CN108217632A - The preparation method of graphene aerogel with superhigh specific surface area - Google Patents
The preparation method of graphene aerogel with superhigh specific surface area Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of graphene aerogel, and in particular to a kind of preparation method of the graphene aerogel with superhigh specific surface area.It dissolves polyvinyl alcohol in ultrasonic disperse in distilled water and is made polyvinyl alcohol water solution, then solid oxidation graphene ultrasonic disperse is obtained into the graphene oxide dispersion of a concentration of 2 11mg/cm3 in polyvinyl alcohol water solution；Graphene oxide dispersion with 0.003~0.3 part of siloxanes is uniformly mixed, obtains oxidation silicon hybridization Graphene gel；Oxidation silicon hybridization Graphene gel is dried, obtains silica with great specific surface area hydridization graphene aerogel；Oxidation silicon hybridization graphene aerogel is put into pyrolysis furnace, is passed through inert gas, furnace cooling obtains superhigh specific surface area graphene aerogel.The specific surface area that the present invention improves graphene aerogel does not significantly affect the generation of the chemical constitution of graphene again simultaneously.
Description
Technical field
The present invention relates to a kind of preparation methods of graphene aerogel, and in particular to a kind of stone with superhigh specific surface area
The preparation method of black alkene aeroge.
Background technology
Graphene aerogel is the three-dimensional porous structure material mutually overlapped by graphene, this material has super
Gently, a series of high features of high-elastic, large specific surface area, conductive and heat-conductive rate, in catalysis, electrochemistry, the energy, sensor, super electricity
Many fields such as appearance, absorption, thermal control have huge application potential.Redox graphene dispersion liquid or aeroge are mesh
A kind of preceding the most commonly used method for preparing graphene aerogel, this method is with method is simple, at low cost, performance is more excellent
The features such as different.But in reduction process, (oxidation) graphene is easy to reunite, therefore the graphene aerogel prepared
Specific surface area be much smaller than graphene specific surface area (2600m2/g), this is very significant considering that the performance of graphene,
Application of the graphene aerogel in many fields is seriously affected.Therefore, improving the specific surface area of graphene aerogel just becomes
It is very important.
Invention content
The overcome the deficiencies in the prior art during purpose of the present invention and a kind of graphene gas with superhigh specific surface area is provided
The preparation method of gel, the specific surface area for improving graphene aerogel do not generate apparent shadow to the chemical constitution of graphene again simultaneously
It rings.
A kind of preparation method of the graphene aerogel with superhigh specific surface area, includes the following steps：
The first step, the preparation of graphene oxide dispersion：It dissolves polyvinyl alcohol in ultrasonic disperse in distilled water and polyethylene is made
Alcohol solution, then solid oxidation graphene ultrasonic disperse is obtained into the institute of a concentration of 2-11mg/cm3 in polyvinyl alcohol water solution
State graphene oxide dispersion；
Second step aoxidizes the preparation of silicon hybridization Graphene gel：Graphene oxide dispersion that the first step is obtained with 0.003~
0.3 part of siloxanes is uniformly mixed, and mixture is warming up to 50~160 DEG C of 3~45h of heat preservation, oxidation silicon hybridization graphene is obtained and coagulates
Glue；
Third walks, dry：The oxidation silicon hybridization Graphene gel that third walks is dried, obtains high-specific surface area oxidation
Silicon hybridization graphene aerogel；
4th step, Pintsch process：The oxidation silicon hybridization graphene aerogel that 4th step obtains is put into pyrolysis furnace, is passed through lazy
Property gas, then heat to 800~1600 DEG C, keep the temperature 1~9h, furnace cooling obtains superhigh specific surface area graphene aerogel.
A concentration of 2.5 mg/cm3 of the polyvinyl alcohol water solution.
Siloxanes described in second step is ethyl orthosilicate, methyl orthosilicate, methyltrimethoxysilane, triethoxysilicane
One kind of alkane or trimethoxy silane.
It uses when intentionally getting aperture and concentrate on the silica with great specific surface area hydridization graphene aerogel of 2~300nm
CO2 supercritical dryings, i.e., by the hydridization Graphene gel that second step the obtains deionized water displacement 2~12 of 3~40 times of volumes
It is secondary, then the ethanol replacement 2~12 times with 3~40 times of volumes, each time swap are 2~10h, obtain the oxidation after solvent displacement
Silicon hybridization Graphene gel, then oxidation silicon hybridization Graphene gel after solvent is replaced are put into CO2 supercritical drying devices
In drying kettle, the CO2 of supercriticality is then passed to, is replaced 3~15 hours, is finally discharged and pressed with the rate of 100KPa/min
Power, furnace cooling take out and can obtain silica with great specific surface area hydridization graphene aerogel.
