CN106517171A - Preparation method of graphene aerogel - Google Patents
Preparation method of graphene aerogel Download PDFInfo
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- CN106517171A CN106517171A CN201510573962.0A CN201510573962A CN106517171A CN 106517171 A CN106517171 A CN 106517171A CN 201510573962 A CN201510573962 A CN 201510573962A CN 106517171 A CN106517171 A CN 106517171A
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Abstract
The invention provides a preparation method of a graphene aerogel. The preparation method comprises the following steps that S1, graphene and amido polymers are added into solvents and dispersed, so that graphene dispersion liquid is obtained; and S2, the graphene dispersion liquid is frozen and dried, so that the graphene aerogel is obtained. According to the preparation method of the graphene aerogel, the polymers containing amido serve as graphene dispersing agents and structural cross-linking agents, firstly strong interaction between the amido in the polymers and the graphene is utilized for dispersing graphene sheet layers in the solvents, and then the graphene dispersion liquid is directly frozen and dried, wherein the amido in the polymers is dried and cross-linked with the graphene sheet layers to form a structural framework, and accordingly the elastic graphene aerogel of a porous structure is prepared. According to the preparation method of the graphene aerogel, the graphene aerogel is directly prepared from graphene powder, process conditions are mild, the steps are simple, large-size graphene aerogel blocks can be produced in a large scale, and the obtained aerogel is good in adsorption characteristic and pressure resistance.
Description
Technical field
The invention belongs to nano-carbon material preparing technical field, is related to a kind of preparation method of graphene aerogel.
Background technology
Graphene aerogel is the porous blocks material being interconnected to form on three dimensions by graphene nanometer sheet.Graphene gas
Gel has the little (1-50mg/cm of density3), porosity height (＞ 50%), the big (100-1200m of specific surface area2/ g), mechanics
Performance is good, flexible, electric conductivity is good, stable chemical nature the features such as, can be used as clean energy resource storage (such as hydrogen, natural
Gas) dielectric material and power storage (such as ultracapacitor) electrode material, in heterogeneous catalysiss, sewage disposal and sensor
Also there is important application prospect in field.
For obtaining the block materials with loose structure, Graphene is prepared by freeze-drying process Graphene hydrogel typically at present
Aeroge.And Graphene cannot realize uniform and stable dispersion in water, it is difficult to directly prepare Graphene water from graphene powder
Gel.Therefore, the method for report is all to prepare Graphene hydrogel from graphene oxide Jing self assemblies and reduction at present, so
Lyophilization obtains graphene aerogel afterwards.The method of reduction is generally electronation or hydrothermal reduction two ways.For example, open
Learn and propose in graphene oxide dispersion in " a kind of graphene aerogel and preparation method thereof " (201010263656.4) on an equal basis
Middle addition reducing agent obtains Graphene hydrogel, then the freeze-dried method for preparing graphene aerogel, but reduction process
Need to introduce the poisonous reducing agents such as hydrazine hydrate, there is potential safety hazard, be unfavorable for the large-scale production of graphene aerogel.Gao Hui etc.
One is proposed in patent " a kind of preparation method with high adsorption three-dimensional self assembly Graphene " (201310110754.8)
Redox graphene lamella obtains Graphene hydrogel simultaneously to plant hydro-thermal method self assembly, then lyophilization Graphene hydrogel system
The method of standby graphene aerogel, hydrothermal reduction avoid the use of poisonous reducing agent, but hydro-thermal needs to enter in closed vessel
OK, it is unfavorable for large scale and prepare with scale graphene aerogel.
Therefore, develop a kind of technology of suitable prepare with scale graphene aerogel to be beneficial to promote graphene aerogel material to exist
The field such as the energy and environmental protection is promoted the use of.
The content of the invention
The shortcoming of prior art in view of the above, it is an object of the invention to provide a kind of preparation method of graphene aerogel,
For solving the problems, such as that graphene aerogel preparation method of the prior art is not suitable for large-scale production.
For achieving the above object and other related purposes, the present invention provides a kind of preparation method of graphene aerogel, including following
Step：
S1：Graphene and amine based polymer is added in a solvent, and is disperseed, obtain graphene dispersing solution；
S2：Graphene dispersing solution described in lyophilization, obtains graphene aerogel.
As a kind of preferred version of the preparation method of the graphene aerogel of the present invention, in step S1, the Graphene
The one kind or many in method, liquid phase stripping method, arc process, high temperature pyrolytic cracking (HTP) and chemical vapour deposition technique is aoxidized-is restored selected from employing
Plant the graphene powder for preparing.
