CN108117061A - The method for producing grapheme foam - Google Patents
The method for producing grapheme foam Download PDFInfo
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- CN108117061A CN108117061A CN201810076928.6A CN201810076928A CN108117061A CN 108117061 A CN108117061 A CN 108117061A CN 201810076928 A CN201810076928 A CN 201810076928A CN 108117061 A CN108117061 A CN 108117061A
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- grapheme foam
- graphene oxide
- fuel molecule
- muffle furnace
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Abstract
The invention discloses a kind of methods for producing grapheme foam, which is characterized in that synthesizes graphene oxide by chemical oxidization method, then fuel molecule is added in graphene oxide solution, become thick gel by mixing, heating, final high temperature is lighted, and obtains product grapheme foam.This method is simple for process, available for extensive synthesizing graphite alkene foamed material；This method is by regulating and controlling the amount of fuel molecule and the temperature of Muffle furnace, so as to control the network cavernous structure of product grapheme foam；The product grapheme foam produced has three-dimensional cavernous structure, has low-density, good electric conductivity, adsorptivity and stability.
Description
Technical field
The present invention relates to technical field of function materials, more particularly to a kind of method for producing grapheme foam.
Background technology
Graphene experienced rapid development so far as a kind of emerging star's material from discovery.Graphene is by carbon
The two-dimensional material of atomic building has good electricity, mechanical characteristic, there is very wide application prospect.As one kind microcosmic two
Material is tieed up, the application of graphene is subject to more limitation, and the macroscopic viewization material of graphene can greatly promote applicability, promote it
Development and application.Based on the three-dimensional macro material of two-dimensional graphene material structure, such as grapheme foam, there is good conductive and heat-conductive
Performance, absorption property etc., available for multiple fields such as the energy, catalysis, sensings.However grapheme material synthesis is difficult, price is held high
It is expensive, constrain its industrial applications and development.
For this purpose, global scientist and enterprise scientific research personnel have carried out a large amount of explorations in the manufacture of grapheme foam material,
And obtain remarkable progress.There is the synthetic technology of some grapheme foams now.For example, Chinese patent literature
CN106629685A discloses a kind of three-dimensional graphene foam with multilevel hierarchy and preparation method thereof, specifically discloses one kind
The method that chemical vapor deposition is carried out on metal foam skeleton prepares grapheme foam.Chinese patent literature CN103213978A
A kind of manufacturing method of grapheme foam is disclosed, specifically discloses the method freezed again with hydro-thermal process graphene oxide solution
Prepare graphene porous foam.But the method for the synthesizing graphite alkene macroscopic bubbles material of above-mentioned patent offer, step is various,
Required instrument is complicated, and manufacture is with high costs, it is difficult to mass produce.Therefore, seek it is a kind of it is efficient, cheap, can advise greatly
The technique of mould synthesizing graphite alkene foam is extremely urgent.
The content of the invention
Based on drawbacks described above, it is an object of the invention to provide a kind of method for efficiently producing grapheme foam, the party
Method can realize simple and quick, scale the preparation of high-performance, multi-functional grapheme foam；Graphene prepared by this method
Foam has preferable electric conductivity, adsorptivity and stability.
Above-mentioned purpose is achieved through the following technical solutions：
A kind of method for producing grapheme foam, which is characterized in that comprise the following steps：
Step 1: graphene oxide is prepared with chemical oxidization method；
It Step 2: by the graphene oxide, is dispersed in water, obtains graphene oxide solution；
Step 3: fuel molecule is uniformly mixed with the graphene oxide solution, mixed solution is obtained；
Step 4: to the mixed solution continuous heating, until becoming sticky colloid；
It is heated Step 5: the colloid is put into the Muffle furnace of preheating, obtains the grapheme foam.
Preferably, the concentration of the graphene oxide solution is 6-10mg/mL；It is highly preferred that the graphene oxide is molten
The concentration of liquid is 6mg/mL.
Preferably, in step 1, the chemical oxidization method utilizes the concentrated sulfuric acid and potassium permanganate oxidation to improve Hummer methods
Graphite composite powder prepares the graphene oxide, wherein, the mass ratio (1-1.5) of the concentrated sulfuric acid and the potassium permanganate:1.
Preferably, the fuel molecule is dissolved in water, in air can completely burned, burning generates a large amount of gases, described
Gas includes CO2、H2O and N2, the burning point of the fuel molecule is 150-500 degrees Celsius.The graphene oxide has oxidation
Property, fuel molecule burns, releases a large amount of gases, network cavernous structure is formed between graphene layer at high temperature.
