Preparation method of graphene with nano ferroferric oxide precipitated on surface

Abstract

The invention belongs to the technical field of materials, and particularly relates to a preparation method of graphene with nano ferroferric oxide precipitated on surface, which concretely comprises the steps of: firstly, oxidizing natural flake graphite and obtaining graphite oxide; further carrying out ultrasonic stripping on the graphite oxide and forming graphene oxide suspension; then, carrying out reduction reaction on the graphene oxide suspension under the action of strong reducing agent, and obtaining black flocculent flake graphene; and finally, taking hydrogen peroxide as an oxidant, and depositing Fe3O4 on the surface of the graphene in an alkaline solution. The invention realizes the modification of nanoscale Fe3O4 for the surface of the graphene. The obtained modified graphene is not doped with other elements except the Fe element, and can be well dispersed in a high-performance resin matrix, so that the mechanical property, the thermal performance, the electromagnetic performance and the friction property of the resin matrix can be improved, and phenolic resin, bismaleimide, cyanate ester and other products can be updated, or a new application field can be developed..

Description

technical field

[0001] The invention belongs to the field of materials, relates to graphene, and in particular to a surface-precipitated nano-ferric oxide (Fe 3 o 4 ) The preparation method of graphene. Background technique

[0002] Graphene has excellent mechanical and electrical properties, and it has great potential application value in many fields. The preparation of graphene / polymer composite materials can improve the mechanical properties of polymers, prepare optical and electrical functional materials, high temperature resistant materials and friction materials, etc. At present, polymer / graphene composite materials have gradually become the main research and application direction of graphene. However, nanometer-scale graphene is insoluble in water and organic solvents, and is extremely prone to agglomeration, resulting in an unsatisfactory aggregation state in the final composite material, which makes it unable to give full play to its own advantages.

[0003] The...

Examples

Embodiment 1

[0026] (1) Preparation of graphite oxide

[0027] Weigh 2g of natural flake graphite and 1g of sodium nitrate, mix well; add concentrated H 2 SO 4 50ml, stirred under ice bath conditions, slowly added the mixture of graphite and sodium nitrate, slowly added 6g KMnO 4 , strictly control the temperature below 10°C, last about 0.5h, keep the temperature and continue to react for 2h; heat to 30°C, react for 3h, continue to slowly increase the temperature to 98°C, and slowly add H 2 O 100ml, keep the reaction at 100°C for about 2 hours, observe the color change; dilute the system with warm water, H 2 O dosage is about 150ml, add 15ml H 2 o 2 ; After the reaction, add a large amount of deionized water to dilute the product, and use 5% dilute hydrochloric acid to wash until the barium chloride solution cannot detect SO 4 2- Until then, it was repeatedly washed with deionized water until the pH value was neutral, and finally filtered and dried to obtain graphite oxide.

[0028...

Embodiment 2

[0033] (1) Preparation of graphite oxide

[0034] Add 30ml of concentrated sulfuric acid and 10ml of concentrated nitric acid into the three-neck flask, mechanically stir in ice-water bath for 20min to obtain mixed acid, take 2g of natural flake graphite and add it, after stirring for 15min, gradually add 6g of potassium chlorate powder slowly, and react for 72h. After the reaction, add a large amount of deionized water to dilute the product, wash with 5% dilute hydrochloric acid until the barium chloride solution cannot detect SO 4 2- Until then, it was repeatedly washed with deionized water until the pH value was neutral, and dried by suction to obtain graphite oxide.

[0035] (2) Graphene is prepared by reducing graphene oxide with zinc powder

[0036] Weigh graphite oxide 0.2g and H 2 O mixed with ultrasonic stripping to obtain 400ml of a suspension with a concentration of 0.5mg / ml, stirred evenly, added 1g of zinc powder, and ultrasonically reacted for 3h. After the re...

