CN106517160B - A kind of preparation method of isotropism super-elasticity graphene aerogel - Google Patents
A kind of preparation method of isotropism super-elasticity graphene aerogel Download PDFInfo
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- C01B2204/00—Structure or properties of graphene
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Abstract
The present invention provides a kind of preparation methods of isotropism super-elasticity graphene aerogel.Graphene oxide aqueous dispersions, reducing agent are mixed with lauryl sodium sulfate (SDS) stirring at low speed first, later high-speed stirred；Heating, then freezed, it after melting at room temperature, is cleaned with ethyl alcohol, constant pressure and dry obtains isotropism super-elasticity graphene aerogel.Present invention process is simple, is suitble to industrialized production, and isotropism is presented in gained graphene aerogel, and cell size is equal, has excellent compression reaction and good chemical property.
Description
【Technical field】
The present invention relates to a kind of preparation methods of isotropism super-elasticity graphene aerogel, belong to new material technology of preparing
Field, while also belonging to aeroge preparing technical field.
【Background technology】
Graphene aerogel is obtained by graphene sheet layer by physically or chemically crosslinking.With two kinds of aeroge and graphene
The double grading of component：Ultralight, porous, conductive, hydrophobic oleophilic oil and there is good compression resilience, these properties make stone
Black alkene aeroge has huge potential using value in terms of catalyst carrier, conductive devices, oily waste treatment and energy snubber.
Graphene aerogel is prepared by raw material of graphene oxide provides possibility for large-scale production graphene aerogel,
And template is widely used in its preparation process, compared to other organic matters as template, ice template method with it more
Add environmental protection, it is succinct the advantages that attracted the extensive concern of researcher.It is able to ice removing completely to keep the poroid knot of graphene at present
Most of method of structure is still supercritical carbon dioxide drying or freeze-drying.Application No. is the Chinese inventions of CN104925787A
Patent is prepared for pure graphene aerogel using constant pressure and dry for the first time, but the aeroge that the method obtains forms hole by template of ice
Shape structure, is formed by direction orientations of the cavernous structure along ice-crystal growth, the properties of aeroge show it is each to
Anisotropic feature, and hole wall is thicker, the specific surface area of made graphene aerogel is smaller.Application No. is in CN105600777A
For state's patent of invention using dodecyl sodium sulfate as foaming agent, the bubble generated using its stirring is template, is prepared for styrene
The grapheme foam of modification, but the invention, first with being freeze-dried again after liquid nitrogen frozen, preparation process is excessively complicated.Therefore it utilizes
Simply, effective method prepares that wall is thin, hyperelastic graphene aerogel, to realizing that its large-scale production still has important reality
Border meaning.
【Invention content】
[technical problems to be solved]
The object of the present invention is to provide a kind of preparation methods of isotropism super-elasticity graphene aerogel.
Another object of the present invention is to provide a kind of methods in regulation and control graphene aerogel aperture.
[technical solution]
Technical scheme of the present invention provides a kind of preparation method of the hyperelastic graphene aerogel of isotropism, special
Sign is：The bubble that the aeroge is formed using lauryl sodium sulfate aqueous solution in stirring is template, then in the case where heat assists
Graphene oxide is restored with reducing agent, strong π-π interact so that graphene sheet layer is arranged closely in around bubble, most
Heat drying removes extra solvent and obtains isotropic super-elasticity graphene aerogel afterwards.Its compression ratio maximum is up to 95%
More than.Wall thickness is between 100nm-160nm, and the size in aperture is between 100-500 μm.
The invention is realized by the following technical scheme：
A kind of preparation method of the hyperelastic graphene aerogel of isotropism, this method is first by graphene oxide moisture
Dispersion liquid, the aqueous solution of lauryl sodium sulfate (SDS) and reducing agent carry out stirring at low speed mixing, then high-speed stirred；Then it heats
Reduction, is allowed to form gel；Melt at room temperature after freezing；Normal pressure is dried after cleaning surpasses to get to isotropic
Elastic graphite alkene aeroge.The aperture of made graphene aerogel can be regulated and controled by the rate of stirring and the temperature of freezing, abscess
The thickness of wall can be regulated and controled by changing the concentration of graphene oxide solution.
In accordance with another preferred embodiment of the present invention, it is characterised in that this approach includes the following steps：
1) graphene oxide aqueous dispersions are prepared.
2) reducing agent, lauryl sodium sulfate aqueous solution and graphene oxide aqueous dispersions stirring at low speed are uniformly mixed；
High-speed stirred is to foam later.
3) the mixed liquor heating 30-360min in step 2) is formed into gel.
4) -80 DEG C again--10 DEG C freezing 3-12h after being cooled to room temperature the gel in step 3), it is solidifying to increase graphene
The intensity of Jiao Bi.