Preferably, the fuel molecule includes glycine (C2H5NO2), alanine (C3H7NO2), urea (CO (NH2)2) with
And sucrose (C12H22O11) in one or more.Preferably, the fuel molecule is glycine；Or preferably, the fuel
Molecule is for glycine with urea with mass ratio 1:1 mixing.
Preferably, control product by controlling the ratio of the fuel molecule and the graphene oxide, i.e., by pair
The adjusting of the concentration of the graphene oxide solution and the quality of the fuel molecule added in, to control the knot of grapheme foam
Structure difference and reducing degree.
Preferably, in step 3, the fuel molecule is 5 with the graphene oxide mass ratio:1-25:1, due to described
The limitation of the solubility of fuel molecule, in step 3, the preferred 20ml of graphene oxide solution volume.It is highly preferred that step
In three, 1-3 grams of the fuel molecule is added in the graphene oxide solution of 20ml, is uniformly mixed.Further,
The fuel molecule of 2g is added to the concentration of 20ml to be uniformly mixed in the graphene oxide solution of 6-10mg/mL.
Preferably, in step 4, the mixed solution is heated to 120-150 degrees Celsius, continues 5-20 minutes, until becoming
For sticky colloid.It is highly preferred that by mixed solution continuous heating 10-15 minutes.
Preferably, in step 5, the preheating temperature of the Muffle furnace is arranged to 150-500 degrees Celsius, the preheating temperature
On the burning point of the fuel molecule, the colloid heats 15-60s in the Muffle furnace；It is highly preferred that the Muffle furnace
Preheating temperature be arranged to 350-400 degrees Celsius, the colloid takes out after placing 30s in Muffle furnace, obtains the porous of black
Shape froth pulp is the grapheme foam.The product has three-dimensional cavernous structure, and density is relatively low, has and preferably leads
Electrically, adsorptivity, stability.
Advantageous effect：
The method of present invention production grapheme foam is by regulating and controlling the amount of fuel molecule and the temperature of Muffle furnace, so as to control
The network cavernous structure of product grapheme foam.In general, fuel molecule is more, and temperature is higher, and combustion reaction is more violent, obtains
The hole arrived is bigger, and hole density is higher, and integral material density is smaller, but correspondingly, mechanical strength can die down.
This method has the following advantages：(1) this method is simple and quick, is easy and fast to, large-scale production graphene
Foamed material；(2) grapheme foam produced has three-dimensional cavernous structure, and density is relatively low, has preferable electric conductivity, suction
Attached property, stability, there are many application prospects；(3) grapheme foam produced by the invention has in the energy, sensing, catalysis etc.
Huge market application foreground.
Description of the drawings
Fig. 1 is the vesicular texture figure that grapheme foam electron scanning micrograph of the present invention is shown.
Fig. 2 is the porous structure figure that grapheme foam transmission electron microscope photo of the present invention is shown.
Fig. 3 is Raman spectrum the results show figure of the present invention.
Fig. 4 is XRD of the present invention (X ray diffracting spectrum) the results show figure.
Fig. 5 is FTIR of the present invention (fourier transform infrared spectroscopy) the results show figure.
Specific embodiment
With reference to the specific embodiment of the present invention and attached drawing 1-5, technical scheme is carried out clear, complete
Whole description.
A kind of method for producing grapheme foam, which is characterized in that comprise the following steps：
Step 1：Graphene oxide is prepared with chemical oxidization method, for the chemical oxidization method to improve Hummer methods, utilization is dense
Sulfuric acid and potassium permanganate oxidation graphite composite powder prepare the graphene oxide, wherein, the concentrated sulfuric acid and the potassium permanganate
Mass ratio (1-1.5):1；
Step 2：The graphene oxide is dispersed in water, it is molten to obtain the graphene oxide that concentration is 6-10mg/mL
Liquid, more preferable concentration are the graphene oxide solution of 6mg/mL；
Step 3：1-3 grams of fuel molecule is added in the graphene oxide solution of 20ml, be uniformly mixed, mixed
Solution is closed, i.e., described fuel molecule is controlled with the graphene oxide mass ratio 5:1-25:Between 1；Wherein, the fuel point
Son can dissolve in water, in air can completely burned, burning generates a large amount of gases, and the gas includes CO2、H2O and N2
Deng；The burning point of the fuel molecule is 150-500 degrees Celsius；Further, the fuel molecule includes glycine (C2H5NO2),
Alanine ((C3H7NO2)), urea (CO (NH2)2) and sucrose (C12H22O11) in one or more；The graphene oxide
With oxidisability, the fuel molecule burns at high temperature, releases a large amount of gases, and the poroid knot of network is formed between graphene layer
Structure；Product is controlled by controlling the ratio of the fuel molecule and the graphene oxide, i.e., by dense to graphene oxide
The adjusting of the quality of degree and the fuel molecule added in, to control the architectural difference of grapheme foam and reducing degree；
Step 4：120-150 degrees Celsius is heated to the mixed solution, continuous heating 5-20 minutes, until becoming viscous
Thick colloid, further preferred continuous heating 10-15 minutes；
Step 5：The colloid is put into the Muffle furnace for being preheated to 150-500 degrees Celsius, is taken out after 15-60s, is obtained
The cellular foam product of black；It is highly preferred that the colloid is put into the Muffle furnace for being preheated to 350-400 degrees Celsius, institute
It states colloid and 30s is heated in Muffle furnace, obtain the cellular foam product of black, which has three-dimensional cavernous structure, and close
Spend it is relatively low, have preferable electric conductivity, adsorptivity, stability.