As a kind of preferred version of the preparation method of the graphene aerogel of the present invention, in step S1, the amido gathers
One or more in shitosan, polyacrylamide, Polyetherimide and polyaniline of compound.
As a kind of preferred version of the preparation method of the graphene aerogel of the present invention, in step S1, the solvent choosing
One or more from water, ethanol, isopropanol, N-Methyl pyrrolidone and N,N-dimethylformamide.
As a kind of preferred version of the preparation method of the graphene aerogel of the present invention, in step S1, the Graphene,
Amine based polymer is 1 with the mass ratio of solvent:0.1～2:5～100.
Used as a kind of preferred version of the preparation method of the graphene aerogel of the present invention, in step S1, the dispersion is adopted
With one or more in ultrasound, stirring and shearing.
As a kind of preferred version of the preparation method of the graphene aerogel of the present invention, in step S2, the freezing is dry
Dry temperature range is -50～0 DEG C, and vacuum ranges are 1.3～13Pa, and sublimation drying scope is 1～100h.
As a kind of preferred version of the preparation method of the graphene aerogel of the present invention, in step S1, the Graphene
Including single or multiple lift Graphene.
As described above, the preparation method of the graphene aerogel of the present invention, has the advantages that：The Graphene gas of the present invention
Gel process for preparing using the polymer of amino-contained as graphene dispersion agent and structure cross-linking agent, first with the amido in polymer
The graphene sheet layer in strong interaction dispersion solvent between Graphene, then directly freezed be dried graphene dispersing solution, its
In, cross-linked graphene lamella forms structural framework to the amido in polymer after the drying, so as to prepare with loose structure
Elastic graphite alkene aeroge.The graphene aerogel preparation method of the present invention introduces amino-contained polymer simultaneously as dispersant and knot
Structure cross-linking agent, directly prepares graphene aerogel from graphene powder, and process conditions are gentle, step is simple, can scale
Production big size graphene aerogel block body, gained aeroge have good characterization of adsorption and pressure drag performance, are expected at water pollution
Applied in the field such as reason and pressure drag sensing.
Description of the drawings
Fig. 1 is shown as the process chart of the preparation method of the graphene aerogel of the present invention.
Fig. 2 is shown as the preparation method of the graphene aerogel of the present invention and prepares gained graphene aerogel in embodiment one
SEM schemes.
Fig. 3 is shown as the pressure that the preparation method of the graphene aerogel of the present invention prepares gained graphene aerogel in embodiment one
Resistance characteristic curve.
Fig. 4 is shown as the preparation method of the graphene aerogel of the present invention and prepares gained graphene aerogel in embodiment one to not
With the adsorbance cartogram of solvent.
Specific embodiment
Embodiments of the present invention are illustrated below by way of specific instantiation, those skilled in the art can be by disclosed by this specification
Content understand easily the present invention other advantages and effect.The present invention can also be added by specific embodiments different in addition
To implement or apply, the every details in this specification can also be based on different viewpoints and application, in the essence without departing from the present invention
Various modifications and changes are carried out under god.
Refer to Fig. 1 to Fig. 4.It should be noted that the diagram provided in the present embodiment only illustrates the present invention in a schematic way
Basic conception, only shown in schema with relevant component in the present invention rather than according to component count during actual enforcement, shape then
And size is drawn, which is actual when the implementing kenel of each component, quantity and ratio can be a kind of random change, and its assembly layout
Kenel is likely to increasingly complex.
The present invention provides a kind of preparation method of graphene aerogel, comprises the following steps：
S1：Graphene and amine based polymer is added in a solvent, and is disperseed, obtain graphene dispersing solution；
S2：Graphene dispersing solution described in lyophilization, obtains graphene aerogel.
Specifically, in step S1, the Graphene selected from employing aoxidize-restore method, liquid phase stripping method, arc process,
The graphene powder that one or more in high temperature pyrolytic cracking (HTP) and chemical vapour deposition technique is prepared.The Graphene includes monolayer
Or multi-layer graphene.
Aoxidize-method of restoring prepares Graphene is with native graphite as raw material, using oxidation reaction (on graphite linings edge carbons
Introduce and contain the oxy radicals such as epoxy and carbonyl containing carboxyl and hydroxyl, interlayer) weaken graphite layers interaction so as to spacing
Increase, is then peeled off graphite oxide and obtains graphene oxide；Then graphene oxide is disperseed (by high speed centrifugation, ultrasound etc.)