Inert gas described in 4th step is one kind in nitrogen, argon gas, helium, neon, Krypton.
4th step is passed through the flow velocity of inert gas as 25~500ml/min, the rate of heating for 1 DEG C/min~60 DEG C/
min。
The invention has the advantages that：A kind of system of graphene aerogel with superhigh specific surface area of the present invention
Preparation Method realizes that raw material fully uniformly mixes in a manner of being mixed by liquid, and reacted generation grain size is minimum, dispersion is equal
Even silica nano particle so as to which graphene dispersion be come, prevents it from reuniting；Deoxidation is removed further through Pintsch process
Silicon, while play the role of similar activation, so that obtained superhigh specific surface area graphene aerogel specific surface area superelevation,
And high temperature stability performance is excellent, has in fields such as catalysis, electrochemistry, the energy, sensor, super capacitor, absorption, thermal controls good
Good application prospect.
Specific embodiment
With embodiment, the invention will be further described below, but these embodiments do not produce protection scope of the present invention
Raw any restrictions.
Embodiment 1
A kind of preparation method of the graphene aerogel with superhigh specific surface area, includes the following steps：
The first step, the preparation of graphene oxide dispersion：It dissolves polyvinyl alcohol in ultrasonic disperse in distilled water and 2.5 mg/ is made
Cm3 polyvinyl alcohol water solutions, then solid oxidation graphene ultrasonic disperse is obtained into a concentration of 2mg/cm in polyvinyl alcohol water solution
3 graphene oxide dispersion；
Second step aoxidizes the preparation of silicon hybridization Graphene gel：Graphene oxide dispersion that the first step is obtained with 0.003 part
Ethyl orthosilicate is uniformly mixed, and mixture is warming up to 50 DEG C of heat preservation 3h, obtains oxidation silicon hybridization Graphene gel；
Third walks, dry：The oxidation silicon hybridization Graphene gel that third walks is dried, obtains high-specific surface area oxidation
Silicon hybridization graphene aerogel；
4th step, Pintsch process：The oxidation silicon hybridization graphene aerogel that 4th step obtains is put into pyrolysis furnace, is passed through nitrogen
Gas then heats to 800 DEG C, keeps the temperature 1h, and furnace cooling obtains superhigh specific surface area graphene aerogel；It is passed through the flow velocity of nitrogen
For 25ml/min, the rate of heating is 1 DEG C/min.
Embodiment 2
A kind of preparation method of the graphene aerogel with superhigh specific surface area, includes the following steps：
The first step, the preparation of graphene oxide dispersion：It dissolves polyvinyl alcohol in ultrasonic disperse in distilled water and 2.5 mg/ is made
Cm3 polyvinyl alcohol water solutions, then solid oxidation graphene ultrasonic disperse is obtained into a concentration of 11mg/ in polyvinyl alcohol water solution
The graphene oxide dispersion of cm3；
Second step aoxidizes the preparation of silicon hybridization Graphene gel：Graphene oxide dispersion that the first step is obtained with 0.3 part just
Methyl silicate is uniformly mixed, and mixture is warming up to 160 DEG C of heat preservation 45h, obtains oxidation silicon hybridization Graphene gel；
Third walks, dry：The oxidation silicon hybridization Graphene gel that third walks is dried, obtains high-specific surface area oxidation
Silicon hybridization graphene aerogel；
4th step, Pintsch process：The oxidation silicon hybridization graphene aerogel that 4th step obtains is put into pyrolysis furnace, is passed through argon
Gas then heats to 1600 DEG C, keeps the temperature 9h, and furnace cooling obtains superhigh specific surface area graphene aerogel；It is passed through the stream of argon gas
Speed is 500ml/min, and the rate of heating is 60 DEG C/min.
