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A kind of preparation method of stable graphene colloidal dispersion liquid

A technology of olefin colloid and dispersion liquid is applied in the field of graphene preparation to achieve the effects of small particles, simple and easy preparation process, and easy control of reaction process

Active Publication Date: 2016-01-20
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] In summary, there is no report on the use of dispersants to solve the problem of easy agglomeration of graphene oxide during the reduction process and thus to prepare stable graphene colloidal dispersions

Method used

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  • A kind of preparation method of stable graphene colloidal dispersion liquid
  • A kind of preparation method of stable graphene colloidal dispersion liquid
  • A kind of preparation method of stable graphene colloidal dispersion liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] A method for preparing graphene dispersion liquid includes the following process steps:

[0049] Combine 1g, 99.85% by weight of graphite powder and 23mL, 98% by weight of H 2 SO 4 Mix in a 250mL beaker and stir at room temperature for 24 hours; in a 40℃ water bath, add 100mg, 99.0wt% NaNO to the beaker 3 And stir for 5min to make it fully dissolved. Slowly add 1500mg, 99.5wt% KMnO to the cup 4 , After adding in about 20min, control the reaction temperature below 5℃ and stir for 30min. Add 3 mL of distilled water to the beaker, wait for 5 minutes, then add 3 mL of distilled water, wait for 5 minutes, add 40 mL of distilled water, and stir for 15 minutes. Stop the water bath, add 140mL distilled water and 10mL, 30wt% H into the beaker 2 O 2 Stir at room temperature for 5 min to terminate the reaction. Centrifuge at 10000r / min for 4min using a centrifuge, wash with 5wt% HCl, and repeat twice. Then use a centrifuge at 8000r / min for 4 minutes, and wash with distilled water t...

Embodiment 2

[0051] A method for preparing a stable graphene dispersion includes the following process steps:

[0052] The graphene in Example 1 was dissolved in 100 mL, 99.7% by weight of ethanol, 70kHz ultrasonic for 30min peeled and dispersed, centrifuged at 12000r / min for 5min, washed with distilled water for 2 to 3 times to wash away residual ethanol. The precipitate was dispersed in 100 mL of distilled water, sonicated at 70 kHz for 30 min, and centrifuged at 10000 r / min for 5 min. The resulting supernatant was a dispersion with a concentration of 0.20 mg / mL and about 12 wt% of single-layer graphene. The prepared graphene dispersion does not have obvious Tyndall effect, its zeta potential is -22.6mV, and the average particle size of graphene is 720.5nm.

Embodiment 3

[0054] A method for preparing a stable graphene colloidal dispersion liquid includes the following process steps:

[0055] The graphene in Example 1 was dissolved in 100mL, 99.7wt% ethanol with 4mg, 98wt% 1-naphthoic acid, 70kHz ultrasonic for 30min peeling and dispersion, centrifuged at 12000r / min for 5min, and washed with distilled water 2-3 times , Wash away residual 1-naphthoic acid and ethanol. The precipitate was dispersed in 100 mL of distilled water, sonicated at 70 kHz for 30 min, and centrifuged at 10000 r / min for 5 min. The resulting supernatant was a colloidal dispersion with a concentration of 0.25 mg / mL and about 25 wt% of single-layer graphene. The prepared stable graphene colloidal dispersion has the Tyndall effect, its zeta potential is -36.2mV, and the average particle size of graphene is 387.3nm.

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Abstract

The invention discloses a preparation method of stable graphene colloidal dispersion liquid, and relates to the technical field of graphene preparation. The stable graphene colloidal dispersion liquid can be obtained by preparing graphene oxide via an improved Hummer's method, reducing graphene oxide and then treating the product by using a dispersing agent. The concentration of the stable graphene colloidal dispersion liquid is 0.21-0.25mg / mL and the stable graphene colloidal dispersion liquid contains 14-25wt% of single-layer graphene. The graphene colloidal dispersion liquid has Tyndall effects and has zeta potential of minus 41-minus 33mV and mean grain size of 250-400nm. The method is simple and practicable, is easy in control of the reaction process, does not have special requirements for equipment, is lower in cost, is easy to popularize and can be widely applied to the fields of nanoelectronics, sensors, nanocomposites, batteries, supercapacitors, hydrogen storage materials and the like.

Description

Technical field [0001] The invention relates to the technical field of graphene preparation, in particular to the reduction of graphene oxide and a preparation method of a stable graphene colloidal dispersion. Background technique [0002] As a new type of two-dimensional carbon nanomaterial, graphene has attracted worldwide attention in recent years. The special nanostructure of graphene makes it have broad application prospects in fields such as nanoelectronics, sensors, nanocomposites, batteries, supercapacitors, and hydrogen storage materials. However, the lack of a controllable way to prepare graphene on a large scale has become a constraint to the effective development and application of its potential. Like carbon nanotubes and many other nanomaterials, the most critical challenge in the mass production of graphene comes from the agglomeration of graphene itself. In the case of insufficient dispersion, the high specific surface area of ​​graphene tends to form irreversibl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04C01B32/194
Inventor 李宏陈希元谢君樑黄进刘子睿
Owner WUHAN UNIV OF TECH
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