Preparation method of aminated graphene oxide

Abstract

The invention relates to a preparation method of aminated graphene oxide, which solves the technical problem of different sizes of material lamellas prepared by the existing preparation method, and comprises the following steps: weighing graphite flakes, and preparing graphene oxide dispersion liquid from the graphite flakes by an improved Hummers method; performing cell disruptor treatment and ultrasonic treatment on the obtained graphene oxide dispersion liquid, and performing freeze drying to obtain graphene oxide powder; adding the obtained graphene oxide powder into an organic solvent, carrying out ultrasonic treatment, and then adding a small molecular amine compound and a dehydration condensing agent for treatment; and carrying out centrifugation and suction filtration on the reaction product through a centrifuge to obtain aminated graphene oxide dispersion liquid with different lamellar sizes, and carrying out freeze drying to obtain aminated graphene oxide powder. The preparation method can be used for preparing aminated graphene oxide.

Description

technical field

[0001] The invention relates to a preparation method of a graphite material, in particular to a preparation method of aminated graphene oxide. Background technique

[0002] Graphene is a two-dimensional monolayer composed of carbon atoms arranged in a hexagonal structure with sp2 hybrid orbitals. This unique structural feature of graphene makes it have good permeability to visible light and has very high electrical and thermal conductivity. At the same time, its mechanical properties are also exceptionally good, and it is also the lightest and thinnest material known. However, in practical applications, graphene is expensive and difficult to produce on a large scale. However, in order to meet the needs of a wider range of applications, the functional modification of graphene is particularly important. In the process of preparing graphene, a derivative called graphene oxide is produced. Pristine graphene or graphene oxide is not suitable for the preparation ...

Examples

Embodiment 1

[0025] The selected graphite flakes in this embodiment are 300 meshes, and the selected small molecule amine is triethylenetetramine.

[0026] The present embodiment prepares a large sheet of aminated graphene oxide from the above raw materials, and its specific steps are as follows:

[0027] Weigh 5g of 300 mesh graphite flakes, and obtain a graphene oxide dispersion by improving the Hummers method and dialysis with deionized water. The improved Hummers method is as follows: add 2.5g sodium nitrate and 120ml concentrated sulfuric acid to 5g flake graphite, then add 15g potassium permanganate, after 2 days of reaction, take a mixed solvent of 30ml hydrogen peroxide and 300ml deionized water, slowly add the reacted system until no gas is released. Then, through deionized water dialysis and ultrasound, two kinds of graphene oxide dispersions were obtained.

[0028] The obtained graphene oxide dispersion was processed by a cell disruptor in an ice-water bath for 15 minutes, fol...

Embodiment 2

[0033] The selected graphite flakes in this embodiment are 300 meshes, and the selected small molecule amine is triethylenetetramine.

[0034] The present embodiment prepares a kind of larger lamellar aminated graphene oxide from the above raw materials, and its specific steps are as follows:

[0035]Weigh 5g of 300-mesh graphite flakes, and obtain a graphene oxide dispersion by improving the Hummers method and dialysis with deionized water. The graphene oxide dispersion is treated by a cell disruptor in an ice-water bath for 45 minutes, followed by ultrasonication for 2 hours. After freeze-drying, graphene oxide powder is obtained. First, 1g of graphene oxide powder and 200ml of DMSO were added to the beaker, followed by 5g of triethylenetetramine and 1g of diisopropylcarbodiimide. After condensing and refluxing at 120°C for 12 hours, adding ethanol to make it layered, centrifuging at a speed of 8000rpm / min for 5 minutes, and freeze-drying the supernatant to obtain a large l...

Embodiment 3

[0040] The selected graphite flakes in this embodiment are 3000 meshes, and the selected small molecule amine is triethylenetetramine (TETA).