Grapheme foam prepared by the present invention can be seen that graphene steeps by the electron scanning micrograph of Fig. 1
Vesicular texture possessed by foam；Fig. 2 transmission electron microscope photos further illustrate the porous structure of the product, hole size
In the micron-scale；Fig. 3 Raman spectrums are the results show that 2D-band peak intensities are far above D-band and G-band, for few layer or individual layer stone
Black alkene is different from the main feature of multi-layer graphene, while G-band peak intensities are more slightly higher than D-band, shows preferable crystallization
Property；Fig. 4 XRD (X ray diffracting spectrum) are the results show that the diffraction maximum of product at 25 degree or so, is the characteristic peak of graphene, and oxygen
The diffraction maximum (10 degree) of graphite completely disappears in the product, shows that graphite oxide is reduced to graphene completely；Fig. 5 FTIR
(fourier transform infrared spectroscopy) shows oxygen the results show that the corresponding peak of C-O functional groups in graphite oxide disappears in the product
Graphite is reduced to graphene completely.
With reference to specific embodiment, technical scheme is clearly and completely described.It is to be understood that these
Embodiment is only illustrative of the invention and is not intended to limit the scope of the invention.Furthermore, it is to be understood that it is reading in the present invention
After appearance, those skilled in the art can make various modifications or changes to the present invention, and such equivalent forms equally fall within the application
The appended claims limited range.
Embodiment one：
Graphene oxide is prepared using improvement Hummer methods first：2g powdered graphites mix 12ml under 80 degrees Celsius of constant temperature
The concentrated sulfuric acid, 2.5g phosphorus pentoxides and 2.5g potassium peroxydisulfates；Reaction is vigorously stirred when 80 degree of holdings 24 are small；Afterwards, by 500ml
Deionized water is slowly added into mixture；Then solution is filtered, and with deionized water rinsing until filtrate pH is neutral；Filter
Cake is dried at room temperature for obtaining black powder, and it is added under ice bath in the 120ml concentrated sulfuric acids and 30ml concentrated nitric acids；Then will
15g potassium permanganate is stirred while being slowly added in above-mentioned solution；After the completion of mixing, it is small to be heated to 35 degrees Celsius of stirrings 96
When, obtain thick liquid；1L deionized waters are then added in, and are slowly added to 30% hydrogen peroxide of 20ml, obtain yellow solution；
Finally solution is filtered, and with 1LHCl solution (1:10) and deionized water rinsing until filtrate for neutrality, filtration cakes torrefaction is treated
With.The graphene oxide water solution of respective concentration is then prepared with deionized water.
The graphene oxide water solution 20ml of 6mg/mL is prepared, 2 grams of glycine is added in solution, is uniformly mixed, obtains
To mixed solution；Then mixed solution is heated to 150 degrees Celsius, continues 10 minutes, until becoming sticky colloid；Finally will
The colloid, which is put into, to be preheated in 250 degree of Muffle furnace, is taken out after 30 seconds, obtains the cellular foam product of black.
Embodiment two：
The graphene oxide water solution 20ml of 6mg/mL is prepared, 2 grams of fuel combination is added in solution, the mixing combustion
Material includes glycine and urea, mass ratio 1:1, it is uniformly mixed, obtains mixed solution；Then mixed solution is heated to 120
Degree Celsius, continue 15 minutes, until becoming sticky colloid；Finally the colloid is put into and is preheated in 400 degree of Muffle furnace, 30
It is taken out after second, obtains the cellular foam product of black.
