CN104401979A - Phase-transfer preparation method of graphene-based composite aerogel - Google Patents
Phase-transfer preparation method of graphene-based composite aerogel Download PDFInfo
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Abstract
The invention discloses a phase-transfer preparation method of graphene-based composite aerogel. The phase-transfer preparation method comprises the following steps of dispersing graphene oxide in an alkaline or neutral aqueous solution to obtain a stable graphene oxide dispersion liquid, dispersing a low-dimensional nanomaterial in a surfactant-containing aqueous solution to obtain a stable low-dimensional nanomaterial dispersion liquid, mixing the graphene oxide dispersion liquid and the low-dimensional nanomaterial dispersion liquid to obtain a uniform mixed solution, carrying out phase-transferring to obtain a stable graphene-low dimensional nanomaterial dispersion liquid, carrying out hydro-thermal treatment to obtain the graphene-based composite aerogel, and carrying out drying treatment on the graphene-based composite aerogel to obtain a desired product. The phase-transfer preparation method has the advantages of simple and controllable processes, environmental friendliness, low cost and large-scale production feasibility. The graphene-based composite aerogel has a novel structure and good mechanical and electrical properties and can be used as an electrode material such as a supercapacitor electrode material or an organic fuel adsorbent.
Description
Technical field
The present invention relates to a kind of graphene-based aerogel, be specifically related to a kind of preparation method of graphene-based composite aerogel, belong to nano-porous materials technical field.
Background technology
At present, the research of graphene-based aerogel composite receives much concern.Graphene-based aerogel composite is compared to simple graphene aerogel, it not only possesses the feature such as high connductivity, high-specific surface area, low density of graphene aerogel, on the other hand, graphene-based aerogel composite also shows out the performance of guest materials, Graphene can with the compounds such as the nanometer sheet of the nano wire of the nano particle of zero dimension, one dimension and two dimension, form graphene-based aerogel composite, the kind of these guest materialss relates to the materials such as metal, metal oxide, inorganics and polymer.The method of the graphene-based composite aerogel of current preparation mainly contains in situ synthesis and mechanically mixing two kinds of methods.In situ synthesis is through pyroprocess by the presoma mixed solution of Graphene and low-dimension nano material, on graphene sheet layer, growth in situ goes out low-dimension nano material, although the method is easier, but this process is difficult to realize control to low-dimension nano material size in composite aerogel, be difficult to obtain that latitude is homogeneous, the nano material of size uniformity; Mechanical mixing can well control the homogeneity of object nano material latitude and size, but used object nano material must stablize to suppress its agglomeration by certain tensio-active agent, remain tensio-active agent in the graphene-based composite Nano aerogel that the method obtains, be difficult to the characteristics and advantages giving full play of low-dimension nano material itself.
In view of the deficiency in above graphene-based composite aerogel preparation method, industry, in the urgent need to developing a kind of homogeneity that can control object nano material size and dimension in Graphene composite aerogel very well, well can play again the method for object low-dimension nano material self character to prepare graphene-based composite aerogel.
Summary of the invention
For deficiency of the prior art, main purpose of the present invention is the phase transition preparation method providing a kind of graphene-based composite aerogel, the graphene-based composite aerogel utilizing the method to obtain can either keep the original feature structure of Graphene, be endowed again new diversification performance, have the performances such as excellent conduction, heat conduction concurrently.
For realizing aforementioned invention object, the technical solution used in the present invention comprises:
A phase transition preparation method for graphene-based composite aerogel, comprises the steps:
Can the stable existence graphene oxide solution of more than 1 day with can the low-dimension nano material dispersion liquid of stable existence more than 1 day mix, through phase transition behavior, obtain the stable dispersions of Graphene and low-dimension nano material;
The stable dispersions of described Graphene and low-dimension nano material is carried out hydrothermal treatment consists, obtains graphene-based composite aquogel;
And, drying treatment is carried out to obtained graphene-based composite aquogel, obtains described graphene-based composite aerogel.
