CN104495820A - Porous graphene aerogel and preparation method thereof - Google Patents
Porous graphene aerogel and preparation method thereof Download PDFInfo
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- CN104495820A CN104495820A CN201410780164.0A CN201410780164A CN104495820A CN 104495820 A CN104495820 A CN 104495820A CN 201410780164 A CN201410780164 A CN 201410780164A CN 104495820 A CN104495820 A CN 104495820A
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Abstract
The invention relates to a porous graphene aerogel and a preparation method thereof. The graphene aerogel is a black spongy solid with porous structure and higher specific area. The preparation method of the graphene aerogel comprises the following steps: adding a reducer into graphene oxide, heating to reduce the graphene oxide to form a three-dimensional structure by self-assembly, and carrying out freeze-drying to obtain the graphene aerogel without destroying the three-dimensional network structure. The method is convenient and easy to control. The graphene aerogel can be used as a fuel-cell catalyst support.
Description
Technical field
The present invention relates to the preparation field of aerogel, particularly a kind of porous graphene aerogel and preparation method thereof.
Background technology
Graphene is a kind of two-dimensional slice of single atomic layer level thickness, can regard the polynuclear plane of sp2 hydbridized carbon atoms composition as.Aerogel adopts special process the liquid gas displacement in wet gel not to be changed the structure of gel network and the highly porous nano material with low density and high-specific surface area that obtains.Three-dimensional grapheme breaks through the application limitations of traditional zero dimension, a peacekeeping two-dimensional graphene, the three-dimensional structure of independently assembling with it can directly apply to electrode of super capacitor, sorbent material, catalyzer, and be greatly better than itself and binding agent etc. combine after electrochemical properties.Realize with Graphene the synthesis of the aerogel being skeleton unit, both the integrated and assemble method of a kind of three-dimensional of two-dimensional graphene had been provided, impart again specific performance when Graphene exists with aerogel form, have that porosity is high, physical strength good, the advantage that specific surface area is large, shows great application potential in catalysis, absorption and electrochemical energy storage etc.
Graphene aerogel (Graphene Aerogel:GA) is the lightest known in the world at present solid material, and there is a lot of hole its inside, is full of air.Every cubic centimetre heavy 0.16 milligram, also lighter than helium, be about the twice of same volume size hydrogen weight.It has adsorptive power that is ultrafast, superelevation to organic solvent, is the material that the oil sucting force that has been in the news is the strongest.Existing oil suction product generally can only inhale the liquid of sole mass about 10 times, and graphene aerogel can absorb about 250 times, reaches as high as 900 times, and only oil suction does not absorb water.Its this characteristic can be used to process Crude Oil at Sea incident of leakage--and graphene aerogel is spread across the sea, just leakage of oil can be sucked in rapidly, because flexible, the oil of inspiration is extruded, and also can recycle.
Therefore, how to obtain Graphene airsetting knot when keeping Graphene original structure feature, thus the performance such as conduction, heat conduction, mechanics farthest utilizing Graphene excellent, be one of important topic of this area scientific worker research.The preparation method of grapheme material has following a few class mechanically peel method, epitaxial growth method, vapour deposition process and arc discharge method usually, but above method needs harsh experiment condition usually, and differ and generate aerogel surely, laboratory preparation method prepares graphene aerogel based on graphene oxide.Its preparation method mainly contains: 1, self-assembly method is redox graphene, generates graphene sheet layer, and the overlap joint of stacking voluntarily of graphene sheet layer forms aerogel structure; 2, construction from part principle is induced to be that graphene oxide is that a kind of colloidal dispersion system thermodynamically belongs to unsure state.Under the inducing action in the external world, the balance of system can be broken, and may realize Graphene gel structure when reaching new balance; 3, chemical crosslink technique adds other components further in the process preparing gel with graphene oxide, between lamella, introduce the structure and properties that chemically crosslinked carrys out modulation graphene aerogel, improve and connected by Van der Waals force between graphene aerogel lamella and the application limitation caused; 4, the template that template uses comprises Nano microsphere class template and foam class template.The present invention is mainly based on the chemical reduction ratio juris in self-assembly method, and by selecting chemical reducing agent to carry out redox graphene, the electrostatic repulsion taken off except reducing graphene film interlayer of functional group, graphene sheet layer overlap joint forms three-dimensional structure.The method relative to the advantage of above additive method is: simple to operate, simple flow, reaction conditions are less demanding, be easier to suitability for industrialized production, and additive method reaction conditions are relatively harsh.