The method of present invention production grapheme foam is by regulating and controlling the amount of fuel molecule and the temperature of Muffle furnace, so as to control
The network cavernous structure of product grapheme foam；This method is simple and quick, is easy and fast to, large-scale production grapheme foam
Material.This method products obtained therefrom has three-dimensional cavernous structure, and density is relatively low, has preferable electric conductivity, adsorptivity, stabilization
Property, there is huge market application foreground.
Claims (10)
- A kind of 1. method for producing grapheme foam, which is characterized in that comprise the following steps：Step 1: graphene oxide is prepared with chemical oxidization method；Step 2: the graphene oxide is dispersed in water, graphene oxide solution is obtained；Step 3: fuel molecule is uniformly mixed with the graphene oxide solution, mixed solution is obtained；Step 4: to the mixed solution continuous heating, until becoming sticky colloid；It is heated Step 5: the colloid is put into the Muffle furnace of preheating, obtains the grapheme foam.
- 2. the method for production grapheme foam as described in claim 1, which is characterized in that in step 1, using the concentrated sulfuric acid and Potassium permanganate oxidation powdered graphite prepares the graphene oxide, wherein, the mass ratio of the concentrated sulfuric acid and the potassium permanganate For 1-1.5:1.
- 3. the method for production grapheme foam as described in claim 1, which is characterized in that wherein, the graphene oxide is molten The concentration of liquid is 6-10mg/mL.
- 4. the method for production grapheme foam as claimed in claim 3, which is characterized in that, will be described in 1-3g in step 3 Fuel molecule is added in the graphene oxide solution of 20ml, is uniformly mixed.
- 5. the method for production grapheme foam as described in claim 1, which is characterized in that wherein, the fuel molecule is dissolved in Water, in air can completely burned, the gas of generation of burning includes CO2、H2O and N2, the burning point of the fuel molecule is 150-500 degrees Celsius.
- 6. the method for production grapheme foam as claimed in claim 5, which is characterized in that wherein, the fuel molecule includes Glycine, alanine, one or more of urea and sucrose.
- 7. the method for production grapheme foam as described in claim 1, which is characterized in that in step 4, the mixing is molten Liquid is heated to 120-150 degrees Celsius, continues 5-20 minutes, until becoming sticky colloid.
- 8. the method for production grapheme foam as claimed in claim 7, which is characterized in that in step 4, the mixing is molten Liquid continuous heating 10-15 minutes.
- 9. the method for production grapheme foam as claimed in claim 5, which is characterized in that in step 5, the Muffle furnace Preheating temperature is arranged to 150-500 degrees Celsius, and the preheating temperature, on the burning point of the fuel molecule, the colloid exists 15-60s is heated in the Muffle furnace.
- 10. the method for production grapheme foam as claimed in claim 9, which is characterized in that in step 5, the Muffle furnace Preheating temperature is arranged to 350-400 degrees Celsius, and the colloid takes out after heating 30s in Muffle furnace.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810076928.6A CN108117061A (en) | 2018-01-26 | 2018-01-26 | The method for producing grapheme foam |
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| CN201810076928.6A CN108117061A (en) | 2018-01-26 | 2018-01-26 | The method for producing grapheme foam |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105668562A (en) * | 2016-04-13 | 2016-06-15 | 北京晶晶星科技有限公司 | Preparation method of graphene |
| CN105688763A (en) * | 2016-04-08 | 2016-06-22 | 江苏大学 | Method for preparing platinum nano particle supported nitrogen-doped three-dimensional graphene aerogel via one-step method |
| CN106311223A (en) * | 2016-08-16 | 2017-01-11 | 南昌大学 | Preparation method of precious metal/graphene nanocomposite |
-
2018
- 2018-01-26 CN CN201810076928.6A patent/CN108117061A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105688763A (en) * | 2016-04-08 | 2016-06-22 | 江苏大学 | Method for preparing platinum nano particle supported nitrogen-doped three-dimensional graphene aerogel via one-step method |
| CN105668562A (en) * | 2016-04-13 | 2016-06-15 | 北京晶晶星科技有限公司 | Preparation method of graphene |
| CN106311223A (en) * | 2016-08-16 | 2017-01-11 | 南昌大学 | Preparation method of precious metal/graphene nanocomposite |
Non-Patent Citations (1)
| Title |
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| YECHENG LI ET AL: "Synthesis of 3D structured graphene as a high performance catalyst support for methanol electro-oxidation", 《NANOSCALE》 * |
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