CN103508439A - Graphene preparation method - Google Patents
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- CN103508439A CN103508439A CN201210203201.2A CN201210203201A CN103508439A CN 103508439 A CN103508439 A CN 103508439A CN 201210203201 A CN201210203201 A CN 201210203201A CN 103508439 A CN103508439 A CN 103508439A
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Abstract
A graphene preparation method comprises the following steps: adding graphite oxide into water, and carrying out ultrasonic dispersion to form a graphene oxide suspension; filtering the graphene oxide suspension, cooling filter residues obtained after the filtration at a temperature of -25 - -10DEG C for 1-2h, and drying the filter residues at a temperature of -60 - -40DEG C under a pressure of 0.5-1Pa for 12-24h to obtain graphene oxide; and heating the graphene oxide to 700-900DEG C under the introduction of a protective gas, and maintaining for 0.5-1h to obtain graphene. Graphene prepared through the graphene preparation method has a large specific surface area.
Description
Technical field
The present invention relates to a kind of preparation method of Graphene.
Background technology
Graphene is a kind of two-dimentional unimolecular layer material, has excellent physical properties, as high theoretical specific surface area, excellent physical strength, good snappiness and high specific conductivity etc., is subject to investigator's extensive concern.Although the theoretical specific surface area of Graphene is up to 2600m
2/ g, but the prepared Graphene specific surface area of general method is generally all at 600m
2/ g left and right, far below its theoretical specific surface area, reason is mainly that adjacent Graphene sector-meeting attracts each other by the Van der Waals force between π key and π key owing to there being large π key on graphene sheet layer, cause agglomeration, the specific surface area of Graphene is reduced greatly.
Summary of the invention
Based on this, be necessary to provide the preparation method of the Graphene that a kind of specific surface area is larger.
A preparation method for Graphene, comprises the steps:
Graphite oxide is added to the water to ultrasonic dispersion and forms graphene oxide suspension;
Filter described graphene oxide suspension, the filter residue that filtration is obtained is positioned under the environment of-25 ℃～-10 ℃ after cooling 1 hour ~ 2 hours, more described filter residue is positioned over to temperature is the dry graphene oxide that obtains for 12 ~ 24 hours under-60 ℃～-40 ℃, the air pressure environment that is 0.1Pa ~ 1Pa; And
Passing under the condition of protective gas, the temperature of described graphene oxide is being increased to 700 ℃ ~ 900 ℃, and keeping 0.5 hour ~ 1 hour, obtaining Graphene.
In an embodiment, described in described graphene oxide suspension, the concentration of graphene oxide is 0.5mg/mL ~ 1mg/mL therein.
In an embodiment, by the time of the ultrasonic dispersion of described graphite oxide, it is 1 hour ~ 2 hours therein.
In an embodiment, described protective gas is selected from least one in nitrogen and argon gas therein.
In an embodiment, the flow velocity of described protective gas is 300mL/min ~ 400mL/min therein.
Therein in an embodiment, the temperature of graphene oxide is increased to 700 ℃ ~ 900 ℃ with the speed of 15 ℃/min ~ 25 ℃/min.
In an embodiment, before the step of preparing graphene oxide suspension, also comprise therein: prepare graphite oxide, prepare graphite oxide and comprise the following steps:
In the mix acid liquor that adds the vitriol oil and concentrated nitric acid to form in graphite, form mixed solution, the temperature of mixed solution is remained on to-2 ℃ ~ 2 ℃ and stir 10min ~ 30min;
In mixed solution, add potassium permanganate, continue that the temperature of mixed solution is remained on to-2 ℃ ~ 2 ℃ and stir 1h;
Mixed solution is warming up to 80 ℃ ~ 90 ℃ and be incubated 0.5h ~ 2h;
In mixed solution, add deionized water, continue at 80 ℃ ~ 90 ℃ insulation 0.5h ~ 2h; And
In mixed solution, add hydrogen peroxide to remove potassium permanganate, suction filtration, washing solids, obtains graphite oxide after drying solid thing.