Formed in water or organic solvent and stablize homogeneous colloidal sol, reduced with reducing agent according still further to certain proportion, obtain monolayer or multilamellar
Graphene.The reduction such as very widely used today hydrazine hydrate, ethylenediamine is reasonable method of reducing, but these reducing agents have
Toxicity, brings many negative effects to environment and the mankind.Therefore, more researchers start with environmentally friendly as anti-bad
The reducing agents such as hematic acid, sodium citrate, reduction acidic amino acid carry out redox graphene.Additionally, some highly acid materials are also opened
Beginning is used by people to redox graphene and prepares graphite ene product, so that increasing Graphene characteristic is represented.Oxygen
It is that the Graphene for preparing has certain defect to change the maximum shortcoming of reducing process, because the graphite oxide obtained through strong oxidizer oxidation
Alkene, might not be completely reduced, and may lose a part of performance, such as light transmission, heat conductivity, especially electric conductivity,
So there is imperfection to a certain extent in the Graphene obtained after some reducing agent reduction, i.e., with proper Graphene
There is difference.But oxide-reduction method is cheap, substantial amounts of Graphene can be prepared, so becoming current the most frequently used preparation
The method of Graphene.
Liquid phase stripping method prepares Graphene and is typically directly graphite or expanded graphite (EG) (general by being rapidly heated to 1000 DEG C
Above Surface oxygen-containing groups are removed to obtain) it is added in certain organic solvent or water, by the effect of ultrasound wave, heating or air-flow
Prepare certain density single or multiple lift graphene solution.
It is, using graphite rod as negative and positive the two poles of the earth, to carry out arc discharge under high current and hydrogeneous atmosphere that arc process prepares Graphene,
In arc discharge process, continuous consumable anode graphite rod is obtained the Graphene of single or multiple lift in reaction chamber wall region.Electricity
Arc method is a kind of typical method for being applied to prepare CNT and fullerene earliest, the Graphene graphite prepared using arc process
Layer rule, crystal formation preferably, are expected to obtain higher electric conductivity and preferable chemical property.
It is carborundum high temperature thermal decomposition method that high temperature pyrolytic cracking (HTP) prepares the most frequently used one kind of Graphene, the method utilize between C, Si compared with
High saturated vapor pressure reduction, heats SiC crystal at high temperature, makes Si atoms depart from SiC crystal, and remaining C is spontaneously heavy
Combination nova forms Graphene.The advantage of this method is that Graphene can be grown directly upon on semi-insulated substrate, need not carry out turning
Shifting can directly carry out device preparation.
Chemical vapour deposition technique grows stone by the use of carbon compounds such as methane as carbon source by its pyrolytic in matrix surface
Black alkene.Two kinds are can be largely classified into from growth mechanism：(1) carburizing analysis carbon mechanism：For the gold with higher molten carbon amounts such as nickel
Category matrix, the carbon atom that carbon source cracking is produced separate out nucleation in high temperature in penetrating into metallic matrix, in cooling again from inside which,
And then grow into Graphene；(2) superficial growth mechanism：For the metallic matrix with relatively low molten carbon amounts such as copper, gaseous state under high temperature
The carbon atom that carbon source is cracked to form is adsorbed in metal surface, and then nucleating growth into " Graphene island ", and passes through " Graphene island "
Two dimension merging of growing up obtain continuous graphene film.Due to CVD method simple, the gained Graphene matter for preparing Graphene
Amount is very high, is capable of achieving large area deposition, and is relatively easy to be transferred to use on various matrixes, therefore the method is widely used in system
Standby grapheme transistor and transparent conductive film, have been increasingly becoming the main method for preparing high-quality graphene at present.
Certainly in other embodiments, the Graphene may also be employed graphene powder prepared by other methods, herein should be inundue
Limit the scope of the invention.
Specifically, in step S1, the amine based polymer is selected from shitosan, polyacrylamide, Polyetherimide and gathers
One or more in aniline.The solvent is selected from water, ethanol, isopropanol, N-Methyl pyrrolidone and N, N- dimethyl formyl
One or more in amine.The mass ratio of the Graphene, amine based polymer and solvent is 1:0.1～2:5～100.
As shown in figure 1, being shown as the process chart of the preparation method of the graphene aerogel of the present invention.The dispersion can be adopted
One or more in ultrasound, stirring and shearing.Wherein, in ultrasonic disperse, supersonic frequency is 20-400kHz；Dispersed with stirring
In, mixing speed is 100-8000rpm；Shearing dispersion is referred to and allows graphene powder to move quickly through shearing machine stator with solvent
The effects such as the small space and mover between, Jing impacts, tear promote the mixing of amino polymer and graphene film interlayer, and beat
Graphene aggregate is opened, wherein, the rotating speed of shearing is in 100-18000rpm.