5) the graphene hydrogel in step 4) is cleaned, remove after impurity under normal pressure 30-70 DEG C of dry 12-48h to get
Isotropic super-elasticity graphene aerogel.
In accordance with another preferred embodiment of the present invention, it is characterised in that：Graphene oxide can be used Brodie methods,
Prepared by the Hummer of Staudenmaier methods, Hummer, s methods and improvement, the methods of s methods, preferably Hummer, and s methods are optimal
It is selected as the Hummer of improvement, s methods.
According to another preferred method of implementation of the present invention, it is characterised in that：Graphene aqueous dispersions used it is a concentration of
2-10mg·ml-1。
In accordance with another preferred embodiment of the present invention, it is characterised in that：The mode of stirring is unrestricted, and preferably magnetic force stirs
It mixes, and the rate of stirring at low speed is 60-300rmin-1, the rate of high-speed stirred is 500-2500rmin-1, preferably 1000-
2000r·min-1。
In accordance with another preferred embodiment of the present invention, it is characterised in that：The time of stirring at low speed is 3-15min, wherein
It is preferred that 5-10min；The time of high-speed stirred is 1-10min, wherein it is preferred that 2-5min.
In accordance with another preferred embodiment of the present invention, it is characterised in that：Reducing agent used be vitamin C, hydrogen iodide and
One or several kinds in hydrazine hydrate.
In accordance with another preferred embodiment of the present invention, it is characterised in that：The temperature of reduction is 60-95 DEG C, wherein it is preferred that
It is 75-85 DEG C.
In accordance with another preferred embodiment of the present invention, it is characterised in that：The size in the aperture of the graphene aerogel can
To be controlled by the temperature for adjusting freezing environment.The temperature of freezing is -10 DEG C--80 DEG C, and preferred temperature is -20 DEG C.
In accordance with another preferred embodiment of the present invention, it is characterised in that：The size in graphene aerogel aperture can pass through
Control stir speed (S.S.), graphene oxide moisture liquid concentration and cryogenic temperature are controlled.
In accordance with another preferred embodiment of the present invention, it is characterised in that：When cleaning solvent used be ethyl alcohol, methanol and
One kind in acetone.
Graphene aerogel prepared in accordance with the present invention it is characterized in that：The wall thickness of the graphene aerogel abscess can lead to
The concentration for crossing graphene oxide aqueous dispersions used is controlled.
Graphene aerogel prepared in accordance with the present invention it is characterized in that：The graphene hydrogel directly heats under normal pressure
It can be obtained graphene aerogel.
[advantageous effect]
The present invention has the following advantages that as a result of technical solution as above：
1, using the method for constant pressure and dry be prepared for isotropism and compression reaction performance reach 95% or more graphene
Aeroge.
2, the graphene aerogel cell wall prepared using this method is thinner, and thickness is between 100-160nm.
3, have isotropic structure, the modulus of vertical and horizontal basic using graphene aerogel prepared by this method
It is identical, show isotropism；And the existing graphene airsetting prepared using constant pressure and dry technology all has anisotropy.
4, the aperture of the graphene aerogel prepared using this method is adjustable between 100-500 μm, and its aperture
It is evenly distributed, size can pass through the temperature of freezing environment, the concentration regulation and control of stir speed (S.S.) and graphene oxide moisture liquid.
5, since the invention has used the atmosphere pressure desiccation of improvement, compared to freeze-drying and supercritical drying, technique is more
What is added is simple, and possibility is provided for large-scale production graphene aerogel.
【Description of the drawings】
Fig. 1 is after graphene oxide aqueous dispersions in embodiment 1, lauryl sodium sulfate aqueous solution and vitamin C mix
The front and back pictorial diagram of stirring.
Fig. 2 is embodiment 1,2,3,4 made graphene aerogel cross section scanning electron microscope (SEM) photographs.
Fig. 3 is embodiment 4 and 1 made graphene aerogel cross section scanning electron microscope (SEM) photograph of comparative example.
Fig. 4 is embodiment 4 and 1 made graphene aerogel vertical section scanning electron microscope (SEM) photograph of comparative example.
Fig. 5 is the photo that the compression of gained graphene aerogel is front and back in embodiment 3.
【Specific implementation mode】
The present invention is further described with reference to embodiment.But protection scope of the present invention is not limited only to this.
Embodiment 1.
Prepare 3mgml-1Graphene oxide aqueous dispersions.The above-mentioned graphene oxide aqueous dispersions of 6ml are taken to be placed in cylinder
In shape bottle, the 50mgml of 0.5ml is added thereto-1The vitamin C of SDS and 36mg, 300rmin-13min is stirred, then
1000r·min-1Magnetic agitation 2min is put into 80 DEG C of air dry ovens and reacts 45min, take out and be put into after being cooled to room temperature-
It freezes 3 hours in 20 DEG C of low temperature environment, melts at room temperature, then cleaned 3 times with ethyl alcohol, the hydrogel after cleaning is put into 60
DEG C air dry oven in dry keep good graphene aerogel for 24 hours to get to form.Its average pore size is 490 μm, hole
Thin and thick 100nm or so.
