CN101948108A - Optimized preparation method of oxidized graphite paper - Google Patents
Optimized preparation method of oxidized graphite paper Download PDFInfo
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- CN101948108A CN101948108A CN 201010299108 CN201010299108A CN101948108A CN 101948108 A CN101948108 A CN 101948108A CN 201010299108 CN201010299108 CN 201010299108 CN 201010299108 A CN201010299108 A CN 201010299108A CN 101948108 A CN101948108 A CN 101948108A
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Abstract
The invention relates to an optimized preparation method of oxidized graphite paper, belonging to the technical field of nanomaterials. The preparation method comprises the following steps: preparing graphene oxide by adopting hydrogen peroxide; then, adding a glutaric dialdehyde solution into the suspension of the graphene oxide; and casting and drying on a substrate after stirring to obtain the oxidized graphite paper with enhanced mechanical properties. The method of the invention is simple and easy, is suitable for large-scale preparation, and can realize large-scale preparation of the oxidized graphite paper. By adding a small amount of cross-linking agent, the obtained oxidized graphite paper with enhanced mechanical properties has regular structure, uniform height and enough mechanical strength.
Description
Technical field
What the present invention relates to is a kind of method of technical field of nano material, specifically is a kind of optimization preparation method of graphite oxide paper.
Background technology
Graphene, as closely arranging the two-dimentional atomic crystal material that constitutes by the monolayer carbon atom, because its unique quantum effect and excellent electricity, calorifics and mechanical property, at the nanometer electronic device and the unicircuit in future, flexible electronic device, novel electron devices such as ultra-high sensitive senser element, matrix material, solar cell, super capacitor, aspects such as hydrogen storage material are with a wide range of applications.In graphene preparation method, chemical dispersion method prepares Graphene, with respect to physical method, because it has the productive rate height, and the simple and lower-cost advantage of preparation method, therefore, this method has become a hot topic of Graphene preparation.
Adopt chemical process with the flaky graphite oxidation, the graphite oxide that obtains can be in water and organic solvent homodisperse, further can prepare graphite oxide paper, at matrix material, aspects such as nanofiltration membrane, ultracapacitor, lithium cell are with a wide range of applications.People such as Rodney S Ruoff write articles the 448th volume 457～460 pages of the 26th phases on Nature, the graphite oxide paper that utilizes the method for filtration under diminished pressure to obtain having considerable intensity.In order further to improve the intensity of graphite oxide paper, people such as Rodney S Ruoff write articles 572～578 pages of the 2nd the 3rd phases of volume on ACS Nano, adopt divalent-metal ion to realize the mechanics of graphite oxide paper is strengthened.
Yet the graphite oxide paper that the method for employing filtration under diminished pressure obtains is not suitable for suitability for industrialized production, is necessary to seek simple method, realizes the mass preparation of graphite oxide paper.Although people such as Titelman GI the 43rd volume on Carbon is write articles for 641～649 pages, the graphene oxide dispersion liquid can become the graphite oxide film by dried coating film, and the preparation that complete big area self-supporting has the graphite oxide paper of considerable intensity does not simultaneously appear in the newspapers.
Summary of the invention
The present invention is directed to the prior art above shortcomings, a kind of optimization preparation method of graphite oxide paper is provided, adopt special base material, with graphite oxide dispersion liquid casting film-forming, can realize the mass preparation of graphite oxide paper, by adding a spot of linking agent, can realize that the mechanics of graphite oxide paper strengthens.This method is simple, is suitable for mass preparation, and can design the graphite oxide paper of different thickness, size and dimension as required, and resulting mechanics enhanced graphite oxide paper has compound with regular structure, highly even and enough physical strength.
The present invention is achieved by the following technical solutions, after the present invention adopts hydrogen peroxide to prepare graphene oxide, add glutaraldehyde solution in the suspension with graphene oxide, after stirring in substrate the curtain coating drying, obtain mechanical property enhanced graphite oxide paper.
Described graphene oxide prepares in the following manner: after frozen water and graphite suspension are carried out the quencher reaction, slowly add aqueous hydrogen peroxide solution and obtain glassy yellow graphene oxide suspension, obtain after filtration carrying out pickling and drying successively behind the tawny filter cake, obtain the graphene oxide solid.
The mass percent concentration of described hydrogen peroxide is 30%;
Described pickling and drying are meant: adopting mass percent is that 3% dilute hydrochloric acid repetitive scrubbing to filtrate does not have SO
4 2-Exist, and then be washed till filtrate with deionized water and do not have Cl
-Exist, 40 ℃ of vacuum-drying 24h in vacuum drying oven obtain the graphene oxide solid then.
Described graphite suspension prepares in the following manner: at room temperature graphite is joined in the vitriol oil, after stirring, add SODIUMNITRATE, carry out cooling process after fully stirring 1h, add potassium permanganate then in batches, be heated to 35 ± 3 ℃ with water-bath at last, fully react and add mixture of ice and water quencher reaction behind the 2h, obtain the brown graphite suspension.