Embodiment 3

[0040] (1) Preparation of graphite oxide

[0041] Weigh 2g of natural flake graphite and 1g of sodium nitrate, mix well; add concentrated H 2 SO 4 50ml, stirred under ice bath, slowly added the mixture of graphite and sodium nitrate, slowly added 6g KMnO 4 , control the temperature below 10°C for about 2 hours, keep the temperature and continue the reaction for 5 hours; heat to 50°C in a water bath for 4 hours; continue to slowly raise the temperature to 90°C, and slowly add H 2 O 100ml, strictly control the temperature at 100°C, keep the reaction for about 5 hours, observe the color change; dilute the system with warm water, H 2 The amount of O is about 150ml, add 15ml of H 2 o 2 ; After the reaction, add a large amount of deionized water to dilute the product, and use 5% dilute hydrochloric acid to wash until the barium chloride solution cannot detect SO 4 2- Until then, it was repeatedly washed with deionized water until the pH value was neutral, and finally filtered...

technical field

[0001] The invention belongs to the field of materials, relates to graphene, and in particular to a surface-precipitated nano-ferric oxide (Fe 3 o 4 ) The preparation method of graphene. Background technique

[0002] Graphene has excellent mechanical and electrical properties, and it has great potential application value in many fields. The preparation of graphene / polymer composite materials can improve the mechanical properties of polymers, prepare optical and electrical functional materials, high temperature resistant materials and friction materials, etc. At present, polymer / graphene composite materials have gradually become the main research and application direction of graphene. However, nanometer-scale graphene is insoluble in water and organic solvents, and is extremely prone to agglomeration, resulting in an unsatisfactory aggregation state in the final composite material, which makes it unable to give full play to its own advantages.

[0003] The...

Examples

Embodiment 1

[0026] (1) Preparation of graphite oxide

[0027] Weigh 2g of natural flake graphite and 1g of sodium nitrate, mix well; add concentrated H 2 SO 4 50ml, stirred under ice bath conditions, slowly added the mixture of graphite and sodium nitrate, slowly added 6g KMnO 4 , strictly control the temperature below 10°C, last about 0.5h, keep the temperature and continue to react for 2h; heat to 30°C, react for 3h, continue to slowly increase the temperature to 98°C, and slowly add H 2 O 100ml, keep the reaction at 100°C for about 2 hours, observe the color change; dilute the system with warm water, H 2 O dosage is about 150ml, add 15ml H 2 o 2 ; After the reaction, add a large amount of deionized water to dilute the product, and use 5% dilute hydrochloric acid to wash until the barium chloride solution cannot detect SO 4 2- Until then, it was repeatedly washed with deionized water until the pH value was neutral, and finally filtered and dried to obtain graphite oxide.

[0028...

Embodiment 2

[0033] (1) Preparation of graphite oxide

[0034] Add 30ml of concentrated sulfuric acid and 10ml of concentrated nitric acid into the three-neck flask, mechanically stir in ice-water bath for 20min to obtain mixed acid, take 2g of natural flake graphite and add it, after stirring for 15min, gradually add 6g of potassium chlorate powder slowly, and react for 72h. After the reaction, add a large amount of deionized water to dilute the product, wash with 5% dilute hydrochloric acid until the barium chloride solution cannot detect SO 4 2- Until then, it was repeatedly washed with deionized water until the pH value was neutral, and dried by suction to obtain graphite oxide.

[0035] (2) Graphene is prepared by reducing graphene oxide with zinc powder

[0036] Weigh graphite oxide 0.2g and H 2 O mixed with ultrasonic stripping to obtain 400ml of a suspension with a concentration of 0.5mg / ml, stirred evenly, added 1g of zinc powder, and ultrasonically reacted for 3h. After the re...

Embodiment 3

[0040] (1) Preparation of graphite oxide

[0041] Weigh 2g of natural flake graphite and 1g of sodium nitrate, mix well; add concentrated H 2 SO 4 50ml, stirred under ice bath, slowly added the mixture of graphite and sodium nitrate, slowly added 6g KMnO 4 , control the temperature below 10°C for about 2 hours, keep the temperature and continue the reaction for 5 hours; heat to 50°C in a water bath for 4 hours; continue to slowly raise the temperature to 90°C, and slowly add H 2 O 100ml, strictly control the temperature at 100°C, keep the reaction for about 5 hours, observe the color change; dilute the system with warm water, H 2 The amount of O is about 150ml, add 15ml of H 2 o 2 ; After the reaction, add a large amount of deionized water to dilute the product, and use 5% dilute hydrochloric acid to wash until the barium chloride solution cannot detect SO 4 2- Until then, it was repeatedly washed with deionized water until the pH value was neutral, and finally filtered...

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