon Materials according to claim 4, it is characterised in that at the charing It is 600~900 DEG C to manage temperature, and soaking time is 2~3h.
- 10. the purposes of a kind of nitrogenous multi-stage porous Carbon Materials according to claim 1, it is characterised in that as super capacitor The electrode material of device.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111530465A (en) * | 2020-05-26 | 2020-08-14 | 湘潭大学 | Preparation method of supported cigarette end porous carbon material catalyst and application of supported cigarette end porous carbon material catalyst in nitrocyclohexane hydrogenation reaction |
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2017
- 2017-10-27 CN CN201711021226.XA patent/CN107720722A/en active Pending
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| US20090151738A1 (en) * | 2007-12-17 | 2009-06-18 | Celanese Acetate Llc | Degradable cigarette filter |
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| Title |
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| CHUNHUI WANG ET AL: "Graphene aerogel composites derived from recycled cigarette filters for electromagnetic wave absorption", 《J. MATER. CHEM. C》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111530465A (en) * | 2020-05-26 | 2020-08-14 | 湘潭大学 | Preparation method of supported cigarette end porous carbon material catalyst and application of supported cigarette end porous carbon material catalyst in nitrocyclohexane hydrogenation reaction |
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