Summary of the invention
In order to solve problems of the prior art, the invention provides a kind of preparation method of porous graphene aerogel, be specially and add reductive agent in graphene oxide, by heat reduction graphene oxide, then three-dimensional structure is self-assembled into, and prepared by the method that cold well quick freezing and lyophilize engage, the tridimensional network of the graphene aerogel obtained can not be destroyed.
Graphene aerogel of the present invention is the black spongy solid with vesicular structure, and mean pore size is at 3-10nm, and specific surface area reaches 500-700 m
2/ g, adsorption desorption isothermal curve is typical Vth type.
Preparation method of the present invention specifically comprises the steps:
(1) get the graphene oxide of certain mass, be scattered in deionized water, compound concentration is the graphene oxide solution of 1mg/ml-6mg/ml, and ultrasonic and magnetic agitation hockets, and fully dispersion obtains finely dispersed graphene oxide water solution;
(2) in graphene oxide water solution, instill appropriate reductive agent, magnetic agitation is even, then pours in container after also sealing, puts into baking oven, at 90-120
obe incubated 6-18 hour under the condition of C steady temperature, obtain Graphene hydrogel;
(3) Graphene hydrogel is taken out, repeatedly carry out soaking, cleaning with deionized water;
(4) taking out Graphene hydrogel is placed in clean container, and described container is put into cold well quick freezing, and cold well temperature is-60
obelow C, then puts into after freeze drier carries out lyophilize certain hour and takes out, obtain graphene aerogel.
In a preferred embodiment of the present invention, fully 6-18 hour is disperseed in step (1).
In a preferred embodiment of the present invention, the concentration of graphene oxide solution is 5mg/ml.
In a preferred embodiment of the present invention, in above-mentioned steps (2), reductive agent used is hydrazine hydrate, and dripping quantity is 500 μ l-1000 μ l, is more preferably 750 μ l.
In a preferred embodiment of the present invention, in above-mentioned steps (2), oven temperature is set as 90-120
oc, soaking time is 6-18 hour; Preferred, oven temperature is set as 95
oc, soaking time is 12 hours.
In a preferred embodiment of the present invention, in above-mentioned steps (3), Graphene hydrogel is soaked 2 days, change water cleaning 4-6 time.
In a preferred embodiment of the present invention, in above-mentioned steps (4), lyophilize 24-48 hour; Preferred, lyophilize 36 hours.
The graphene aerogel that the present invention prepares can be applied to the carrier of redox catalyst, and this carrier has the advantage of tridimensional network, high-specific surface area, high porosity.
The present invention adopts a kind of simple effective method to prepare the graphene aerogel of three-dimensional porous structure, by the use of specific reductant, cold well quick freezing with to be cryodesiccatedly combined and the parameter Effective Regulation of preparation process, the graphene aerogel prepared has high-specific surface area, high porosity.Its making method is simple, and easy to operate, with low cost, superior performance, has a extensive future.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph adopting hydrazine hydrate (a), quadrol (b), xitix (c), Ursol D (d) graphene aerogel prepared by reductive agent respectively;
Fig. 2 adopts hydrazine hydrate to be the transmission electron microscope picture of graphene aerogel prepared by reductive agent;
Fig. 3 is adsorption desorption isothermal curve figure and the graph of pore diameter distribution of the graphene aerogel prepared by consumption adopting different hydrazine hydrate;
Fig. 4 is the adsorption desorption isothermal curve figure that sample is incubated the graphene aerogel prepared by different time in an oven.
Embodiment
The present invention is illustrated further below in conjunction with accompanying drawing and embodiment.It should be understood that these embodiments are only for illustration of the present invention, and be not used in and limit the scope of the invention.
embodiment 1
In the present embodiment, be that graphene aerogel prepared by reductive agent with hydrazine hydrate, concrete steps are as follows.