In an embodiment, the solid-to-liquid ratio of described graphite and the described vitriol oil and concentrated nitric acid is 1g:(85mL ~ 95mL therein): (24mL ~ 25mL).
In an embodiment, the mass ratio of described graphite and described potassium permanganate is 1:3 ~ 1:6 therein.
Therein in an embodiment, to adding massfraction in mixed solution, be that 30% superoxol is removed potassium permanganate, the solid-to-liquid ratio of described potassium permanganate and described superoxol is 1g:1mL ~ 1g:3ml.
The preparation method of above-mentioned Graphene, in the filter residue that graphene oxide suspension filtered is obtained, contain water, filter residue is positioned under the environment of-25 ℃～-10 ℃ after cooling 1 hour ~ 2 hours, water-cooled in filter residue is frozen into as ice, under the environment that afterwards filter residue to be positioned over to temperature and to be-60 ℃ ~-40 ℃, air pressure be 0.1Pa ~ 1Pa, now also direct gasification becomes vaporous water, thereby graphene oxide is dried and can effectively prevents the reunion of graphene oxide lamella, thereby the specific surface area of the Graphene obtaining is larger.
Accompanying drawing explanation
Fig. 1 is preparation method's the schema of the Graphene of an embodiment;
Fig. 2 is the adsorption-desorption isothermal curve of the Graphene of embodiment 1 preparation.
Embodiment
For above-mentioned purpose of the present invention, feature and advantage can be become apparent more, below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in detail.A lot of details have been set forth in the following description so that fully understand the present invention.But the present invention can implement to be much different from alternate manner described here, and those skilled in the art can do similar improvement without prejudice to intension of the present invention in the situation that, so the present invention is not subject to the restriction of following public concrete enforcement.
Refer to Fig. 1, the preparation method of the Graphene of an embodiment, comprises the steps:
Step S110, prepare graphite oxide.
Preparing graphite oxide comprises the following steps:
Step 1, add the vitriol oil and concentrated nitric acid to form in graphite mix acid liquor in form mixed solution, the temperature of mixed solution is remained on to-2 ℃ ~ 2 ℃ and stirs 10min ~ 30min.
Preferably, the purity of graphite is 99.5%.Graphite is that particle diameter is micron-sized powder.
Preferably, the solid-to-liquid ratio of graphite and the vitriol oil and concentrated nitric acid is 1g:(85mL ~ 95mL): (24mL ~ 25mL).
Preferably, mixed solution is positioned in ice-water bath and stirs 20 minutes.
Preferably, the mass concentration of concentrated nitric acid is 98%, and the mass concentration of concentrated nitric acid is 65%.
Step 2, in mixed solution, add potassium permanganate, continue that the temperature of mixed solution is remained on to-2 ℃ ~ 2 ℃ and stir 1 hour.
Preferably, the mass ratio of the graphite in mixed solution and potassium permanganate is 1:3 ~ 1:6.
Step 3, mixed solution is warming up to 80 ℃ ~ 90 ℃ and keep 0.5 hour ~ 2 hours.
Step 4, in mixed solution, add deionized water, continue 80 ℃ ~ 90 ℃ insulations 0.5 hour ~ 2 hours.
Preferably, the solid-to-liquid ratio of graphite and deionized water is 1g:(60mL ~ 92mL).
Step 5, in mixed solution, add hydrogen peroxide to remove potassium permanganate, suction filtration, washing solids, obtains graphite oxide after drying solid thing.
Preferably, to adding massfraction in mixed solution, be that 30% superoxol is removed potassium permanganate, the solid-to-liquid ratio of potassium permanganate and superoxol is 1g:1mL ~ 1g:3ml.
Preferably, use successively dilute hydrochloric acid and deionized water repetitive scrubbing solids.
Preferably, by solids vacuum-drying 12 hours at 60 ℃.
Be appreciated that step S110 also can omit, now directly buy graphite oxide.
Step S120, graphite oxide is added to the water to ultrasonic dispersion forms graphene oxide suspension.