Described graphite is natural flaky graphite of 200～500 purposes or expanded graphite;
The described vitriol oil is that mass percent concentration is 98% the vitriol oil;
Described cooling process is cooled to 0 ℃ or following for reaction vessel being placed ice bath or cryosel bathe;
The described potassium permanganate that in batches adds is meant that the potassium permanganate amount of each adding is 2g～3g, and the timed interval that at every turn adds potassium permanganate is 20min, so that the temperature of reaction system remains on below 15 ℃.
The suspension of described graphene oxide is meant: graphene oxide is scattered in the water, and its concentration is 0.1mg/mL～5mg/mL;
Described substrate is tetrafluoroethylene, polycarbonate, polyethylene, polypropylene, polyimide, steel plate, PET, polyaryletherketone, polyvinyl chloride, polyvinylidene difluoride (PVDF), urethane, poly(lactic acid), polystyrene, ABS resin, polyacrylonitrile, poly (arylene ether nitrile), polyethersulfone, polysiloxane, Mierocrystalline cellulose, rubber, Polyvinyl carbazole, mica, Resins, epoxy, resol, maleic resin or fluoro-resin;
Described curtain coating drying is meant: in temperature is 20 ℃～80 ℃ baking oven, and dry 6h～24h film forming.
The mass percentage concentration of described glutaraldehyde solution is 2%～100%;
The quality percentage composition of described glutaraldehyde is 0.1%～5%;
The described reaction times is 10min～2h.
Compared with prior art, the invention has the advantages that and adopt special substrate, realize the mass preparation of graphite oxide paper adopting glutaraldehyde as cross linker simultaneously, realize that the mechanics of graphite oxide paper strengthens by the method for casting film-forming.
Description of drawings
Fig. 1 is the inventive method synoptic diagram.
Fig. 2 is the graphite oxide synoptic diagram;
Wherein: Fig. 2 a is the graphite oxide atomic force micrograph, and Fig. 2 b is graphite oxide altitude distribution figure, and Fig. 2 c is the electron scanning micrograph of graphite oxide.
Fig. 3 is the sem photograph of graphite oxide paper cross section.
Fig. 4 is the stress-strain curve diagram of graphite oxide paper.
Embodiment
Below embodiments of the invention are elaborated, present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
As shown in Figure 1, the large-scale producing method of the described graphite oxide paper of present embodiment may further comprise the steps:
The first step, at room temperature joins the natural flaky graphite of 10g 500 purposes in the 1000mL flask, mechanical stirring evenly after, add the 5g SODIUMNITRATE, continue to stir 1h, ice bath is cooled to 0 ℃, then, in 5h, add 30g potassium permanganate in batches, keep temperature of reaction system not to be higher than 15 ℃, remove ice bath, temperature of reaction system is risen to 35 ± 3 ℃ with heating in water bath, fully stirring reaction is 2 hours, obtains the brown graphite suspension.
Second step, the frozen water of 500mL is added quencher reaction in the flask, slowly add mass percent concentration subsequently and be 30% aqueous hydrogen peroxide solution 35mL, obtain glassy yellow graphene oxide suspension.
The 3rd the step, with the graphite oxide suspension filtered, obtain the tawny filter cake.With mass percentage concentration is that the washing of 3% dilute hydrochloric acid solution does not have SO until filtrate
4 2-Till the existence, continue to wash with water, until the no Cl of filtrate
-Exist, resulting filter cake places 40 ℃ of vacuum-drying 24h of vacuum drying oven, obtains the graphene oxide solid.
The 4th goes on foot, graphene oxide is scattered in the water, forms the dispersion liquid of 0.5mg/mL, prolongs film forming at tetrafluoroethylene substrate upper reaches, behind 60 ℃ of heat treated 24h, peels off and can obtain graphite oxide paper.
As shown in Figure 1, the mechanics Enhancement Method of the described graphite oxide paper of present embodiment may further comprise the steps:
The first step, at room temperature joins the natural flaky graphite of 10g 500 purposes in the 1000mL flask, mechanical stirring evenly after, add the 5g SODIUMNITRATE, continue to stir 1h, ice bath is cooled to 0 ℃, then, in 5h, add 30g potassium permanganate in batches, keep temperature of reaction system not to be higher than 15 ℃, remove ice bath, temperature of reaction system is risen to 35 ± 3 ℃ with heating in water bath, fully stirring reaction is 2 hours, obtains the brown graphite suspension.
Second step, the frozen water of 500mL is added quencher reaction in the flask, slowly add mass percent concentration subsequently and be 30% aqueous hydrogen peroxide solution 35mL, obtain glassy yellow graphene oxide suspension.
The 3rd the step, with the graphite oxide suspension filtered, obtain the tawny filter cake.With mass percentage concentration is that the washing of 3% dilute hydrochloric acid solution does not have SO until filtrate
4 2-Till the existence, continue to wash with water, until the no Cl of filtrate
-Exist, resulting filter cake places 40 ℃ of vacuum-drying 24h of vacuum drying oven, obtains the graphene oxide solid.