Due to having strong interaction between the amido in polymer and graphene sheet layer surface atom, in ultrasound, stirring or shearing
Under Deng operation, amine based polymer molecule can be penetrated between the graphene sheet layer of reunion, opened Graphene aggregate, and adsorbed
In graphene film layer surface so that cannot reunite again between graphene sheet layer, so as to stablize dispersion of the Graphene in coordinative solvent,
The amine based polymer can be effectively in dispersion solvent graphene sheet layer.
Also known as sublimation drying, material first can be freezed in refrigerating plant, then is vacuum dried for lyophilization, also can directly dry
Dry indoor Jing is evacuated rapidly and freezes, and the heat of vaporization needed for sublimation process is typically supplied with heat radiation.
Specifically, in step S2, the cryodesiccated temperature range is -50～0 DEG C, and vacuum ranges are 1.3～13Pa,
Sublimation drying scope is 1～100h.In freezing dry process, the amine based polymer is crosslinked stone again as structure cross-linking agent
Black alkene lamella forms structural framework, after lyophilization Preset Time, you can obtain the elastic graphite alkene aeroge with loose structure.
The graphene aerogel preparation method of the present invention is using the polymer of amino-contained as graphene dispersion agent and structure cross-linking agent, first
First with the graphene sheet layer in the strong interaction dispersion solvent between the amido and Graphene in polymer, then directly freezed
Graphene dispersing solution is dried, wherein, cross-linked graphene lamella forms structural framework to the amido in polymer after the drying, so as to make
It is standby to obtain the elastic graphite alkene aeroge with loose structure.The present invention directly prepares graphene aerogel from graphene powder,
Process conditions are gentle, step is simple, and be produced on a large scale big size graphene aerogel block body.
Technical scheme is described in detail below by specific embodiment.
Embodiment one
100mg is added into 100mL deionized waters by aoxidizing-restoring the graphene powder of method acquisition with 25mg shitosans
In, graphene powder is fully dispersed in water by ultrasound, forms stable dispersion liquid.Take above-mentioned dispersion liquid and add container
In, at -30 DEG C, lyophilization 24h under the conditions of 1.5Pa obtains graphene aerogel block.Fig. 2,3,4 are respectively gained
The SEM pictures of graphene aerogel, piezoresistive characteristic curve and the adsorbance cartogram to different solvents.Can see, obtain
Graphene aerogel is the block materials of porous, with good pressure-sensitive character, and has very big suction to water and part organic solvent
Attached amount (30-60 times about conducted oneself with dignity), is expected to process material as voltage sensitive sensor and water pollution.
Embodiment two
500mg is added in 100mL deionized waters with 80mg polyanilines by the graphene powder that liquid phase stripping method is obtained,
Graphene powder is fully dispersed in water by ultrasound, forms stable dispersion liquid.Take in above-mentioned dispersion liquid addition container,
At -30 DEG C, lyophilization 36h under the conditions of 1.5Pa obtains graphene aerogel block.
Embodiment three
100mg is added in 100mL deionized waters with 50mg polyacrylamides by the graphene powder that arc process is obtained,
Graphene powder is fully dispersed in water by ultrasound, forms stable dispersion liquid.Take in above-mentioned dispersion liquid addition container,
At -40 DEG C, lyophilization 20h under the conditions of 2Pa obtains graphene aerogel block.
Example IV
100mg is added into 100mL deionized waters by the graphene powder that high temperature pyrolytic cracking (HTP) is obtained with 25mg Polyetherimide
In, and graphene powder is fully dispersed in water by ultrasound, form stable dispersion liquid.Take above-mentioned dispersion liquid and add and hold
In device, at -25 DEG C, lyophilization 48h under the conditions of 3Pa obtains graphene aerogel block.
In sum, graphene aerogel preparation method of the invention is using the polymer of amino-contained as graphene dispersion agent and structure
Cross-linking agent, first with the graphene sheet layer in the strong interaction dispersion solvent between the amido and Graphene in polymer, so
Directly freezed is dried graphene dispersing solution afterwards, and wherein, cross-linked graphene lamella forms structural bone to the amido in polymer after the drying
Frame, so that prepare the elastic graphite alkene aeroge with loose structure.The graphene aerogel preparation method of the present invention is introduced
Amino-contained polymer directly prepares graphene aerogel, work from graphene powder simultaneously as dispersant and structure cross-linking agent
Skill mild condition, step are simple, and be produced on a large scale big size graphene aerogel block body, and gained aeroge has absorption well
Characteristic and pressure drag performance, are expected to be applied in the field such as water pollution process and pressure drag sensing.So, the present invention effectively overcomes
Various shortcoming of the prior art and have high industrial utilization.