Preferably, the graphite oxide of preparing in step S110 is added deionized water for ultrasonic disperse 1 hour ~ 2 hours.
Preferably, the power of ultrasonic dispersion is 500W.
Preferably, in graphene oxide suspension, the concentration of graphene oxide is 0.5mg/mL ~ 1mg/mL.
Step S130, filtration graphene oxide suspension, the filter residue that filtration is obtained is positioned under the environment of-25 ℃～-10 ℃ after cooling 1 hour ~ 2 hours, then filter residue is positioned over to temperature is the dry graphene oxide that obtains for 12 ~ 24 hours under-60 ℃～-40 ℃, the air pressure environment that is 0.1Pa ~ 1Pa.
In this step, in the filter residue that graphene oxide suspension filtered is obtained, contain water, filter residue is positioned under the environment of-25 ℃～-10 ℃ after cooling 1 hour ~ 2 hours, water-cooled in filter residue is frozen into as ice, under the environment that afterwards filter residue to be positioned over to temperature and to be-60 ℃～-40 ℃, air pressure be 0.1Pa ~ 1Pa, now also direct gasification becomes vaporous water, thereby graphene oxide is dried and can be effectively prevented the reunion of graphene oxide lamella.
Step S140, passing under the condition of protective gas, the temperature of the residing environment of graphene oxide is being warming up to 700 ℃ ~ 900 ℃, and keeps 0.5 hour ~ 1 hour, obtaining Graphene.
Preferably, protective gas is selected from least one in nitrogen and argon gas.
Preferably, the flow velocity of protective gas is 300mL/min ~ 400mL/min.
Preferably, the temperature of the residing environment of graphene oxide is warming up to 700 ℃ ~ 900 ℃ with the temperature rise rate of 15 ℃/min ~ 25 ℃/min.
Preferably, the Graphene obtaining at protective gas atmosphere borehole cooling to room temperature.
The preparation method of above-mentioned Graphene, in the filter residue that graphene oxide suspension filtered is obtained, contain water, filter residue is positioned under the environment of-25 ℃～-10 ℃ after cooling 1 hour ~ 2 hours, water-cooled in filter residue is frozen into as ice, filter residue being positioned over to temperature is afterwards-60 ℃～-40 ℃, air pressure is under the environment of 0.1Pa ~ 1Pa, now also direct gasification becomes vaporous water, this can cause oxidized graphite flake interlayer to have Hen great gap, thereby graphene oxide is dried and can effectively prevents to the reunion of graphene oxide lamella, thereby the specific surface area of the Graphene obtaining is larger.
Below in conjunction with specific embodiment, further illustrate.
Embodiment 1
The present embodiment is by graphite oxide, through peeling off and lyophilize, peeling off that to prepare the process flow sheet of Graphene as follows again:
Graphite → graphite oxide → graphene oxide → Graphene
(1) graphite: purity 99.5%;
(2) graphite oxide: take the graphite 1g that (1) moderate purity is 99.5% and add in the mixing solutions being formed by the 90ml vitriol oil (massfraction is 98%) and 25ml concentrated nitric acid (massfraction is 65%), mixture is placed under frozen water mixing bath environment and is stirred 20 minutes, in mixture, add 6g potassium permanganate at leisure again, stir 1 hour, then mixture is heated to 85 ° of C and keeps 30 minutes, add afterwards 92ml deionized water to continue to keep 30 minutes under 85 ° of C, finally add 10ml superoxol (massfraction 30%), stir 10 minutes, mixture is carried out to suction filtration, with 100ml dilute hydrochloric acid and 150ml deionized water, solids is washed respectively successively again, wash altogether three times, last solid matter is the dry graphite oxide that obtains for 12 hours in 60 ° of C vacuum drying ovens,
(3) graphene oxide: the graphite oxide obtaining in (2) is dispersed in deionized water, the solubility of graphite oxide solution is 0.5mg/ml, the ultrasonic apparatus that is 500W with power is carried out ultrasonic to graphite oxide solution, continue 2 hours, filter, the solids after filtering is moved in the environment of-25 ° of C, after 1 hour, move to again in the environment that-50 ° of C, pressure are 1Pa, continue 12 hours, obtain graphene oxide;
(4) Graphene: get the graphene oxide obtaining in (3) and be placed in argon gas (flow velocity: 400ml/min) under atmosphere, with 20 ° of C/min temperature rise rates, graphene oxide temperature is around risen to 800 ° of C, and keep 30 minutes, finally at argon gas, (flow velocity: 400ml/min) atmosphere drops to room temperature, obtains Graphene.