The 4th goes on foot, graphene oxide is scattered in the water, form the dispersion liquid of 0.5mg/mL, adding quality percentage composition is 0.1% glutaraldehyde, stirring reaction 1h, prolong film forming at tetrafluoroethylene substrate upper reaches, behind 60 ℃ of heat treated 24h, peel off and can obtain mechanical property enhanced graphite oxide paper, its mechanical property has improved 20%.
Step such as embodiment 1 in the process that adds potassium permanganate, reduce to cooling temperature-10 ℃, and the mean sizes of resulting flake graphite alkene has increased by 50%.
Step such as embodiment 1, graphene oxide is scattered in the water, and the concentration that forms dispersion liquid becomes 5mg/mL by 0.5mg/mL, the mechanical properties decrease 20% of resulting graphite oxide paper.
Step such as embodiment 2 bring up to 1% with the quality percentage composition of glutaraldehyde from 0.1%, and the mechanical property of resulting graphite oxide paper has improved 40%.
In the preparation process of graphene oxide, by adopting the method for potassium permanganate/vitriol oil intercalation oxidation, obtain can be in organic solvent individual layer dispersive graphene oxide sheet, help in reduction process, further obtaining dispersive Graphene in organic solvent.Utilize atomic force microscope and scanning electronic microscope, the pattern of graphene oxide is characterized.The atomic force microscope picture of graphene oxide shows that mono-layer graphite oxide alkene is smooth and level and smooth, shown in the thickness chart 2b, is about 0.8～1.2nm shown in Fig. 2 a.The scanning electron microscope picture shows that graphene oxide is of a size of micron level shown in Fig. 2 c.
In the preparation process of graphite oxide paper,, come the thickness of controlled oxidation graphite paper by the concentration and the volume of controlled oxidation graphite suspension.By the quality percentage composition and the reaction times of control glutaraldehyde, come the mechanical strength of controlled oxidation graphite paper.
Claims (10)
1. the optimization preparation method of a graphite oxide paper, it is characterized in that, after the employing hydrogen peroxide prepares graphene oxide, add glutaraldehyde solution in the suspension with graphene oxide, after stirring in substrate the curtain coating drying, obtain mechanical property enhanced graphite oxide paper.
2. the optimization preparation method of graphite oxide paper according to claim 1, it is characterized in that, described graphene oxide prepares in the following manner: after frozen water and graphite suspension are carried out the quencher reaction, slowly add aqueous hydrogen peroxide solution and obtain glassy yellow graphene oxide suspension, obtain after filtration carrying out pickling and drying successively behind the tawny filter cake, obtain the graphene oxide solid.
3. the optimization preparation method of graphite oxide paper according to claim 1 and 2 is characterized in that, the mass percent concentration of described hydrogen peroxide is 30%.
4. the optimization preparation method of graphite oxide paper according to claim 2 is characterized in that, described pickling and drying are meant: adopting mass percent is that 3% dilute hydrochloric acid repetitive scrubbing to filtrate does not have SO
4 2-Exist, and then be washed till filtrate with deionized water and do not have Cl
-Exist, 40 ℃ of vacuum-drying 24h in vacuum drying oven obtain the graphene oxide solid then.
5. the optimization preparation method of graphite oxide paper according to claim 2, it is characterized in that, described graphite suspension prepares in the following manner: at room temperature graphite is joined in the vitriol oil, after stirring, add SODIUMNITRATE, carry out cooling process after fully stirring 1h, add potassium permanganate then in batches, be heated to 35 ± 3 ℃ with water-bath at last, fully react and add mixture of ice and water quencher reaction behind the 2h, obtain the brown graphite suspension.
6. the optimization preparation method of graphite oxide paper according to claim 5, it is characterized in that, the described potassium permanganate that in batches adds is meant that the potassium permanganate amount of each adding is 2g～3g, and the timed interval that at every turn adds potassium permanganate is 20min, so that the temperature of reaction system remains on below 15 ℃.
7. the optimization preparation method of graphite oxide paper according to claim 1 and 2 is characterized in that, the suspension of described graphene oxide is meant: graphene oxide is scattered in the water, and its concentration is 0.1mg/mL～5mg/mL.
8. the optimization preparation method of graphite oxide paper according to claim 1, it is characterized in that described substrate is tetrafluoroethylene, polycarbonate, polyethylene, polypropylene, polyimide, steel plate, PET, polyaryletherketone, polyvinyl chloride, polyvinylidene difluoride (PVDF), urethane, poly(lactic acid), polystyrene, ABS resin, polyacrylonitrile, poly (arylene ether nitrile), polyethersulfone, polysiloxane, Mierocrystalline cellulose, rubber, Polyvinyl carbazole, mica, Resins, epoxy, resol, maleic resin or fluoro-resin.
9. the optimization preparation method of graphite oxide paper according to claim 1 is characterized in that, the mass percentage concentration of described glutaraldehyde solution is 2%～100%.
10. a graphite oxide paper is characterized in that, adopts the described method of above-mentioned arbitrary claim to prepare.
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