Embodiment 3
A kind of preparation method of the graphene aerogel with superhigh specific surface area, includes the following steps：
The first step, the preparation of graphene oxide dispersion：It dissolves polyvinyl alcohol in ultrasonic disperse in distilled water and 2.5 mg/ is made
Cm3 polyvinyl alcohol water solutions, then solid oxidation graphene ultrasonic disperse is obtained into a concentration of 3mg/cm in polyvinyl alcohol water solution
3 graphene oxide dispersion；
Second step aoxidizes the preparation of silicon hybridization Graphene gel：Graphene oxide dispersion that the first step is obtained with 0.005 part
Methyltrimethoxysilane is uniformly mixed, and mixture is warming up to 60 DEG C of heat preservation 5h, obtains oxidation silicon hybridization Graphene gel；
Third walks, dry：The oxidation silicon hybridization Graphene gel that third walks is dried, obtains high-specific surface area oxidation
Silicon hybridization graphene aerogel；
4th step, Pintsch process：The oxidation silicon hybridization graphene aerogel that 4th step obtains is put into pyrolysis furnace, is passed through helium
Gas then heats to 900 DEG C, keeps the temperature 3h, and furnace cooling obtains superhigh specific surface area graphene aerogel；It is passed through the flow velocity of helium
For 40ml/min, the rate of heating is 3 DEG C/min.
Embodiment 4
A kind of preparation method of the graphene aerogel with superhigh specific surface area, includes the following steps：
The first step, the preparation of graphene oxide dispersion：It dissolves polyvinyl alcohol in ultrasonic disperse in distilled water and 2.5 mg/ is made
Cm3 polyvinyl alcohol water solutions, then solid oxidation graphene ultrasonic disperse is obtained into a concentration of 9mg/cm in polyvinyl alcohol water solution
3 graphene oxide dispersion；
Second step aoxidizes the preparation of silicon hybridization Graphene gel：Graphene oxide dispersion that the first step is obtained with 0.25 part
Methyltrimethoxysilane is uniformly mixed, and mixture is warming up to 150 DEG C of heat preservation 42h, obtains oxidation silicon hybridization Graphene gel
；
Third walks, dry：The oxidation silicon hybridization Graphene gel that third walks is dried, obtains high-specific surface area oxidation
Silicon hybridization graphene aerogel；
4th step, Pintsch process：The oxidation silicon hybridization graphene aerogel that 4th step obtains is put into pyrolysis furnace, is passed through neon
Gas then heats to 1500 DEG C, keeps the temperature 7h, and furnace cooling obtains superhigh specific surface area graphene aerogel；It is passed through the stream of neon
Speed is 450ml/min, and the rate of heating is 58 DEG C/min.
Embodiment 5
A kind of preparation method of the graphene aerogel with superhigh specific surface area, includes the following steps：
The first step, the preparation of graphene oxide dispersion：It dissolves polyvinyl alcohol in ultrasonic disperse in distilled water and 2.5 mg/ is made
Cm3 polyvinyl alcohol water solutions, then solid oxidation graphene ultrasonic disperse is obtained into a concentration of 7mg/cm in polyvinyl alcohol water solution
3 graphene oxide dispersion；
Second step aoxidizes the preparation of silicon hybridization Graphene gel：The graphene oxide dispersion that the first step is obtained and 0.2 part of first
Base trimethoxy silane is uniformly mixed, and mixture is warming up to 100 DEG C of heat preservation 30h, obtains oxidation silicon hybridization Graphene gel；
Third walks, dry：The oxidation silicon hybridization Graphene gel that third walks is dried, obtains high-specific surface area oxidation
Silicon hybridization graphene aerogel；
4th step, Pintsch process：The oxidation silicon hybridization graphene aerogel that 4th step obtains is put into pyrolysis furnace, is passed through krypton
Gas then heats to 1200 DEG C, keeps the temperature 5h, and furnace cooling obtains superhigh specific surface area graphene aerogel；It is passed through the stream of Krypton
Speed is 400ml/min, and the rate of heating is 48 DEG C/min.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should all be included in the protection scope of the present invention.