(1) get the graphene oxide of 100mg, be dispersed in the deionized water of 20ml, compound concentration is the graphene oxide solution of 5mg/ml, and ultrasonic and magnetic agitation hockets, and fully dispersion 12 hours, obtains finely dispersed graphene oxide water solution.
(2) in graphene aqueous solution, instill 500 μ l hydrazine hydrates, magnetic agitation half hour, then pour in weighing bottle, after sealing, weighing bottle is put into baking oven, 95
obe incubated 6 hours under the condition of C steady temperature, obtain Graphene hydrogel.
(3) Graphene hydrogel is taken out, repeatedly carry out soaking, cleaning with deionized water.
(4) taking out Graphene hydrogel is placed in suitable container, and the container holding Graphene hydrogel is put into cold well quick freezing, and cold well temperature is-60
obelow C, then puts into freeze drier and carries out lyophilize, take out, finally obtain graphene aerogel after lyophilize certain hour.
Comparative example 1:
The present embodiment is one of comparative example of above-described embodiment 1.
In the present embodiment, adopt quadrol to be that graphene aerogel prepared by reductive agent, concrete preparation method is substantially identical with the preparation method in embodiment 1.Difference replaces 500 μ l hydrazine hydrates with 500 μ l quadrols in (2) step.
Comparative example 2:
The present embodiment is the comparative example two of above-described embodiment 1.
In the present embodiment, adopt xitix to be that graphene aerogel prepared by reductive agent, concrete preparation method is substantially identical with the preparation method in embodiment 1.Difference replaces 500 μ l hydrazine hydrates with 100mg xitix in (2) step.
Comparative example 3:
The present embodiment is the comparative example three of above-described embodiment 1.
In the present embodiment, adopt Ursol D to be that graphene aerogel prepared by reductive agent, concrete preparation method is substantially identical with the preparation method in embodiment 1.Difference replaces 500 μ l hydrazine hydrates with 100mg Ursol D in (2) step.
Fig. 1 is above-described embodiment 1, comparative example 1, comparative example 2 and comparative example 3 graphene aerogel scanning electron microscope (SEM) photograph.Fig. 2 is the transmission electron microscope picture of above-described embodiment 1 graphene aerogel.Four scanning electron microscope (SEM) photographs as can be seen from Fig. 1, topographical difference is comparatively large, and hydrazine hydrate is that graphene aerogel fold prepared by reductive agent is relative with hole more, and Ursol D takes second place, and xitix and the graphene aerogel prepared by quadrol have a small amount of hole and fold.
embodiment 2
In the present embodiment, still adopt hydrazine hydrate to be that graphene aerogel prepared by reductive agent, substantially identical with embodiment 1 of its preparation method, difference is, in step (2), the infusion volume of hydrazine hydrate is become 750 μ l.
Comparative example:
The present embodiment is the comparative example of above-described embodiment 2.
In the present embodiment, adopt different amounts hydrazine hydrate to be that graphene aerogel prepared by reductive agent, concrete preparation method is substantially identical with the preparation method in embodiment 1.Difference is, in step (2), the infusion volume of hydrazine hydrate is become 1000 μ l.
Fig. 3 is above-described embodiment 1, embodiment 2, the adsorption desorption isothermal curve of embodiment 2 comparative example and graph of pore diameter distribution.Above-mentioned three adsorption desorption isothermal curves are all typical Vth types, and Pore Diameter is all at about 3.7nm, and difference is that the specific surface area difference of three kinds of samples is very large, respectively: 267.400 m
2/ g, 597.343 m
2/ g, 497.201 m
2/ g, can find out, the specific surface area of the graphene aerogel prepared when the consumption of reductive agent hydrazine hydrate is 750 μ l is maximum.
embodiment 3
In the present embodiment, still adopt hydrazine hydrate to be that graphene aerogel prepared by reductive agent, substantially identical with embodiment 1 of its preparation method, difference changes soaking time in an oven into 12 hours in step (2).
Comparative example:
The present embodiment is the comparative example of above-described embodiment 3.
In the present embodiment, adopt different soaking time to prepare graphene aerogel, concrete preparation method is substantially identical with the preparation method in embodiment 1.Difference changes soaking time in an oven into 18 hours in step (2).
