Preparation method of graphene oxide

A technology of graphene and rock oxide, which is applied in the field of preparing graphene oxide, to achieve the effects of reducing production costs, reducing waste acid and waste liquid, and controlling the degree of oxidation

Active Publication Date: 2016-02-24
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The idea of ​​the present invention is to prepare graphene oxide by heating and oxidizing graphite raw materials under the action of alkaline solution, oxygen at a certain pressure, and a pro-oxidant, so as to overcome the defects in the oxidation stage of graphene prepared by redox method, and the oxidation degree of this method is controllable , has little damage to the graphite structure, and is an environmentally friendly synthesis route. The lye produced can be recycled after treatment, with low cost and simple method, which effectively avoids the problems of waste acid and separation difficulties in the strong acid oxidation process.

Method used

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  • Preparation method of graphene oxide

Examples

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Embodiment 1

[0017] This embodiment illustrates that the graphite is 325 meshes of natural flake graphite, the alkali is KOH, and the pro-oxidant is KNO 3 reaction process and results.

[0018] Take 3g325 mesh natural flake graphite, 12gKOH, 3gKNO 3 , put into a reaction kettle, add 25ml of deionized water, and stir for 10min. After the reactor was sealed, the gas in the reactor was replaced with oxygen three times, and then filled with oxygen to 5Mpa, the reactor was heated to 450°C, and the reaction was stirred for 36 hours. After the reaction was completed, cool to room temperature, and the reactant was separated from solid and liquid. The solid product was first washed with 5% dilute hydrochloric acid, then washed with deionized water until neutral, and dried at 100°C to obtain 2.752 g of graphene oxide solid. The liquid phase is recovered, and after the concentration of the solution alkali is adjusted according to the concentration of the KOH solution before the reaction, it is recy...

Embodiment 2

[0020] This embodiment illustrates that the graphite is 325 meshes of natural flake graphite, the alkali is KOH, and the pro-oxidant is KNO 3 reaction process and results.

[0021] With 13mL of lye recovered in Example 1, add 6.25gKOH and 17mL deionized water to adjust to the same concentration according to the concentration of KOH measured before the reactor of Example 1 was sealed, and get 3g325 mesh natural flake graphite, 3gKNO 3 , put it into the reaction kettle, add 25ml circulating lye, and stir for 10min. After the reactor was sealed, the gas in the reactor was replaced with oxygen three times, and then the reactor was heated to 600° C. with 3 Mpa of oxygen, and the reaction was stirred for 36 hours. After the reaction was completed, it was cooled to room temperature, the reactant was separated from solid and liquid, and the solid product was washed with 5% dilute hydrochloric acid, then washed with deionized water until neutral, and dried at 100°C to obtain 2.804 g o...

Embodiment 3

[0023] This embodiment illustrates that the graphite is 325 meshes of natural flake graphite, the alkali is NaOH, and the pro-oxidant is NaNO 3 reaction process and results.

[0024] Take 5g325 mesh natural flake graphite, 12gNaOH, 3gNaNO 3 , put into a reaction kettle, add 25ml of deionized water, and stir for 10min. After the reactor was sealed, the gas in the reactor was replaced with oxygen three times, and then the reactor was heated to 450° C. with 5 Mpa of oxygen, and the reaction time was stirred for 36 hours. After the reaction was completed, cool to room temperature, the reactants were separated into solid and liquid, and the solid was washed with 10% dilute hydrochloric acid, then washed with deionized water until neutral, and dried at 100°C to obtain 4.763 g of graphene oxide solid. The liquid phase is recovered, and after the concentration of the solution alkali is adjusted according to the concentration of the NaOH solution before the reaction, it is recycled a...

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Abstract

The invention relates to a preparation method of graphene oxide. The method comprises the steps of adding a graphite raw material and a pro-oxidant into aqueous alkali and placing in a sealed container, wherein 1 to 50g of graphite raw material and 1 to 30g of pro-oxidant are added into every 100ml of aqueous alkali; displacing gas in the container with oxygen and charging the oxygen till the pressure is 1 to 20 Mpa, reacting at the temperature of 101 DEG C to 650 DEG C, taking a reacted product out after the reaction is finished, performing solid-liquid separation, washing an obtained solid phase and drying, so as to obtain a graphene oxide solid product, and a liquid phase is recycled and is reused after being treated. By adopting the preparation method, the large dosages of strong acid and strong oxidant can be avoided in the reaction, waste acid and waste liquid are reduced, the extent of the reaction can be adjusted by controlling the reaction temperature and the oxygenating pressure, the structural damage loss of the graphene oxide prepared in a strong acidic condition is effectively avoided, and the tedious separation and washing processes for preparing the graphene oxide are simplified. The aqueous alkali is recyclable, so that the production cost is effectively reduced, the process is simple, the flow is short, and the cost is low.

Description

technical field [0001] The invention relates to a method for preparing graphene oxide. Background technique [0002] Graphene oxide (GO) is an important intermediate for preparing graphene by redox method. In 2004, Andre Geim and Konstantin Novoselov, physicists at the University of Manchester in the United Kingdom, successfully separated single-layer graphene from graphite, confirmed that it can exist alone and discovered the integer quantum Hall effect. And the quantum Hall effect under normal temperature conditions, the two detonated the research on graphene after they jointly won the 2010 Nobel Prize in Physics. The breaking strength of graphene is 200 times that of steel, and it has good elasticity, and the stretching range can reach 20% of its own size. Graphene has great potential to become a substitute for silicon, manufacture ultra-miniature transistors, and be used to produce future supercomputers. The speed of computer processors will increase hundreds of times....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 李福祥薛达
Owner TAIYUAN UNIV OF TECH
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