Refer to Fig. 2, Figure 2 shows that the adsorption-desorption isothermal curve that the Graphene of embodiment 1 preparation utilizes BET PORE SIZE APPARATUS FOR to draw.Curve is wherein isothermal desorption curve, and curve is below isothermal adsorption curve.The specific surface area that can be drawn the Graphene of embodiment 1 preparation by Fig. 2 is 756m
2/ g.
Embodiment 2
The present embodiment is by graphite oxide, through peeling off and lyophilize, peeling off that to prepare the process flow sheet of Graphene as follows again:
Graphite → graphite oxide → graphene oxide → Graphene
(1) graphite: purity 99.5%;
(2) graphite oxide: take the graphite 3g that (1) moderate purity is 99.5% and add in the mixing solutions being formed by the 285ml vitriol oil (massfraction is 98%) and 72ml concentrated nitric acid (massfraction is 65%), mixture is placed under frozen water mixing bath environment and is stirred 20 minutes, in mixture, add 12g potassium permanganate at leisure again, stir 1 hour, then mixture is heated to 85 ° of C and keeps 30 minutes, add afterwards 150ml deionized water to continue to keep 30 minutes under 85 ° of C, finally add 18ml superoxol (massfraction 30%), stir 10 minutes, mixture is carried out to suction filtration, with 200ml dilute hydrochloric acid and 30ml deionized water, solids is washed respectively successively again, wash altogether three times, last solid matter is the dry graphite oxide that obtains for 12 hours in 60 ° of C vacuum drying ovens,
(3) graphene oxide: the graphite oxide obtaining in (2) is dispersed in deionized water, the solubility of graphite oxide solution is 0.5mg/ml, the ultrasonic apparatus that is 500W with power is carried out ultrasonic to graphite oxide solution, continue 2 hours, filter, the solids after filtering is moved in the environment of-15 ° of C, after 2 hours, move to again in the environment that-20 ° of C, pressure are 0.5Pa, continue 20 hours, obtain graphene oxide;
(4) Graphene: get the graphene oxide obtaining in (3) and be placed in argon gas (flow velocity: 300ml/min) under atmosphere, with 25 ° of C/min temperature rise rates, graphene oxide temperature is around risen to 700 ° of C, and keep 30 minutes, finally at argon gas, (flow velocity: 300ml/min) atmosphere drops to room temperature, obtains Graphene.
The Graphene of embodiment 2 preparations is through the test of BET PORE SIZE APPARATUS FOR, and its specific surface area is 813m
2/ g.
