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Method for preparing high-purity small oxidized graphene

A graphene, small-scale technology, applied in the direction of single-layer graphene, etc., can solve the problems of high cost, complex process and high toxicity

Inactive Publication Date: 2016-07-20
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The present invention mainly aims at the problems of low purity, high toxicity, complicated process and high cost in the existing preparation method of graphene oxide, and provides a preparation method of high-purity and small-size graphene oxide

Method used

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  • Method for preparing high-purity small oxidized graphene
  • Method for preparing high-purity small oxidized graphene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] First, place the aphanitic graphite in a 20% hydrofluoric acid solution (diluted with ethanol, that is, 40% HF and ethanol 1:1 to make a 20% HF solution), wash with hydrofluoric acid for 2 hours under stirring, and centrifuge. Use ethanol and water to wash and centrifuge, repeat several times until the pH is about 7, and dry at 80°C to obtain HF-purified aphanitic graphite. Add 0.6g of HF-purified aphanitic graphite and 3g of potassium permanganate Add 30mL concentrated sulfuric acid with a concentration of 98% to the lining of a 50mL polytetrafluoroethylene reactor and cool at 0°C for 12 hours. Cover, let stand at 0°C for 1.5h, then react in an oven at 90°C for 2h, after natural cooling, take out the polytetrafluoroethylene reactor from the stainless steel shell, and slowly pour the reaction mixture into 0.5L deionized In water, after stirring evenly, add 5mL aqueous hydrogen peroxide solution with a mass concentration of 25%, stir until the suspension is brownish yell...

Embodiment 2

[0024] The high-temperature melting method is mixed with a certain proportion of alkali, calcined at a high temperature of 400-600 ° C, washed to remove water-soluble substances, acid-washed to remove oxide impurities easily soluble in acid, and then washed and dried to obtain purified Aphanitic graphite, 6g of aphanitic graphite purified by high-temperature melting method, 60g of potassium ferrate were added to the lining of a 200ml polytetrafluoroethylene reactor and 150ml of concentrated phosphoric acid with a concentration of 85.5% were cooled at -2°C for 12h, After cooling, add concentrated phosphoric acid to the inner lining of the above-mentioned reaction kettle, place it in a stainless steel reaction kettle and cover it tightly, let it stand at 0°C for 4 hours, and then react in an oven at 90°C for 1 hour; after natural cooling, put the polytetrafluoroethylene Take out the ethylene reaction kettle from the stainless steel kettle shell, slowly pour the reaction mixture i...

Embodiment 3

[0027]Add 10g of aphanitic graphite purified by high-temperature melting method, 30g of potassium dichromate into the inner lining of 1000ml polytetrafluoroethylene reactor and 800ml of perchloric acid, respectively cool at -5°C for 24h, after cooling, add perchloric acid Put it into the lining of the above-mentioned reaction kettle, put it in a stainless steel reaction kettle and cover it tightly, let it stand at 0°C for 1h, and then react in an oven at 80°C for 4h; after natural cooling, remove the polytetrafluoroethylene reaction kettle from the stainless steel kettle Take out the shell, slowly pour the reaction mixture into 5L deionized water, stir evenly, add 50mL aqueous hydrogen peroxide solution with a mass concentration of 25%, stir until the suspension is brownish yellow or bright yellow, and dissolve the suspension solution, let it stand overnight, remove the supernatant, centrifuge, wash with 1M dilute hydrochloric acid for 5 times, and then wash with distilled wate...

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Abstract

The invention belongs to the technical field of oxidized graphene, and particularly relates to a method for preparing small oxidized graphene from cryptocrystalline graphite.The method mainly solves the problems of existing oxidized graphene preparing methods that purity is low, toxicity is high, technology is complicated and cost is high.According to the method, purified cryptocrystalline graphite, concentrated acid and strong oxidant are evenly mixed for reaction in an airtight environment at the temperature of 80-120 DEG C, a reaction mixture is slowly poured into an excessive amount of deionized water, uniform stirring is conducted, then an aqueous hydrogen peroxide solution with the mass concentration of 25% is added till turbid liquid becomes brown or luminous yellow, acid pickling and washing are conducted till pH value becomes 6-7, and then centrifugal separation is conducted to generate the small oxidized graphene.The ratio of the mass of purified cryptocrystalline graphite to the volume of concentrated acid is 1 : (20-80), and the mass ratio of purified cryptocrystalline graphite to purified cryptocrystalline graphite is 1 : (3-10).

Description

technical field [0001] The invention belongs to the technical field of graphene oxide, in particular to a method for preparing small-sized graphene oxide from aphanitic graphite. Background technique [0002] Graphene is a new type of carbonaceous material with the thickness of a single layer of carbon atoms, which is arranged in a two-dimensional honeycomb lattice structure. Graphene is made of carbon atoms with sp 2 The monoatomic carbon layer formed by hybridization has a very stable structure and has excellent mechanical properties, peculiar electrical properties and good thermal properties. Studies have found that the Young's modulus of graphene can reach 11000GPa, the fracture strength can reach 125GPa, and the thermal conductivity The rate is up to 5000W / (m·K), and the theoretical specific surface area is up to 2630m 2 / g, and has the properties of perfect quantum tunneling effect, half-integer quantum Hall effect and never-disappearing conductivity, and has good ap...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
CPCC01B2204/02C01P2002/72
Inventor 马灿良赵云李思殿
Owner SHANXI UNIV
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