Further, the aperture of described graphene-based composite aerogel is 1nm ~ 4 μm, porosity 75.0-99.5%, and density is 0.02-0.5g/cm
3, specific surface area is 100-900m
2/ g, specific conductivity is 0.1 ~ 100 S/m.
Compared with prior art, advantage of the present invention comprises:
(1) the present invention obtain aerogel and not only achieve the homogeneous compound of Graphene and low-dimension nano material size uniformity, dimension, aerogel has good mechanical property, and avoid the parcel of other tensio-active agents on low-dimension nano material surface, give full play to low-dimension nano material and the special advantage of Graphene itself.
(2) simple, the environmental protection of aerogel preparation technology of the present invention, scale operation is suitable for.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, the accompanying drawing that the following describes is only some embodiments recorded in the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the electron scanning micrograph of graphene-polypyrrole nano-particles reinforcement aerogel in embodiment 1;
Fig. 2 is the electron scanning micrograph of Graphene in embodiment 2-nano silver wire composite aerogel;
Fig. 3 is the electron scanning micrograph of embodiment 3 China and Mexico alkene-tungsten oxide nano composite aerogel;
Fig. 4 is the electron scanning micrograph of embodiment 4 China and Mexico alkene-molybdenum disulfide nano sheet composite aerogel.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be described in detail the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under the prerequisite not making creative work, all belongs to the scope of protection of the invention.
As previously mentioned, in view of existing graphene-based composite aerogel class material is in performance, the equal Shortcomings in the aspects such as preparation technology, inventor is through studying for a long period of time and putting into practice in a large number, technical scheme of the present invention is proposed, its mainly with graphene oxide and low-dimension nano material for initial reactant, particularly mix using graphene oxide as a kind of tensio-active agent with the nano material homogeneous phase of low-dimensional, by stirring, ultrasonic disperse, phase transition, be by the stable solution of graphene oxide by the low-dimension nano material solution transition by surfactants stabilize, Graphene-low-dimension nano material the composite aerogel with three-dimensional structure form is obtained again through the simple operations such as hydrothermal treatment consists and supercritical drying.
Further say, the phase transition preparation method of a kind of graphene-based composite aerogel provided by the invention comprises:
Can the stable existence graphene oxide solution of more than 1 day with can the low-dimension nano material dispersion liquid of stable existence more than 1 day mix, through phase transition behavior, obtain the stable dispersions of Graphene and low-dimension nano material;
The stable dispersions of described Graphene and low-dimension nano material is carried out hydrothermal treatment consists, obtains graphene-based composite aquogel;
And, drying treatment is carried out to obtained graphene-based composite aquogel, obtains described graphene-based composite aerogel.
Further, the phase transition preparation method of described graphene-based composite aerogel comprises: be scattered in by graphene oxide in alkalescence or neutral aqueous solution, forms described graphene oxide dispersion.
Further, the phase transition preparation method of described graphene-based composite aerogel comprises: be scattered in by low-dimension nano material in the aqueous solution containing tensio-active agent, forms low-dimension nano material dispersion liquid.
Comparatively preferred, the concentration of described graphene oxide dispersion is 0.4mg/mL ~ 15mg/mL.
Aforementioned oxidation Graphene can by the suitable method known to industry, such as Hummers chemical method preparation.
Comparatively preferred, it is 10 that described alkaline aqueous solution comprises concentration
-4the alkaline matter of ~ 1.0 mol/L.
Wherein, described alkaline matter can be selected from but be not limited to potassium hydroxide or sodium hydroxide.
Comparatively preferred, the concentration of described low-dimension nano material dispersion liquid is 1mg/mL ~ 50mg/mL.
Comparatively preferred, be the tensio-active agent of 1 mg/mL ~ 100mg/mL containing concentration in described low-dimension nano material dispersion liquid.
Wherein, described tensio-active agent is at least selected from polyvinylpyrrolidone, cetyl trimethylammonium bromide, any one in Sodium dodecylbenzene sulfonate, brocide, ammonium lauryl sulfate, but is not limited thereto.
