CN105480969A - Method for preparing three-dimensional graphene by adopting ethyl cellulose as raw material - Google Patents
Method for preparing three-dimensional graphene by adopting ethyl cellulose as raw material Download PDFInfo
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- CN105480969A CN105480969A CN201511024460.9A CN201511024460A CN105480969A CN 105480969 A CN105480969 A CN 105480969A CN 201511024460 A CN201511024460 A CN 201511024460A CN 105480969 A CN105480969 A CN 105480969A
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- ethyl cellulose
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/30—Three-dimensional structures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
Abstract
The invention discloses a method for preparing three-dimensional graphene by adopting ethyl cellulose as the raw material. The method comprises the steps that analytically pure ethyl cellulose and NaOH are dissolved in ethyl alcohol according to the molar ratio of 1 to 1-3 to form sol, aging is conducted on the obtained sol for 12 h to obtain gel, and the gel is dried at 80 DEG C for 6 h to obtain dried gel; carbonization is conducted on the obtained dried gel in an argon atmosphere at the temperature ranging from 700 DEG C to 1000 DEG C, a carbonized product is washed through deionized water till PH of a solution ranges from 6.8 to 7.2, suction filtration is conducted on the solution, a product is obtained, the product is dried for 5 h at 60 DEG C, and the product three-dimensional graphene is obtained. The method for preparing the three-dimensional graphene takes the ethyl cellulose as the raw material, the three-dimensional graphene is prepared by adopting a sol-gel method, the raw material of the reaction is easy to obtain, the cost is low, process equipment is simple, and energy consumption is low.
Description
Technical field
The present invention relates to technical field of graphene, particularly a kind of method preparing three-dimensional grapheme.
Background technology
Graphene is that carbon atom is with sp
2the chip architecture that hydridization is formed, because it has large specific surface area, good conductivity, good physical and chemical stability, high light transmission rate and high physical strength, since being found just to attract attention.
But have stronger Van der Waals force between graphene film, make between sheet easily superimposed, its specific surface area declines, thus causes its performance to be restricted.Three-dimensional grapheme is caused by Graphene self-assembly, not only has the specific surface area that Graphene is large, has the specific conductivity compared favourably with Graphene simultaneously, makes it have larger application prospect at energy storage technology and catalytic field.
The method the preparing three-dimensional grapheme main template-CVD [ZongpingChen reported at present, WencaiRen, LiboGao, BiluLiu, SongfengPeiandHui-MingCheng, Three-dimensionalflexibleandconductiveinterconnectedgrap henenetworksgrownbychemicalvapourdeposition [J], NatureMaterials, 10, 424 – 428 (2011)], graphene oxide self-assembly method [YuxiXu, ZhaoyangLin, FlexibleSolid-StateSupercapacitorsBasedonThreeDimensiona lGrapheneHydrogelFilms [J] .ACSNANO, 5, 4042-4049 (2013], biological carbon synthesis method [Xiang-FenJiang, Xue-BinWang, High-throughputfabricationofstruttedgraphenebyammonium-a ssistedchemicalblowingforhigh-performancesupercapacitors [J], Nanoenergy, 2015, 16:81-90] wherein template-CVD need sacrifice template, the Nonrenewable resources such as methane are adopted to be raw materials for production, cause production cost high, productive rate is low.It is precursor that graphene oxide self-assembly method need prepare graphene oxide, complex process, and production cost is high, is unfavorable for scale operation.
Summary of the invention
The object of the present invention is to provide a kind of ethyl cellulose that adopts to be the method that three-dimensional grapheme prepared by raw material, this equipment requirements is low, technique is simple, energy consumption is low and easily control.
In order to achieve the above object, the present invention adopts following technical scheme:
Adopt ethyl cellulose to be the method that three-dimensional grapheme prepared by raw material, comprise the following steps:
1) analytical pure ethyl cellulose and NaOH are dissolved in obtained colloidal sol in ethanol with the mol ratio of 1:1 ~ 3;
2) by the at room temperature ageing of prepared colloidal sol, gel is obtained;
3) gained gel drying is obtained xerogel;
4) be protection gas with argon gas by xerogel, in tube furnace, carbonizing treatment is carried out in 700 ~ 1000 DEG C of insulations;
5) by the product deionized water wash after carbonization until solution PH=6.8 ~ 7.2, by solution suction filtration, obtain product, obtain three-dimensional grapheme by after product drying.
Further, step 2) in digestion time be 12h.