Embodiment 2
The type of material therefor and technological process are with embodiment 1, the difference is that a concentration of 4mgml of graphene oxide-1,
Ascorbic dosage is 48mg.Finally obtain shape and keep good cellular graphene aerogel, internal holes still it is larger its
Average pore size is 420 μm.
Embodiment 3
The type of material therefor and technological process are with embodiment 1, the difference is that a concentration of 5mgml of graphene oxide-1,
Ascorbic dosage is 60mg.It has obtained shape and has kept good graphene aerogel, internal holes size is more uniform, average
Aperture is 300 μm.Its wall thickness is 120nm.
Embodiment 4
The type of material therefor and technological process are with embodiment 1, the difference is that a concentration of 7mgml of graphene oxide-1,
Ascorbic dosage is 84mg.Obtained shape and kept good graphene aerogel, pore size distribution more uniformly and
Average pore size is 250 μm.Its wall thickness is 160nm.
Embodiment 5
The type of material therefor and technological process are with embodiment 3, the difference is that the rate stirred after mixing is 500r
min-1, finally obtained shape and kept good graphene aerogel.
Embodiment 6
The type of material therefor and technological process are with embodiment 3, the difference is that the rate of high-speed stirred is after mixing
1500r·min-1, finally obtained shape and kept good cellular graphene aerogel.
Embodiment 7
The type of material therefor and technological process are with embodiment 3, the difference is that the rate of high-speed stirred is after mixing
2000r·min-1, finally obtained shape and kept good cellular graphene aerogel.
Embodiment 8
The type and process flow embodiment 3 of material therefor, the difference is that the rate of high-speed stirred is 2500r after mixing
min-1, finally obtained shape and kept good cellular graphene aerogel.
Embodiment 9
The type of material therefor and technological process are with embodiment 3, the difference is that the rate of high-speed stirred is after mixing
3000r·min-1, finally obtained shape and kept good cellular graphene aerogel.
Embodiment 10
The type of material therefor and technological process are -80 DEG C with the temperature of freezing environment unlike embodiment 3, final
It has arrived shape and has kept good cellular graphene aerogel.Its aperture is 100 μm or so, compared with gained graphene in embodiment 3
The aperture of aeroge is small.
Comparative example 1
Prepare 5mgml-1Graphene oxide aqueous dispersions.The above-mentioned graphene oxide aqueous dispersions of 6ml are taken to be placed in cylinder
In shape bottle, the vitamin C of 60mg, 1000rmin-1Magnetic agitation 2min is put into 80 DEG C of air dry ovens and reacts 45min, takes
Go out after being cooled to room temperature to be put into -20 DEG C of refrigerator and freeze 3 hours, melts at room temperature after taking-up, cleaned 3 times with ethyl alcohol later,
The hydrogel cleaned is put into drying in 60 DEG C of air dry oven later and keeps good graphene for 24 hours to get to form
Aeroge.But this graphene aerogel wall relatively thickness is 240nm, and aperture averaging is 800 μm, shows anisotropy.
Comparative example 2
The type of material therefor and technological process are with embodiment 3, the difference is that by graphene oxide water solution, dodecyl
Direct 2000rmin after aqueous sodium persulfate solution and vitamin C mixing-1Stir 2min.Inside finally obtained graphene aerogel
Structure is inhomogenous, and defect is more.
Comparative example 3
The type of material therefor and technological process are with embodiment 3, the difference is that by graphene oxide water solution, dodecyl
200rmin after aqueous sodium persulfate solution and vitamin C mixing-1Graphene hydrogel is directly reduced to after stirring at low speed 2min.Most
The material obtained eventually is substantially without abscess.
Comparative example 4
The type of material therefor and technological process are with embodiment 3, the difference is that the temperature of freezing environment is -190 DEG C, finally
Obtained graphene aerogel hole caves in, and cannot keep the original form of hydrogel.
