A kind of preparation method of ultrahigh specific surface area graphene airgel

A technology of graphene airgel and ultra-high specific surface area, which is applied in the field of preparation of graphene airgel, can solve the problems of insufficient increase of specific surface area of ​​graphene airgel and unfavorable performance of graphene, etc. Increased surface area, excellent high temperature stability, and ultra-high specific surface area

Active Publication Date: 2017-01-25
NAT UNIV OF DEFENSE TECH
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  • Abstract
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Problems solved by technology

At the same time, the activation process itself will have a certain impact on the chemical structure of graphene, causing more defects and vacancies on graphene, which will adversely affect some properties of graphene (aerogel).
[0006] In addition, methods to increase the specific surface area of ​​graphene aerogels also include the template method (that is, to prepare graphene aerogels with other large specific surface area materials as templates) and the introduction of polymerization inhibitors (that is, to prevent oxidation with certain compounds (graphene ) and other methods, but these methods are not as effective as the activation method for increasing the specific surface area of ​​graphene airgel, and the specific surface area of ​​the prepared graphene airgel is generally no more than 1200m 2 / g

Method used

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  • A kind of preparation method of ultrahigh specific surface area graphene airgel
  • A kind of preparation method of ultrahigh specific surface area graphene airgel
  • A kind of preparation method of ultrahigh specific surface area graphene airgel

Examples

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Embodiment 1

[0038] (1) 3g graphite powder is mixed with 15g potassium permanganate, 40ml concentrated phosphoric acid is mixed with 360ml concentrated sulfuric acid to obtain mixed acid, and gained mixed acid is added to gained graphite powder / In the mixture of potassium permanganate, heat up to 50°C, react for 12 hours under the condition of mechanical stirring at 300r / min, add the mixture obtained from the reaction into 400ml of ice water containing 10ml of 30% hydrogen peroxide, and centrifuge at a speed of 2000r / min to obtain centrifuged Dissolve the extract in 200ml of deionized water and centrifuge at a speed of 2000r / min for 1h, then dissolve the extract in 200ml of 30% hydrochloric acid and centrifuge at a speed of 2000r / min for 1h, and finally centrifuge The extract was dissolved in 200ml of ethanol and centrifuged at a speed of 2000r / min for 1h (3 times), and the extract was vacuum-dried at 50°C to obtain graphene oxide.

[0039] (2) Add 1g of the graphene oxide obtained in ste...

Embodiment 2～162

[0051] The process parameters used in Examples 2 to 162 are shown in Table 1, and the process is the same as in Example 1, except that the type of siloxane, the ratio of deionized water to graphene oxide, the ratio of siloxane to oxidized 4 parameters such as graphene dispersion ratio, pyrolysis temperature, except the process parameter written in the table, all the other process parameters are identical with embodiment 1.

[0052] Table 1 Example 2-162 preparation process parameters and properties of ultra-high specific surface area graphene airgel

[0053]

[0054]

[0055]

[0056]

[0057]

[0058]

[0059]

[0060]

[0061]

[0062]

Embodiment 163

[0064] The difference between embodiment 163 and embodiment 1 lies in the fourth step, and other process parameters are the same as embodiment 1. The fourth step of Example 163 is: replace the hybrid graphene gel obtained in step (3) with 10 times the volume of deionized water and ethanol for 10 times, each replacement time is 6h, to obtain the silicon oxide after solvent replacement hybrid graphene gel, and then put the silica hybrid graphene gel after solvent replacement into CO 2 In the drying kettle of the supercritical drying device, then the supercritical CO 2 , replaced for 5 hours, and finally released the pressure at a rate of 100KPa / min, and cooled with the furnace to obtain graphene airgel with ultra-high specific surface area.

[0065] The properties of the ultra-high specific surface area graphene airgel obtained in Example 163 are shown in Table 3.

[0066] In the fourth step, the volume of deionized water and ethanol, the number of replacements and the time ma...

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Abstract

The invention discloses a preparation method of graphene aerogel with an ultrahigh specific surface area, and aims to enlarge the specific surface area of graphene aerogel without affecting the chemical structure of graphene. The preparation method comprises the following steps: taking graphite powder and siloxane as the main raw materials, preparing oxidized graphene, preparing a dispersion liquid of oxidized graphene, preparing silicon oxide hybridized graphene gel, drying the gel, and finally carrying out high-temperature decomposition to obtain the graphene aerogel with an ultrahigh specific surface area. The raw materials are mixed in liquid, after reactions, silicon oxide nano particles with an extremely small particle size can be evenly dispersed, thus the graphene is dispersed, and the agglomeration is prohibited. Furthermore, high-temperature decomposition is performed to remove the silicon oxide, at the same time the high-temperature decomposition has a certain activating effect, thus the prepared graphene aerogel has an ultrahigh specific surface area, which can reach 2491 m<2> / g, and at the same time the chemical structure is barely influenced.

Description

technical field [0001] The invention relates to a preparation method of graphene airgel, in particular to a preparation method of graphene airgel with ultra-high specific surface area. [0002] technical background [0003] Graphene airgel is a three-dimensional porous structure material formed by overlapping graphene. This material has a series of characteristics such as ultra-light, high elasticity, large specific surface area, and high electrical and thermal conductivity. It is used in catalysis, electrochemistry, energy, Sensors, supercapacitors, adsorption, thermal control, and many other fields have great application potential. Reduced graphene oxide dispersion or aerogel is currently the most commonly used method for preparing graphene aerogel. This method has the characteristics of simple method, low cost and excellent performance. However, during the reduction process, (oxidized) graphene is easy to agglomerate, so the specific surface area of ​​the prepared graphen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04
Inventor 岳晨午冯坚姜勇刚冯军宗
Owner NAT UNIV OF DEFENSE TECH
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