Among a comparatively preferred embodiment, step (3) comprising:
In room temperature environment, described graphene oxide solution is mixed with described low-dimension nano material dispersion liquid, and through stirring and/or ultrasonic disperse, then through phase transition behavior, obtain the stable dispersions of Graphene and low-dimension nano material.
Particularly preferred, the operational condition of aforementioned stirring comprises: stir 1min ~ 900min with the speed of 10 ~ 10000 revs/min.
Wherein, the mode of stirring can be machinery, magnetic agitation etc.
Particularly preferred, the condition of aforementioned ultrasonic dispersion comprises: ultrasonic time is 0.5min ~ 200min, and ultrasonic power is 50 ~ 1000W, and ultrasonic frequency is 50 ~ 100KHz.
Among a comparatively preferred embodiment, in the stable dispersions of described Graphene and low-dimension nano material, the mass ratio of contained graphene oxide and low-dimension nano material is 100:1 ~ 1:100.
Among a comparatively preferred embodiment, in step (3), phase transition behavior is washing centrifugal process, and wherein, washing centrifugal number of times is 1 ~ 50 time, and centrifugal rotational speed is 1000 ~ 10000 revs/min.
Among a comparatively preferred embodiment, hydrothermal treatment consists temperature described in step (4) is 80 DEG C ~ 180 DEG C, and the time is 5 ~ 96h.
Among a comparatively preferred embodiment, the drying mode adopted in step (5) comprises lyophilize or supercritical drying.
More preferred, the condition of foregoing freeze drying comprises: freezing temp is-20 DEG C ~-170 DEG C, and drying temperature is 0 DEG C ~ 80 DEG C, and vacuum tightness is 100 ~ 60000Pa, and time of drying is 2 ~ 48h.
More preferred, aforementioned supercritical drying comprises:
Adopt small molecular alcohol or small molecules ketone to replace the aqueous solvent existed in described graphene-based composite aquogel and soluble reaction thing, reaction product, obtain graphene-based compound alcogel or graphene-based compound ketone gel,
And, adopt Supercritical Ethanol or supercritical co to carry out drying to described graphene-based compound alcogel or graphene-based compound ketone gel, obtain described graphene-based composite aerogel.
Wherein, described small molecular alcohol can be selected but be not limited to ethanol.
Wherein, described small molecules ketone can be selected but be not limited to acetone.
Such as, in an exemplary embodiments, the phase transition preparation method of described graphene-based composite aerogel comprises the steps:
(1) be scattered in by graphene oxide in alkalescence or neutral aqueous solution, formation can stable existence more than 1 day, the graphene oxide dispersion of particularly 1 day ~ 300 days;
(2) be scattered in by low-dimension nano material in the surface-active aqueous solution, formation can stable existence more than 1 day, the dispersion liquid of particularly 1 day ~ 300 days;
(3) described graphene oxide solution is placed in room temperature environment, adds low-dimension nano material dispersion, mix, through phase transition behavior, obtain the stable dispersions of Graphene and low-dimension nano material;
(4) stable dispersions of Graphene and low-dimension nano material is carried out hydrothermal treatment consists, obtain graphene-based composite aquogel;
(5) obtained graphene-based composite aquogel is carried out lyophilize or supercritical drying, obtain described graphene-based composite aerogel.
Further, the aperture of the graphene-based composite aerogel utilizing preceding method to prepare is 1nm ~ 4 μm, porosity 75.0-99.5%, and density is 0.02-0.5g/cm
3, specific surface area is 100-900m
2/ g, specific conductivity is 0.1 ~ 100 S/m.
Graphene-based composite aerogel of the present invention can as electrode materials, the such as application such as electrode material for super capacitor or organic-fuel sorbent material.
Aerogel structure of the present invention is novel, has good mechanical, electric property etc., and preparation technology is simple, environmental protection, can be mass-produced.