Fig. 4 is above-described embodiment 1, embodiment 3, the adsorption desorption isothermal curve of embodiment 3 comparative example and graph of pore diameter distribution.Above-mentioned three adsorption desorption isothermal curves are all typical Vth types, and Pore Diameter is all between 3.7-3.8nm, and difference is that the specific surface area difference of three kinds of samples is very large, respectively: 179.406 m
2/ g, 538.206 m
2/ g, 248.141 m
2/ g, can find out, when in an oven soaking time is that the specific surface area of 12 little graphene aerogels prepared is constantly maximum.
Above-described embodiment has been described in detail technical scheme of the present invention; be understood that and the foregoing is only specific embodiments of the invention; be not limited to the present invention; all make in spirit of the present invention any amendment, supplement or similar fashion substitute etc., all should be included within protection scope of the present invention.
Claims (10)
1. the preparation method of a porous graphene aerogel, it is characterized in that, reductive agent is added in graphene oxide, by heat reduction graphene oxide, then three-dimensional structure is self-assembled into, and prepared by the method that cold well quick freezing and lyophilize engage, the tridimensional network of the graphene aerogel obtained can not be destroyed.
2. preparation method according to claim 1, is characterized in that, specifically comprises the steps:
(1) get the graphene oxide of certain mass, be scattered in deionized water, compound concentration is the graphene oxide solution of 1mg/ml-6mg/ml, and ultrasonic and magnetic agitation hockets, and fully dispersion obtains finely dispersed graphene oxide water solution;
(2) in graphene oxide water solution, instill appropriate reductive agent, magnetic agitation is even, then pours in container after also sealing, puts into baking oven, at 90-120
obe incubated 6-18 hour under the condition of C steady temperature, obtain Graphene hydrogel;
(3) Graphene hydrogel is taken out, repeatedly carry out soaking, cleaning with deionized water;
(4) taking out Graphene hydrogel is placed in clean container, and described container is put into cold well quick freezing, and cold well temperature is-60
obelow C, then puts into after freeze drier carries out lyophilize certain hour and takes out, obtain graphene aerogel.
3. preparation method according to claim 2, is characterized in that, in step (1), the concentration of graphene oxide solution is 5mg/ml, fully dispersion 6-18 hour.
4. preparation method according to claim 1 and 2, is characterized in that, in step (2), reductive agent used is hydrazine hydrate, and dripping quantity is 500 μ l-1000 μ l.
5. preparation method according to claim 1 and 2, is characterized in that, in step (2), reductive agent used is hydrazine hydrate, and dripping quantity is 750 μ l.
6. preparation method according to claim 2, is characterized in that, in above-mentioned steps (2), oven temperature is set as 90-120
oc, soaking time is 6-18 hour.
7. preparation method according to claim 2, is characterized in that, in above-mentioned steps (3), Graphene hydrogel is soaked 2 days, changes water cleaning 4-6 time.
8. preparation method according to claim 2, is characterized in that, in above-mentioned steps (4), and lyophilize 24-48 hour.
9. the graphene aerogel that the preparation method according to any one of claim 1-8 prepares, is characterized in that, described graphene aerogel has the black spongy solid of vesicular structure, and mean pore size is at 3-10nm, and specific surface area reaches 500-700 m
2/ g, adsorption desorption isothermal curve is typical Vth type.
10. the graphene aerogel described in claim 9 is applied to the carrier of redox catalyst.
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| CN105126751A (en) * | 2015-06-26 | 2015-12-09 | 中国航空工业集团公司北京航空材料研究院 | Graphene porous material for adsorbing flue gas |
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| CN106082202A (en) * | 2016-06-29 | 2016-11-09 | 北京化工大学 | A kind of preparation method and application of graphene aerogel |
| CN106477562A (en) * | 2016-09-27 | 2017-03-08 | 清华大学 | A kind of preparation of self assembled three-dimensional graphene macroform powdery absorbent and application |
| CN106517162A (en) * | 2016-12-15 | 2017-03-22 | 中国航空工业集团公司北京航空材料研究院 | Preparation method of nitrogen/ sulphur co-doping three-dimensional graphene sponge |
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