Further, step 3) in by gained gel at 60 DEG C of dry 6h, obtain xerogel;
Further, step 4) in time of carbonizing treatment be 3h.
Further, step 4) in specifically product is obtained three-dimensional grapheme at 60 DEG C of dry 5h.
Further, a kind of ethyl cellulose that adopts of the present invention is the method that three-dimensional grapheme prepared by raw material, comprises the following steps:
1) analytical pure ethyl cellulose and NaOH are dissolved in obtained colloidal sol in ethanol with the mol ratio of 1:2;
2) by prepared colloidal sol at room temperature ageing 12h, gel is obtained;
3) by gained gel at 60 DEG C of dry 6h, obtain xerogel;
4) by xerogel with argon gas be protection gas, 900 DEG C of insulation 3h carry out carbonizing treatment;
5) by the product deionized water wash after carbonization until solution PH=7.0, by solution suction filtration, obtain product, at 60 DEG C of dry 5h, obtain three-dimensional grapheme.
Further, step 1) middle ethanol: the mass ratio of the mixture of ethyl cellulose and NaOH is 15 ~ 30:1.
Relative to prior art, the present invention has following beneficial effect:
The present invention take ethyl cellulose as raw material, sol-gel method is adopted to prepare three-dimensional grapheme, the raw material of this reaction is easy to get and cost is low, and processing unit is simple, and energy consumption is low, and this reaction is carried out at ambient pressure, using ethanol as reaction solvent, security is good, and feasibility is strong, so very economical, practical, there is good industrial prospect.The three-dimensional grapheme prepared has good charge storage performance, greatly reduces production cost simultaneously, has larger industrial prospect.
Accompanying drawing explanation
Fig. 1 is the Raman spectrogram of three-dimensional grapheme prepared by the present invention;
Fig. 2 is the SEM figure of prepared three-dimensional grapheme.
Embodiment
Embodiment 1
Adopt ethyl cellulose to be the method that three-dimensional grapheme prepared by raw material, comprise the following steps:
1) analytical pure ethyl cellulose and NaOH are dissolved in obtained colloidal sol in ethanol in proper amount (ethanol: the mass ratio of the mixture of ethyl cellulose and NaOH is for 20:1) with the mol ratio of 1:1;
2) by prepared colloidal sol at room temperature ageing 12h, gel is obtained;
3) by gained gel at 60 DEG C of dry 6h, obtain xerogel;
4) by xerogel with argon gas be protection gas, 900 DEG C of insulation 3h carry out carbonizing treatment;
5) by the product deionized water wash after carbonization until solution PH=6.8, by solution suction filtration, obtain product, at 60 DEG C of dry 5h, obtain three-dimensional grapheme.
Embodiment 2
Adopt ethyl cellulose to be the method that three-dimensional grapheme prepared by raw material, comprise the following steps:
1) analytical pure ethyl cellulose and NaOH are dissolved in obtained colloidal sol in ethanol in proper amount (ethanol: the mass ratio of the mixture of ethyl cellulose and NaOH is for 15:1) with the mol ratio of 1:3;
2) by prepared colloidal sol at room temperature ageing 12h, gel is obtained;
3) by gained gel at 60 DEG C of dry 6h, obtain xerogel;
4) by xerogel with argon gas be protection gas, 700 DEG C of insulation 3h carry out carbonizing treatment;
5) by the product deionized water wash after carbonization until solution PH=7.0, by solution suction filtration, obtain product, at 60 DEG C of dry 5h, obtain three-dimensional grapheme.
Embodiment 3
Adopt ethyl cellulose to be the method that three-dimensional grapheme prepared by raw material, comprise the following steps:
1) analytical pure ethyl cellulose and NaOH are dissolved in right amount obtained colloidal sol in (ethanol: the mass ratio of the mixture of ethyl cellulose and NaOH is for 20:1) with the mol ratio of 1:2;
2) by prepared colloidal sol at room temperature ageing 12h, gel is obtained;
3) by gained gel at 60 DEG C of dry 6h, obtain xerogel;
4) by xerogel with argon gas be protection gas, 900 DEG C of insulation 3h carry out carbonizing treatment;
5) by the product deionized water wash after carbonization until solution PH=7.0, by solution suction filtration, obtain product, at 60 DEG C of dry 5h, obtain three-dimensional grapheme.