Claims (5)
1. a kind of preparation method of the graphene aerogel with superhigh specific surface area, which is characterized in that include the following steps：
The first step, the preparation of graphene oxide dispersion：It dissolves polyvinyl alcohol in ultrasonic disperse in distilled water and polyethylene is made
Alcohol solution, then solid oxidation graphene ultrasonic disperse is obtained into a concentration of 2-11mg/cm in polyvinyl alcohol water solution3Institute
State graphene oxide dispersion；
Second step aoxidizes the preparation of silicon hybridization Graphene gel：Graphene oxide dispersion that the first step is obtained with 0.003~
0.3 part of siloxanes is uniformly mixed, and mixture is warming up to 50~160 DEG C of 3~45h of heat preservation, oxidation silicon hybridization graphene is obtained and coagulates
Glue；
Third walks, dry：The oxidation silicon hybridization Graphene gel that third walks is dried, obtains high-specific surface area oxidation
Silicon hybridization graphene aerogel；
4th step, Pintsch process：The oxidation silicon hybridization graphene aerogel that 4th step obtains is put into pyrolysis furnace, is passed through inertia
Gas then heats to 800~1600 DEG C, keeps the temperature 1~9h, and furnace cooling obtains superhigh specific surface area graphene aerogel.
2. the preparation method of the graphene aerogel according to claim 1 with superhigh specific surface area, which is characterized in that
A concentration of 2.5mg/cm of the polyvinyl alcohol water solution3。
3. the preparation method of the graphene aerogel according to claim 1 with superhigh specific surface area, which is characterized in that
Siloxanes described in second step is ethyl orthosilicate, methyl orthosilicate, methyltrimethoxysilane, triethoxysilane or front three
One kind of oxysilane.
4. the preparation method of the graphene aerogel according to claim 1 with superhigh specific surface area, which is characterized in that
Inert gas described in 4th step is one kind in nitrogen, argon gas, helium, neon, Krypton.
5. the preparation method of the graphene aerogel according to claim 1 with superhigh specific surface area, which is characterized in that
The flow velocity that 4th step is passed through inert gas is 25~500ml/min, and the rate of heating is 1 DEG C/min~60 DEG C/min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111517774A (en) * | 2020-04-28 | 2020-08-11 | 青岛迦南美地家居用品有限公司 | Preparation method of magnetic graphene oxide aerogel |
| WO2020244263A1 (en) * | 2019-06-06 | 2020-12-10 | 青岛理工大学 | Graphene oxide-teos/silane composite gel material, preparation method therefor and use thereof |
| GB2595009A (en) * | 2019-06-06 | 2021-11-17 | Univ Qingdao Technology | Graphene oxide-TEOS/silane composite gel material, preparation method therefor and use thereof |
| CN115819000A (en) * | 2021-12-31 | 2023-03-21 | 南京诚赢集约建材科技有限公司 | Pilot test method based on mixed dispersion of asphalt regenerant and graphene |
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| CN104828810A (en) * | 2015-05-07 | 2015-08-12 | 中国人民解放军国防科学技术大学 | Preparation method of graphene aerogel with ultrahigh specific surface area |
| CN104843676A (en) * | 2014-12-03 | 2015-08-19 | 北汽福田汽车股份有限公司 | Preparation method for graphene aerogel |
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2018
- 2018-02-05 CN CN201810114082.0A patent/CN108217632A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104843676A (en) * | 2014-12-03 | 2015-08-19 | 北汽福田汽车股份有限公司 | Preparation method for graphene aerogel |
| CN104828810A (en) * | 2015-05-07 | 2015-08-12 | 中国人民解放军国防科学技术大学 | Preparation method of graphene aerogel with ultrahigh specific surface area |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020244263A1 (en) * | 2019-06-06 | 2020-12-10 | 青岛理工大学 | Graphene oxide-teos/silane composite gel material, preparation method therefor and use thereof |
| GB2595009A (en) * | 2019-06-06 | 2021-11-17 | Univ Qingdao Technology | Graphene oxide-TEOS/silane composite gel material, preparation method therefor and use thereof |
| GB2595009B (en) * | 2019-06-06 | 2023-07-26 | Univ Qingdao Technology | Graphene oxide-tetraethyl orthosilicate/silane composite gel material, and preparation method and use thereof |
| US11879069B2 (en) | 2019-06-06 | 2024-01-23 | Qingdao university of technology | Graphene orthosilicate/silane composite gel material, and preparation method and use thereof |
| CN111517774A (en) * | 2020-04-28 | 2020-08-11 | 青岛迦南美地家居用品有限公司 | Preparation method of magnetic graphene oxide aerogel |
| CN115819000A (en) * | 2021-12-31 | 2023-03-21 | 南京诚赢集约建材科技有限公司 | Pilot test method based on mixed dispersion of asphalt regenerant and graphene |
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Application publication date: 20180629 |