As seen from Figure 1 by graphene oxide, body after lauryl sodium sulfate aqueous solution and vitamin C are mixed
Product is increased by about one time, and the increase of its volume is because SDS stirrings, which are added, forms bubble, these bubbles are subsequent graphite
The formation of alkene aeroge provides template.As can see from Figure 2 with the increase of graphene oxide concentration, the thickness of graphene wall
Degree increases, and hole is more uniform, and shows honeycomb structure, and the formation to demonstrate cavernous structure has benefited from SDS foaming.Figure
3 be the cross-sectional view of the graphene aerogel formed in embodiment 4 and comparative example 1, it can be seen that the present invention foams to be formed with SDS
Abscess is the graphene aerogel of template, and abscess is circle, and average diameter is 250 μm, and does not add SDS, using ice crystal as template
The abscess of graphene aerogel is ellipse, and its major diameter is 800 μm or so, and 200 μm or so of minor axis diameter, aperture is bright
It is aobvious larger.This is because SDS, which foams, shows circle, and graphite aeroge cellular structure prepared by existing constant pressure and dry technology
It is limited to the form and dimension of the ice as template, and the dosage of SDS and the rate of stirring are depended on the size of SDS foaming,
Therefore the abscess-size of the made graphene aerogel of the present invention is more easy to control.Made graphene gas of the invention as can be seen from Figure 4
The vertical section of gel still shows round blister, and the vertical section of graphene aerogel prepared by existing constant pressure and dry technology is in
Reveal longitudinal orderly channel design.And it can be seen that the cell wall of the made graphene aerogel of the present invention is thinner by comparison,
Between 100-160nm, slim and graceful transparence is presented.It can see from being compressed in Fig. 5 in front and back photo, the made graphite of the present invention
Deformation can restore after the compression ratio of alkene aeroge reaches 95% and compresses, and illustrate it with good compression resilience.
Claims (8)
1. a kind of preparation method of isotropism super-elasticity graphene aerogel, this method be using graphene oxide as raw material, and
It is prepared as template using the abscess that lauryl sodium sulfate aqueous solution stirring generates；It is characterized in that this method is depositing in reducing agent
Under, after graphene oxide aqueous dispersions are mixed with lauryl sodium sulfate aqueous solution stirring at low speed, then high-speed stirred foaming,
Then graphene oxide layer is restored to form tridimensional network, then freezes reinforcing graphene sheet layer and is formed by hole wall, most
Normal heating is dried afterwards, obtains isotropic graphene aerogel；
The cryogenic temperature that freezing is strengthened is -20 to -10 DEG C, and the temperature of normal heating drying is 30-70 DEG C, and the dry time is
12-48h；Temperature by graphene oxide layer reduction is 60-80 DEG C；
The compression ratio of made graphene aerogel reaches 95% or more；The size in its aperture is 100-500 μm；Wall thickness is 100nm-
160nm；
Made graphene aerogel pore size can pass through stir speed (S.S.), graphene oxide moisture liquid concentration and cryogenic temperature control
System；The thickness of cell wall can be regulated and controled by changing the concentration of graphene oxide aqueous dispersions.
2. a kind of preparation method of graphene aerogel as described in claim 1, it is characterised in that this approach includes the following steps：
1) graphene oxide aqueous dispersions are prepared；
2) reducing agent, lauryl sodium sulfate aqueous solution and graphene oxide aqueous dispersions stirring at low speed are uniformly mixed；Later
High-speed stirred is to foam；
3) the made mixed liquor of step 2) is heated, forms gel；
4) it will be freezed after the made gel cooling of step 3)；
5) will graphene hydrogel in step 4) melt after clean, normal heating drying is to get to isotropic super-elasticity
Graphene aerogel.
3. preparation method according to claim 2, it is characterised in that：The rate and high-speed stirred rate of stirring at low speed be respectively
60-300r·min-1And 500-3000rmin-1, mixing time is respectively 3-15min and 1-10min.
4. preparation method according to claim 2, it is characterised in that：The graphene oxide can be used Brodie methods,
It is prepared by the Hummer of Staudenmaier methods, Hummer, s methods and improvement, s methods.
5. preparation method according to claim 2, it is characterised in that：A concentration of 2-10mgml of graphene aqueous dispersions used-1。
6. preparation method according to claim 2, it is characterised in that：The temperature that step 3 is thermally formed gel is 60-75 DEG C, is added
The hot time is 30-360min, and the time that step 4 freezes is 3-12h.
7. preparation method according to claim 2, it is characterised in that：Reducing agent used is in vitamin C, hydrogen iodide and hydrazine hydrate
One or several kinds.
8. preparation method according to claim 2, it is characterised in that：Solvent used is in ethyl alcohol, methanol and acetone when cleaning
One kind.
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| CN102659099B (en) * | 2012-05-29 | 2015-04-08 | 上海二工大资产经营有限公司 | Preparation method of anisotropic graphene foam |
| CN104495820A (en) * | 2014-12-17 | 2015-04-08 | 北京化工大学 | Porous graphene aerogel and preparation method thereof |
| CN105384165B (en) * | 2015-12-18 | 2017-05-10 | 首都师范大学 | Spongy-like lightweight graphene aerogel preparation method |
| CN105600777B (en) * | 2016-01-29 | 2017-07-28 | 北京理工大学 | A kind of preparation method of the three-dimensional graphene foam of polystyrene modification |
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