Embodiment 4
Adopt ethyl cellulose to be the method that three-dimensional grapheme prepared by raw material, comprise the following steps:
1) analytical pure ethyl cellulose and NaOH are dissolved in obtained colloidal sol in ethanol in proper amount (ethanol: the mass ratio of the mixture of ethyl cellulose and NaOH is for 30:1) with the mol ratio of 1:3;
2) by prepared colloidal sol at room temperature ageing 12h, gel is obtained;
3) by gained gel at 60 DEG C of dry 6h, obtain xerogel;
4) by xerogel with argon gas be protection gas, 800 DEG C of insulation 3h carry out carbonizing treatment;
5) by the product deionized water wash after carbonization until solution PH=7.2, by solution suction filtration, obtain product, at 60 DEG C of dry 5h, obtain three-dimensional grapheme.
Fig. 1 is the Raman spectrogram of three-dimensional grapheme prepared by the embodiment of the present invention 3, and Fig. 2 is the SEM figure of prepared three-dimensional grapheme, as can be seen from the figure for product is the Graphene with three-dimensional structure.
Claims (7)
1. adopt ethyl cellulose to be the method that three-dimensional grapheme prepared by raw material, it is characterized in that, comprise the following steps:
1) analytical pure ethyl cellulose and NaOH are dissolved in obtained colloidal sol in ethanol with the mol ratio of 1:1 ~ 3;
2) by the at room temperature ageing of prepared colloidal sol, gel is obtained;
3) gained gel drying is obtained xerogel;
4) be protection gas with argon gas by xerogel, in tube furnace, carbonizing treatment is carried out in 700 ~ 1000 DEG C of insulations;
5) by the product deionized water wash after carbonization until solution PH=6.8 ~ 7.2, by solution suction filtration, obtain product, obtain three-dimensional grapheme by after product drying.
2. a kind of ethyl cellulose that adopts according to claim 1 is the method that three-dimensional grapheme prepared by raw material, it is characterized in that, step 2) in digestion time be 12h.
3. a kind of ethyl cellulose that adopts according to claim 1 is the method that three-dimensional grapheme prepared by raw material, it is characterized in that, step 3) in by gained gel at 60 DEG C of dry 6h, obtain xerogel.
4. a kind of ethyl cellulose that adopts according to claim 1 is the method that three-dimensional grapheme prepared by raw material, it is characterized in that, step 4) in time of carbonizing treatment be 3h.
5. a kind of ethyl cellulose that adopts according to claim 1 is the method that three-dimensional grapheme prepared by raw material, it is characterized in that, step 4) in specifically product is obtained three-dimensional grapheme at 60 DEG C of dry 5h.
6. a kind of ethyl cellulose that adopts according to claim 1 is the method that three-dimensional grapheme prepared by raw material, it is characterized in that, comprises the following steps:
1) analytical pure ethyl cellulose and NaOH are dissolved in obtained colloidal sol in ethanol with the mol ratio of 1:2;
2) by prepared colloidal sol at room temperature ageing 12h, gel is obtained;
3) by gained gel at 60 DEG C of dry 6h, obtain xerogel;
4) by xerogel with argon gas be protection gas, 900 DEG C of insulation 3h carry out carbonizing treatment;
5) by the product deionized water wash after carbonization until solution PH=7.0, by solution suction filtration, obtain product, at 60 DEG C of dry 5h, obtain three-dimensional grapheme.
7. a kind of ethyl cellulose that adopts according to claim 1 is the method that three-dimensional grapheme prepared by raw material, it is characterized in that, step 1) middle ethanol: the mass ratio of the mixture of ethyl cellulose and NaOH is 15 ~ 30:1.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108190871A (en) * | 2018-03-13 | 2018-06-22 | 陕西科技大学 | It is a kind of to prepare the method with three-dimensional class graphene structural carbon material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104692368A (en) * | 2015-02-11 | 2015-06-10 | 武汉科技大学 | Graphene prepared by taking cellulose as raw material and preparation method thereof |
| CN105060289A (en) * | 2015-09-21 | 2015-11-18 | 中南大学 | Method for preparing fewer-layer graphene on basis of biomass waste |
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- 2015-12-30 CN CN201511024460.9A patent/CN105480969A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104692368A (en) * | 2015-02-11 | 2015-06-10 | 武汉科技大学 | Graphene prepared by taking cellulose as raw material and preparation method thereof |
| CN105060289A (en) * | 2015-09-21 | 2015-11-18 | 中南大学 | Method for preparing fewer-layer graphene on basis of biomass waste |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108190871A (en) * | 2018-03-13 | 2018-06-22 | 陕西科技大学 | It is a kind of to prepare the method with three-dimensional class graphene structural carbon material |
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