[0041] The present embodiment prepares a kind of smaller lamellar aminated graphene oxide from above raw material, and its specific steps are as follows:

[0042] Weigh 5g of 3000-mesh graphite flakes, and obtain a graphene oxide dispersion by improving the Hummers method and dialysis with deionized water. The graphene oxide dispersion is treated by a cell disruptor in an ice-water bath for 20 minutes, followed by ultrasonication for 2 hours. After freeze-drying, graphene oxide powder is obtained. First 1g graphene oxide powder and 200ml THF are added in the beaker, followed by adding TETA5g and N-N'-dicyclohexylcarboimide 1g. After condensing and reflux for 24 hours at 120°C, add ethanol to make it layered, centrifuge at a speed of 8000rpm / min for 10min, and then freeze-dry the supernatant to obtain medium-layer triethylenetetramine-...

technical field

[0001] The invention relates to a preparation method of a graphite material, in particular to a preparation method of aminated graphene oxide. Background technique

[0002] Graphene is a two-dimensional monolayer composed of carbon atoms arranged in a hexagonal structure with sp2 hybrid orbitals. This unique structural feature of graphene makes it have good permeability to visible light and has very high electrical and thermal conductivity. At the same time, its mechanical properties are also exceptionally good, and it is also the lightest and thinnest material known. However, in practical applications, graphene is expensive and difficult to produce on a large scale. However, in order to meet the needs of a wider range of applications, the functional modification of graphene is particularly important. In the process of preparing graphene, a derivative called graphene oxide is produced. Pristine graphene or graphene oxide is not suitable for the preparation ...

Examples

Embodiment 1

[0025] The selected graphite flakes in this embodiment are 300 meshes, and the selected small molecule amine is triethylenetetramine.

[0026] The present embodiment prepares a large sheet of aminated graphene oxide from the above raw materials, and its specific steps are as follows:

[0027] Weigh 5g of 300 mesh graphite flakes, and obtain a graphene oxide dispersion by improving the Hummers method and dialysis with deionized water. The improved Hummers method is as follows: add 2.5g sodium nitrate and 120ml concentrated sulfuric acid to 5g flake graphite, then add 15g potassium permanganate, after 2 days of reaction, take a mixed solvent of 30ml hydrogen peroxide and 300ml deionized water, slowly add the reacted system until no gas is released. Then, through deionized water dialysis and ultrasound, two kinds of graphene oxide dispersions were obtained.

[0028] The obtained graphene oxide dispersion was processed by a cell disruptor in an ice-water bath for 15 minutes, fol...

Embodiment 2

[0033] The selected graphite flakes in this embodiment are 300 meshes, and the selected small molecule amine is triethylenetetramine.

[0034] The present embodiment prepares a kind of larger lamellar aminated graphene oxide from the above raw materials, and its specific steps are as follows:

[0035]Weigh 5g of 300-mesh graphite flakes, and obtain a graphene oxide dispersion by improving the Hummers method and dialysis with deionized water. The graphene oxide dispersion is treated by a cell disruptor in an ice-water bath for 45 minutes, followed by ultrasonication for 2 hours. After freeze-drying, graphene oxide powder is obtained. First, 1g of graphene oxide powder and 200ml of DMSO were added to the beaker, followed by 5g of triethylenetetramine and 1g of diisopropylcarbodiimide. After condensing and refluxing at 120°C for 12 hours, adding ethanol to make it layered, centrifuging at a speed of 8000rpm / min for 5 minutes, and freeze-drying the supernatant to obtain a large l...

Embodiment 3

[0040] The selected graphite flakes in this embodiment are 3000 meshes, and the selected small molecule amine is triethylenetetramine (TETA).

[0041] The present embodiment prepares a kind of smaller lamellar aminated graphene oxide from above raw material, and its specific steps are as follows:

[0042] Weigh 5g of 3000-mesh graphite flakes, and obtain a graphene oxide dispersion by improving the Hummers method and dialysis with deionized water. The graphene oxide dispersion is treated by a cell disruptor in an ice-water bath for 20 minutes, followed by ultrasonication for 2 hours. After freeze-drying, graphene oxide powder is obtained. First 1g graphene oxide powder and 200ml THF are added in the beaker, followed by adding TETA5g and N-N'-dicyclohexylcarboimide 1g. After condensing and reflux for 24 hours at 120°C, add ethanol to make it layered, centrifuge at a speed of 8000rpm / min for 10min, and then freeze-dry the supernatant to obtain medium-layer triethylenetetramine-...

Images