Also technical scheme of the present invention is further described by reference to the accompanying drawings below by way of some embodiments.But selected embodiment only for illustration of the present invention, and does not limit and scope of the present invention.
embodiment 1:graphene oxide dispersion is configured to the solution of 8mg/mL, stirs 20 minutes, ultrasonic 30 minutes, obtain the graphene oxide solution that dispersion is homogeneous, this gets solution 10mL; The polyvinylpyrrolidonesolution solution of 4mg/mL polypyrrole nano particle, wherein the concentration of polyvinylpyrrolidone is 5mg/mL, getting this solution 10mL joins in above-mentioned graphene oxide solution, stir 30 minutes, ultrasonic 15 minutes again, obtain the graphene oxide-polypyrrole nano particle Homogeneous phase mixing liquid mixed; The dispersion liquid of the graphene oxide mixed obtained and polypyrrole nano particle is carried out phase transition (centrifugal washing 10 times, centrifugal rotational speed is 10000 revs/min), the dispersion liquid of graphene oxide phase transition completed-polypyrrole nano particle is transferred in tetrafluoroethylene reactor, carry out hydrothermal treatment consists and obtain graphene-polypyrrole nano-particles reinforcement hydrogel, the condition of hydro-thermal is 180 degree, 12h.The hydrogel obtained is obtained graphene-polypyrrole nano-particles reinforcement alcogel through alcohol solvent displacement, afterwards that graphene-polypyrrole nano-particles reinforcement alcogel is dry through supercritical co, obtain graphene-polypyrrole nano-particles reinforcement aerogel, be denoted as rGO-PPy.
The microtexture of graphene-polypyrrole nano-particles reinforcement aerogel (rGO-PPy) obtained in this embodiment is shown in Fig. 1.
The structure of graphene-polypyrrole nano-particles reinforcement aerogel (rGO-PPy) obtained in this embodiment and performance perameter are in table 1.
embodiment 2:graphene oxide dispersion is configured to the solution of 8mg/mL, stirs 20 minutes, ultrasonic 30 minutes, obtain the graphene oxide solution that dispersion is homogeneous, this gets solution 10mL; The polyvinylpyrrolidonesolution solution of 4mg/mL nano silver wire, wherein the concentration of polyvinylpyrrolidone is 5mg/mL, gets this solution 10mL and joins in above-mentioned graphene oxide solution, stirs 30 minutes, ultrasonic 15 minutes again, obtain the graphene oxide-nano silver wire Homogeneous phase mixing liquid mixed; The dispersion liquid of the graphene oxide mixed obtained and nano silver wire is carried out phase transition (centrifugal washing 10 times, centrifugal rotational speed is 10000 revs/min), the dispersion liquid of graphene oxide-nano silver wire phase transition completed is transferred in tetrafluoroethylene reactor, carry out hydrothermal treatment consists and obtain Graphene-nano silver wire composite aquogel, the condition of hydro-thermal is 180 degree, 12h.The hydrogel obtained is obtained Graphene-nano silver wire compound alcogel through alcohol solvent displacement, afterwards that Graphene-nano silver wire compound alcogel is dry through supercritical co, obtain Graphene-nano silver wire composite aerogel, be denoted as rGO-Ag NWs.
The microtexture of Graphene-nano silver wire composite aerogel (rGO-Ag NWs) obtained in this embodiment is shown in Fig. 2.
The structure of Graphene-nano silver wire composite aerogel (rGO-Ag NWs) obtained in this embodiment and performance perameter are in table 1.
embodiment 3:graphene oxide dispersion is configured to the solution of 8mg/mL, stirs 20 minutes, ultrasonic 30 minutes, obtain the graphene oxide solution that dispersion is homogeneous, this gets solution 10mL; The polyvinylpyrrolidonesolution solution of 4mg/mL tungsten oxide nano, wherein the concentration of polyvinylpyrrolidone is 5mg/mL, getting this solution 10mL joins in above-mentioned graphene oxide solution, stir 30 minutes, ultrasonic 15 minutes again, obtain the graphene oxide-tungsten oxide nano Homogeneous phase mixing liquid mixed; The dispersion liquid of the graphene oxide mixed obtained and tungsten oxide nano is carried out phase transition (centrifugal washing 10 times, centrifugal rotational speed is 10000 revs/min), the dispersion liquid of graphene oxide-tungsten oxide nano phase transition completed is transferred in tetrafluoroethylene reactor, carry out hydrothermal treatment consists and obtain Graphene-tungsten oxide nano composite aquogel, the condition of hydro-thermal is 180 degree, 12h.The hydrogel obtained is obtained Graphene-tungsten oxide nano compound alcogel through alcohol solvent displacement, afterwards that Graphene-tungsten oxide nano compound alcogel is dry through supercritical co, obtain Graphene-tungsten oxide nano composite aerogel, be denoted as rGO-W
18o
49.