Embodiment 3
The present embodiment is by graphite oxide, through peeling off and lyophilize, peeling off that to prepare the process flow sheet of Graphene as follows again:
Graphite → graphite oxide → graphene oxide → Graphene
(1) graphite: purity 99.5%;
(2) graphite oxide: take the graphite 5g that (1) moderate purity is 99.5% and add in the mixing solutions being formed by the 420ml vitriol oil (massfraction is 98%) and 120ml concentrated nitric acid (massfraction is 65%), mixture is placed under frozen water mixing bath environment and is stirred 20 minutes, in mixture, add 20g potassium permanganate at leisure again, stir 1 hour, then mixture is heated to 85 ° of C and keeps 30 minutes, add afterwards 300ml deionized water to continue to keep 30 minutes under 85 ° of C, finally add 40ml superoxol (massfraction 30%), stir 10 minutes, mixture is carried out to suction filtration, with 400ml dilute hydrochloric acid and 800ml deionized water, solids is washed respectively successively again, wash altogether three times, last solid matter is the dry graphite oxide that obtains for 12 hours in 60 ° of C vacuum drying ovens,
(3) graphene oxide: the graphite oxide obtaining in (2) is dispersed in deionized water, the solubility of graphite oxide solution is 1mg/ml, the ultrasonic apparatus that is 500W with power is carried out ultrasonic to graphite oxide solution, continue 2 hours, filter, the solids after filtering is moved in the environment of-25 ° of C, after 1 hour, move to again in the environment that-45 ° of C, pressure are 0.5Pa, continue 12 hours, obtain graphene oxide;
(4) Graphene: get the graphene oxide obtaining in (3) and be placed in argon gas (flow velocity: 400ml/min) under atmosphere, with 15 ° of C/min temperature rise rates, graphene oxide temperature is around risen to 900 ° of C, and keep 1 hour, finally at argon gas, (flow velocity: 400ml/min) atmosphere drops to room temperature, obtains Graphene.
The Graphene of embodiment 3 preparations is through the test of BET PORE SIZE APPARATUS FOR, and its specific surface area is 724m
2/ g.
Embodiment 4
The present embodiment is by graphite oxide, through peeling off and lyophilize, peeling off that to prepare the process flow sheet of Graphene as follows again:
Graphite → graphite oxide → graphene oxide → Graphene
(1) graphite: purity 99.5%;
(2) graphite oxide: take the graphite 1g that (1) moderate purity is 99.5% and add in the mixing solutions being formed by the 90ml vitriol oil (massfraction is 98%) and 25ml concentrated nitric acid (massfraction is 65%), mixture is placed under frozen water mixing bath environment and is stirred 20 minutes, in mixture, add 4g potassium permanganate at leisure again, stir 1 hour, then mixture is heated to 85 ° of C and keeps 30 minutes, add afterwards 92ml deionized water to continue to keep 30 minutes under 85 ° of C, finally add 9ml superoxol (massfraction 30%), stir 10 minutes, mixture is carried out to suction filtration, with 100ml dilute hydrochloric acid and 150ml deionized water, solids is washed respectively successively again, wash altogether three times, last solid matter is the dry graphite oxide that obtains for 12 hours in 60 ° of C vacuum drying ovens,
(3) graphene oxide: the graphite oxide obtaining in (2) is dispersed in deionized water, the solubility of graphite oxide solution is 0.5mg/ml, the ultrasonic apparatus that is 500W with power is carried out ultrasonic to graphite oxide solution, continue 2 hours, filter, the solids after filtering is moved in the environment of-10 ° of C, after 2 hours, move to again in the environment that-60 ° of C, pressure are 0.1Pa, continue 24 hours, obtain graphene oxide;
(4) Graphene: get the graphene oxide obtaining in (3) and be placed in argon gas (flow velocity: 400ml/min) under atmosphere, with 20 ° of C/min temperature rise rates, graphene oxide temperature is around risen to 800 ° of C, and keep 1 hour, finally at argon gas, (flow velocity: 400ml/min) atmosphere drops to room temperature, obtains Graphene.
The Graphene of embodiment 4 preparations is through the test of BET PORE SIZE APPARATUS FOR, and its specific surface area is 879m
2/ g.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a preparation method for Graphene, is characterized in that, comprises the steps:
Graphite oxide is added to the water to ultrasonic dispersion and forms graphene oxide suspension;
Filter described graphene oxide suspension, the filter residue that filtration is obtained is positioned under the environment of-25 ℃～-10 ℃ after cooling 1 hour ~ 2 hours, more described filter residue is positioned over to temperature is the dry graphene oxide that obtains for 12 ~ 24 hours under-60 ℃～-40 ℃, the air pressure environment that is 0.1Pa ~ 1Pa; And
Passing under the condition of protective gas, the temperature of described graphene oxide is being increased to 700 ℃ ~ 900 ℃, and keeping 0.5 hour ~ 1 hour, obtaining Graphene.