The principle and its effect of above-described embodiment only illustrative present invention, it is of the invention not for limiting.It is any to be familiar with this skill
The personage of art all can carry out modifications and changes to above-described embodiment under the spirit and the scope without prejudice to the present invention.Therefore, such as
Those of ordinary skill in the art completed under without departing from disclosed spirit and technological thought all etc.
Effect modifications and changes, should be covered by the claim of the present invention.
Claims (8)
1. a kind of preparation method of graphene aerogel, it is characterised in that comprise the following steps：
S1：Graphene and amine based polymer is added in a solvent, and is disperseed, obtain graphene dispersing solution；
S2：Graphene dispersing solution described in lyophilization, obtains graphene aerogel.
2. the preparation method of graphene aerogel according to claim 1, it is characterised in that：It is in step S1, described
Graphene is aoxidized-is restored in method, liquid phase stripping method, arc process, high temperature pyrolytic cracking (HTP) and chemical vapour deposition technique selected from employing
The graphene powder for preparing for one or more.
3. the preparation method of graphene aerogel according to claim 1, it is characterised in that：It is in step S1, described
One or more in shitosan, polyacrylamide, Polyetherimide and polyaniline of amine based polymer.
4. the preparation method of graphene aerogel according to claim 1, it is characterised in that：It is in step S1, described
One or more in water, ethanol, isopropanol, N-Methyl pyrrolidone and N,N-dimethylformamide of solvent.
5. the preparation method of graphene aerogel according to claim 1, it is characterised in that：It is in step S1, described
The mass ratio of Graphene, amine based polymer and solvent is 1:0.1～2:5～100.
6. the preparation method of graphene aerogel according to claim 1, it is characterised in that：It is in step S1, described
Dispersion is using one or more in ultrasound, stirring and shearing.
7. the preparation method of graphene aerogel according to claim 1, it is characterised in that：It is in step S2, described
Cryodesiccated temperature range is -50～0 DEG C, and vacuum ranges are 1.3～13Pa, and sublimation drying scope is 1～100h.
8. the preparation method of graphene aerogel according to claim 1, it is characterised in that：It is in step S1, described
Graphene includes single or multiple lift Graphene.
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| CN106947198A (en) * | 2017-04-17 | 2017-07-14 | 中国工程物理研究院核物理与化学研究所 | A kind of aerogel material and preparation method thereof |
| CN107051404A (en) * | 2017-04-07 | 2017-08-18 | 南京信息工程大学 | A kind of hydrophobic adsorbent based on graphene oxide |
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| CN107051404A (en) * | 2017-04-07 | 2017-08-18 | 南京信息工程大学 | A kind of hydrophobic adsorbent based on graphene oxide |
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| CN109502581A (en) * | 2018-12-13 | 2019-03-22 | 浙江农林大学 | A kind of preparation method and applications of graphene-based aeroge |
| CN109817992A (en) * | 2019-01-12 | 2019-05-28 | 袁玲燕 | A kind of preparation method of the dedicated redox elctro-catalyst of magnesium air fuel cell |
| CN109925981A (en) * | 2019-03-13 | 2019-06-25 | 太原理工大学 | A kind of preparation method of the graphene composite aerogel of high compression-strength |
| CN111187506A (en) * | 2020-01-15 | 2020-05-22 | 青岛科技大学 | Method for preparing composite material from graphene nano paste |
| CN111187506B (en) * | 2020-01-15 | 2021-12-28 | 青岛科技大学 | Method for preparing composite material from graphene nano paste |
| CN111268669A (en) * | 2020-01-20 | 2020-06-12 | 洛阳理工学院 | Preparation method of graphene/silver nanowire composite aerogel |
| CN111285358A (en) * | 2020-02-10 | 2020-06-16 | 洪永建 | Preparation method and application of modified graphene aerogel |
| CN111346577A (en) * | 2020-03-30 | 2020-06-30 | 浙江晶鑫特种纸业有限公司 | Preparation method and application of high-elasticity layered graphene oxide composite aerogel |
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| CN115724642B (en) * | 2022-11-04 | 2023-11-21 | 西北工业大学 | Preparation method of nanometer covalent-connection graphene prefabricated body with improved compressive strength |
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