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Preparation method of graphene airgel based on emulsion method

A graphene aerogel, emulsion method, applied in the field of materials, can solve the problems of inability to control porosity, high toxicity of aromatic hydrocarbons, harsh operating conditions, etc., and achieve good lateral and vertical extrusion resilience, accurate porosity Control, effect of good mechanical strength

Active Publication Date: 2019-06-14
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the following problems still exist in the preparation of graphene aerogels: (1) high-pressure and high-temperature reactions in hydrothermal kettles or special technical means are required; (2) the extrusion resilience of graphene aerogels is not good, Most of them are characterized by longitudinal extrusion resilience and poor transverse extrusion resilience; (3) It is impossible to simply and effectively control the pore structure and porosity of graphene airgel, and to achieve accurate control of porosity within a certain range, Generally require harsh operating conditions, such as low temperature conditions
However, in the prior art, the Pickering emulsion in which graphene oxide is a stabilizer has the following problems: (1) Aromatic hydrocarbons are usually used as the oil phase. Due to the high toxicity of aromatic hydrocarbons, many problems will arise in practical applications; High concentrations of aromatic hydrocarbons can cause acute poisoning, anesthetize the central nervous system, and even endanger life; low concentrations of aromatic hydrocarbons can cause chronic poisoning, which can cause great damage to the nervous system and blood system of the human body, and even induce leukemia and cancer.
(2) The stability of the system is not enough; this is due to the strong hydrophilicity of graphene oxide, the emulsified volume obtained during the emulsion preparation process is small, and after a certain period of time, the emulsion droplets appear to merge and even demulsify.
Currently, there is no research report on the preparation of graphene aerogels using Pickering emulsions.

Method used

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  • Preparation method of graphene airgel based on emulsion method
  • Preparation method of graphene airgel based on emulsion method
  • Preparation method of graphene airgel based on emulsion method

Examples

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Embodiment 1

[0030]Utilize improved Hummers method to prepare graphite oxide: graphite powder 2g, 98% sulfuric acid 92ml, sodium nitrate 2g, add to 500ml round bottom flask, stir at 0~10 ℃ for 2 hours, slowly add potassium permanganate 12g at the same time, heat up to 35 ℃, continue to stir for 1 hour, add 160ml deionized water and raise the temperature to 95℃, react for 30 minutes, add 10ml 30% hydrogen peroxide to remove excess potassium permanganate. Dialysis for one week, freeze-drying to obtain graphite oxide powder.

[0031] The preparation method of the graphene airgel based on emulsion method comprises the following steps:

[0032] (1) Prepare graphene oxide solution: take 0.3g graphite oxide prepared by Hummers method, and ultrasonically disperse it in 100g water for 1h, thereby obtaining graphene oxide aqueous solution;

[0033] (2) Preparation of Pickering emulsion: add 0.9g ascorbic acid and 0.5g sodium chloride to the graphene oxide aqueous solution obtained in step (1); add ...

Embodiment 2

[0036] Different from Example 1, the preparation method based on the graphene airgel of emulsion method may further comprise the steps:

[0037] (1) Preparation of graphene oxide solution: Weigh 0.6g of prepared graphite oxide, and ultrasonically disperse it in 100g of water for 2h, thereby obtaining a graphene oxide aqueous solution;

[0038] (2) Preparation of Pickering emulsion: add 1.8g ascorbic acid and 1.0g potassium chloride to the graphene oxide aqueous solution obtained in step (1); add nitric acid to adjust pH=3, add 25ml soybean oil, and adopt a stirring rate of 16000r / min Stir for 3 minutes until evenly stirred to obtain a stable homogeneous Pickering emulsion;

[0039] (3) Preparation of graphene airgel: the Pickering emulsion prepared in step (2) was subjected to a hydrothermal reaction at a temperature of 90° C., the reaction time was 5 hours, and the graphene hydrogel was obtained after the reaction; the graphene Put the hydrogel into a container with built-in...

Embodiment 3

[0041] Different from Example 1, the preparation method based on the graphene airgel of emulsion method may further comprise the steps:

[0042] (1) Preparation of graphene oxide solution: Weigh 1 g of prepared graphite oxide, and disperse it in 100 g of water by ultrasonication for 0.5 h, thereby obtaining a graphene oxide aqueous solution;

[0043] (2) Prepare Pickering emulsion: 5.0g ascorbic acid and 1.5g magnesium chloride are added in the graphene oxide aqueous solution that step (1) obtains; Add hydrochloric acid and adjust pH=1, add 50ml rapeseed oil, adopt the stirring speed of 2000r / min to stir Stir for 5 minutes until evenly to obtain a stable homogeneous Pickering emulsion;

[0044] (3) Preparation of graphene airgel: the Pickering emulsion prepared in step (2) was subjected to a hydrothermal reaction at a temperature of 50° C., the reaction time was 20 hours, and the graphene hydrogel was obtained after the reaction; the graphene Put the hydrogel into a container...

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Abstract

The invention provides a preparation method for assembling a gel under hydrothermal conditions by using graphene Pickering emulsion as a soft template. The Pickering emulsion of the present invention consists of the following components: in parts by weight, 0.3 to 1 part of graphite oxide, 0 to 1.84 parts of salt, 0.00365 to 0.63 parts of acid, 0.9 to 5 parts of ascorbic acid, 100 parts of water and 0.2 parts of ~1 volume of vegetable oil in water. The preparation method of the present invention does not require complicated operating conditions and strong corrosive substances, can realize accurate porosity control, and can realize large-scale preparation; at the same time, the graphene airgel prepared by the present invention has good lateral and longitudinal extrusion Resilience performance, the pore structure remains open, and it has excellent adsorption capacity for petroleum products, and has broad application prospects.

Description

technical field [0001] The invention belongs to the field of materials, in particular to the preparation of graphene airgel, in particular to a method for preparing graphene airgel based on an emulsion method. Background technique [0002] Graphene airgel is a graphene three-dimensional material obtained through special operations using graphene oxide as a raw material. Three-dimensional graphene airgel has superior surface area, abundant pore volume, and ultra-low density, and has broad research prospects and application value in supercapacitors, catalyst supports, and environmental protection. The developed pore structure inside graphene airgel makes it have superior organic solvent adsorption capacity, generally up to hundreds of times its own weight. The adsorption of organic solvents by graphene airgel is mainly physical adsorption, and its pore structure and extrusion resilience will affect the adsorption rate, adsorption capacity, and recycling. [0003] Based on th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/184
CPCC01P2004/03C01P2006/10C01P2006/14
Inventor 刘会娥黄扬帆陈爽马雁冰王振有丁传芹
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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