2. the preparation method of Graphene according to claim 1, is characterized in that, described in described graphene oxide suspension, the concentration of graphene oxide is 0.5mg/mL ~ 1mg/mL.
3. the preparation method of Graphene according to claim 1, is characterized in that, by the time of the ultrasonic dispersion of described graphite oxide, is 1 hour ~ 2 hours.
4. the preparation method of Graphene according to claim 1, is characterized in that, described protective gas is selected from least one in nitrogen and argon gas.
5. the preparation method of Graphene according to claim 1, is characterized in that, the flow velocity of described protective gas is 300mL/min ~ 400mL/min.
6. the preparation method of Graphene according to claim 1, is characterized in that, the temperature of graphene oxide is increased to 700 ℃ ~ 900 ℃ with the speed of 15 ℃/min ~ 25 ℃/min.
7. the preparation method of Graphene according to claim 1, is characterized in that, before the step of preparing graphene oxide suspension, also comprises: prepare graphite oxide, prepare graphite oxide and comprise the following steps:
In the mix acid liquor that adds the vitriol oil and concentrated nitric acid to form in graphite, form mixed solution, the temperature of mixed solution is remained on to-2 ℃ ~ 2 ℃ and stir 10min ~ 30min;
In mixed solution, add potassium permanganate, continue that the temperature of mixed solution is remained on to-2 ℃ ~ 2 ℃ and stir 1h;
Mixed solution is warming up to 80 ℃ ~ 90 ℃ and be incubated 0.5h ~ 2h;
In mixed solution, add deionized water, continue at 80 ℃ ~ 90 ℃ insulation 0.5h ~ 2h; And
In mixed solution, add hydrogen peroxide to remove potassium permanganate, suction filtration, washing solids, obtains graphite oxide after drying solid thing.
8. the preparation method of Graphene according to claim 7, is characterized in that, the solid-to-liquid ratio of described graphite and the described vitriol oil and concentrated nitric acid is 1g:(85mL ~ 95mL): (24mL ~ 25mL).
9. the preparation method of Graphene according to claim 7, is characterized in that, the mass ratio of described graphite and described potassium permanganate is 1:3 ~ 1:6.
10. the preparation method of Graphene according to claim 7, it is characterized in that, to adding massfraction in mixed solution, be that 30% superoxol is removed potassium permanganate, the solid-to-liquid ratio of described potassium permanganate and described superoxol is 1g:1mL ~ 1g:3ml.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103787326A (en) * | 2014-03-06 | 2014-05-14 | 南开大学 | Preparation method of grapheme material with three-dimensional network structure |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830459A (en) * | 2010-05-20 | 2010-09-15 | 复旦大学 | Method for preparing dry graphene powder |
-
2012
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830459A (en) * | 2010-05-20 | 2010-09-15 | 复旦大学 | Method for preparing dry graphene powder |
Non-Patent Citations (4)
| Title |
|---|
| LAURA J.COTE ET AL.: "Langmuir Blodgett Assembly of Graphite Oxide Single Layers", 《J.AM.CHEM.SOC.》 * |
| XUFENG ZHOU ET AL.,: "Graphene foam as an anode for high-rate Li-ion batteries", 《IOP CONF.SERIES: MATERIALS SCIENCE AND ENGINEERING》 * |
| YING LONG ET AL.: "Oxidation of SO2 to SO3 catalyzed by graphene oxide foams", 《JOURNAL OF MATERIALS CHEMISTRY》 * |
| 傅玲等: "Hummesr法制备氧化石墨时影响氧化程度的工艺因素研究", 《炭素》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103787326A (en) * | 2014-03-06 | 2014-05-14 | 南开大学 | Preparation method of grapheme material with three-dimensional network structure |
| CN103787326B (en) * | 2014-03-06 | 2015-06-17 | 南开大学 | Preparation method of grapheme material with three-dimensional network structure |
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Application publication date: 20140115 |