Graphene-tungsten oxide nano composite aerogel (rGO-W obtained in this embodiment
18o
49) microtexture see Fig. 3.
Graphene-tungsten oxide nano composite aerogel (rGO-W obtained in this embodiment
18o
49) structure and performance perameter in table 1.
embodiment 4:graphene oxide dispersion is configured to the solution of 8mg/mL, stirs 20 minutes, ultrasonic 30 minutes, obtain the graphene oxide solution that dispersion is homogeneous, this gets solution 10mL; The polyvinylpyrrolidonesolution solution of 4mg/mL molybdenum disulfide nano sheet, wherein the concentration of polyvinylpyrrolidone is 5mg/mL, getting this solution 10mL joins in above-mentioned graphene oxide solution, stir 30 minutes, ultrasonic 15 minutes again, obtain the graphene oxide-molybdenum disulfide nano sheet Homogeneous phase mixing liquid mixed; The dispersion liquid of the graphene oxide mixed obtained and molybdenum disulfide nano sheet is carried out phase transition (centrifugal washing 10 times, centrifugal rotational speed is 10000 revs/min), the dispersion liquid of graphene oxide-molybdenum disulfide nano sheet phase transition completed is transferred in tetrafluoroethylene reactor, carry out hydrothermal treatment consists and obtain Graphene-molybdenum disulfide nano sheet composite aquogel, the condition of hydro-thermal is 180 degree, 12h.The hydrogel obtained is obtained Graphene-molybdenum disulfide nano sheet compound alcogel through alcohol solvent displacement, afterwards that Graphene-molybdenum disulfide nano sheet compound alcogel is dry through supercritical co, obtain Graphene-molybdenum disulfide nano sheet composite aerogel, be denoted as rGO-MoS
2.
Graphene-molybdenum disulfide nano sheet composite aerogel (rGO-MoS obtained in this embodiment
2) microtexture see Fig. 4.
Graphene-molybdenum disulfide nano sheet composite aerogel (rGO-MoS obtained in this embodiment
2) structure and performance perameter in table 1.
Summarize it, compared with existing Graphene composite aerogel preparation technology, avoid tensio-active agent carrys out stable low-dimension nano material to technique of the present invention on the one hand, it also avoid the uncontrollability of in situ synthesis side in dimension and size on the other hand, thus the distinctive performance of low-dimension nano material itself that can play greatly as object, the graphene-based composite aerogel obtained not only has the high-specific surface area of graphene aerogel, the characteristics such as excellent electroconductibility, and show low-dimension nano material diversification performance, further expand the range of application of graphene-based composite aerogel.
graphene-based composite aerogel structure and performance parameters in table 1. embodiment 1-4
It should be noted that, in this article, term " comprises ", " comprising " or its any other variant are intended to contain comprising of nonexcludability, thus make to comprise the process of a series of key element, method, article or equipment and not only comprise those key elements, but also comprise other key elements clearly do not listed, or also comprise by the intrinsic key element of this process, method, article or equipment.
Should be understood that; the above is only the specific embodiment of the present invention, for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (11)
1. a phase transition preparation method for graphene-based composite aerogel, is characterised in that and comprises the steps:
Can the stable existence graphene oxide solution of more than 1 day with can the low-dimension nano material dispersion liquid of stable existence more than 1 day mix, through phase transition behavior, obtain the stable dispersions of Graphene and low-dimension nano material;
The stable dispersions of described Graphene and low-dimension nano material is carried out hydrothermal treatment consists, obtains graphene-based composite aquogel;
And, drying treatment is carried out to obtained graphene-based composite aquogel, obtains described graphene-based composite aerogel.
