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A high-efficiency purification method of water-dispersible carbon nanomaterials

A technology of carbon nanomaterials and purification methods, which is applied in the field of high-efficiency purification of water-dispersible carbon nanomaterials, and can solve problems such as inability to produce high yields

Active Publication Date: 2022-08-05
WUHAN UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

[0005] The invention provides a high-efficiency purification method of water-dispersible carbon nanomaterials. Aiming at the mixture of highly water-dispersible azo dye carbon nanomaterials obtained by ball milling, common low-cost and environmentally friendly inorganic salt / alkali aqueous solutions can be used to efficiently assist centrifugation Separation and purification of carbon nanomaterials without affecting their physical and chemical properties such as dispersibility and photoelectrochemical properties, thereby effectively overcoming the problem that simple centrifugation, dialysis and filtration cannot purify a mixture of azo dye ball-milled carbon nanomaterials with high yield and low cost. Paves the way for large-scale preparation of highly water-dispersible and surface-derivatizable carbon nanomaterials

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0022] Dissolve 3 mg of Congo red spheres in 1 mL of water, and after ultrasonic dispersion for 1 minute, the solution was transferred to a dialysis bag for dialysis for 24 hours. The aqueous solution outside the dialysis bag did not change color, but the dialysis bag adsorbed a lot of red, indicating that free Congo red molecules could not be removed by dialysis. .

Embodiment 2

[0024] Dissolve 4 mg of a ball-milled mixture of single-walled carbon nanotubes and Congo red with a mass ratio of 1:3 in 1 mL of water. After ultrasonic dispersion for 1 minute, centrifuge at 15,000 rpm for 10 minutes. The obtained solution has a black precipitate at the bottom, and the upper solution is still relatively clear. Deep black-red; in contrast, the upper solution was dark red after centrifugation of 3 mg / mL Congo red aqueous solution. This phenomenon shows that even with a higher centrifugal speed, some highly dispersed carbon nanotubes cannot be centrifuged, and this phenomenon is also applicable to the centrifugal separation of graphene nanosheets.

Embodiment 3

[0026] Fullerene C with a mass ratio of 1:3 60 4 mg of the ball-milled mixture with Congo red was dissolved in 1 mL of water, and after ultrasonic dispersion for 1 minute, the resulting solution was filtered and washed with a 0.1-micron pore size mixed cellulose filter until the filtrate had no obvious red color. During filtration, brown C on the filter can be observed 60 There was little solid residue, and the filtrate at the end of the filtration washing was light brown, indicating some high dispersibility of C 60 The filtrate enters the filtrate through the filtration membrane, and the loss in the filtration and washing process is large and the speed is very slow.

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Abstract

The invention provides a high-efficiency purification method for water-dispersible carbon nanomaterials. Dissolve the ball-milled mixture of carbon nanomaterials, water-soluble azo dye molecules and derivatized modified molecules with water, then mix it with the inorganic salt / alkali aqueous solution, and centrifuge at a centrifugal speed of 3,000 to 10,000 rpm for 1 to 30 minutes , suck out the upper dye aqueous solution, then add water to ultrasonically dissolve the bottom precipitate; repeat the above-mentioned salting-out-assisted centrifugation purification process until washing to obtain carbon nanomaterials dispersed in water. The outstanding feature of the present invention is: using common alkalis and salts as auxiliary sedimentation agents, the efficient separation of free dye molecules and water-dispersible carbon nanomaterials can be achieved in a short time and at a low centrifugal speed. The loss of nanomaterials is small, the purification reagent is environmentally friendly, and the cost is low, and the purification process has no effect on the physical and chemical properties of the carbon nanomaterials in terms of water dispersibility and optoelectronic properties.

Description

technical field [0001] The invention belongs to the field of material synthesis, and in particular relates to a high-efficiency purification method for water-dispersible carbon nanomaterials. Background technique [0002] Carbon nanomaterials represented by fullerenes, carbon nanotubes and graphene have unique physical and chemical properties such as structure, optoelectronics, and mechanics, and have led many revolutions in the field of materials science. It has broad application prospects in many fields such as medicine. However, a key factor limiting the large-scale application of these materials is how to achieve their efficient dispersion in various solvents, which is an important prerequisite for the construction of a large number of carbon-based functional materials, thin films and devices. Compared with organic solvents, water solvents have the characteristics of green environmental protection, low cost, and good biocompatibility. The preparation of carbon nanomater...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/174C01B32/17C01B32/196C01B32/194C01B32/198C01B32/156C01B21/082
CPCC01B32/174C01B32/17C01B32/196C01B32/194C01B32/198C01B32/156C01B21/0605
Inventor 胡成国杨佳
Owner WUHAN UNIV
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