2. the phase transition preparation method of graphene-based composite aerogel according to claim 1, be characterised in that and comprise: graphene oxide is scattered in alkalescence or neutral aqueous solution, form described graphene oxide dispersion, and the concentration of described graphene oxide dispersion is 0.4mg/mL ~ 15mg/mL.
3. the phase transition preparation method of graphene-based composite aerogel according to claim 2, being characterised in that described alkaline aqueous solution comprises concentration is 10
-4the alkaline matter of ~ 1.0 mol/L, described alkaline matter comprises potassium hydroxide or sodium hydroxide.
4. the phase transition preparation method of graphene-based composite aerogel according to claim 1, be characterised in that and comprise: low-dimension nano material is scattered in the aqueous solution containing tensio-active agent, form low-dimension nano material dispersion liquid, and the concentration of described low-dimension nano material dispersion liquid is 1mg/mL ~ 50mg/mL.
5. the phase transition preparation method of graphene-based composite aerogel according to claim 4, be characterised in that in described low-dimension nano material dispersion liquid containing the tensio-active agent that concentration is 1 mg/mL ~ 100mg/mL, described tensio-active agent is at least selected from polyvinylpyrrolidone, cetyl trimethylammonium bromide, any one in Sodium dodecylbenzene sulfonate, brocide, ammonium lauryl sulfate.
6. the phase transition preparation method of graphene-based composite aerogel according to claim 1, be characterised in that step (3) comprising: in room temperature environment, described graphene oxide solution is mixed with described low-dimension nano material dispersion liquid, and stir 1min ~ 900min and/or ultrasonic disperse 0.5min ~ 200min with the speed of 10 ~ 10000 revs/min, again through phase transition behavior, obtain the stable dispersions of Graphene and low-dimension nano material.
7. the phase transition preparation method of graphene-based composite aerogel according to claim 1 or 6, in the stable dispersions being characterised in that described Graphene and low-dimension nano material, the mass ratio of contained graphene oxide and low-dimension nano material is 100:1 ~ 1:100.
8. the phase transition preparation method of graphene-based composite aerogel according to claim 1, be characterised in that in step (3), phase transition behavior is washing centrifugal process, wherein, washing centrifugal number of times is 1 ~ 50 time, and centrifugal rotational speed is 1000 ~ 10000 revs/min.
9. the phase transition preparation method of graphene-based composite aerogel according to claim 1, be characterised in that hydrothermal treatment consists temperature described in step (4) is 80 DEG C ~ 180 DEG C, the time is 5 ~ 96h.
10. the phase transition preparation method of graphene-based composite aerogel according to claim 1, is characterised in that the drying mode adopted in step (5) comprises lyophilize or supercritical drying;
Wherein, cryodesiccated condition comprises: freezing temp is-20 DEG C ~-170 DEG C, and drying temperature is 0 DEG C ~ 80 DEG C, and vacuum tightness is 100 ~ 60000Pa, and time of drying is 2 ~ 48h;
Wherein, supercritical drying comprises:
Small molecular alcohol or small molecules ketone is adopted to replace the aqueous solvent existed in described graphene-based composite aquogel and soluble reaction thing, reaction product, obtain graphene-based compound alcogel or graphene-based compound ketone gel, described small molecular alcohol comprises ethanol, described small molecules ketone comprises acetone
And, adopt Supercritical Ethanol or supercritical co to carry out drying to described graphene-based compound alcogel or graphene-based compound ketone gel, obtain described graphene-based composite aerogel.
The 11. graphene-based composite aerogels that according to any one of claim 1-10 prepared by method, it is characterized in that the aperture of described graphene-based composite aerogel is 1nm ~ 4 μm, porosity 75.0-99.5%, density is 0.02-0.5g/cm
3, specific surface area is 100-900m
2/ g, specific conductivity is 0.1 ~ 100 S/m.
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