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Preparation method for preparing graphene dispersion liquid by electrochemical swelling

A graphene dispersion, electrochemical technology, applied in graphene, nano-carbon and other directions, can solve the problems of long electrolysis time, inability to effectively improve the graphene monolayer rate, uncontrollable graphene sheet layers and thickness, etc. Achieve the effect of speeding up dispersion, reducing the difficulty of peeling, and improving the single-layer rate

Inactive Publication Date: 2019-04-02
厦门十一维科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this technical solution takes a long time for electrolysis each time, and the number and thickness of the graphene sheets of the obtained composite material cannot be controlled, and the graphene monolayer rate cannot be effectively improved.

Method used

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  • Preparation method for preparing graphene dispersion liquid by electrochemical swelling
  • Preparation method for preparing graphene dispersion liquid by electrochemical swelling
  • Preparation method for preparing graphene dispersion liquid by electrochemical swelling

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Use a double-electrode electrochemical cell for intercalation reaction, take 40mL of tetraethylammonium bromide / acetonitrile solution with a concentration of 8mg / mL as the electrolyte, fix 1.0g of graphite sheets on the copper wires with conductive copper strips, and apply 12V Voltage for electrolysis reaction for 1.0h, rinsed with 0.2mol / mL PVP / DMF solution for 0.5h, ultrasonicated the rinsed graphene solution for 5min, and then centrifuged the dispersion at 1000rpm / min for 0.5h , and then washed twice with isopropanol IPA to remove the PVP in the solution. The graphene dispersion was centrifuged again for 3 min at a centrifugation speed of 1000 rpm / min, and then the precipitate IPA was removed from the graphene solution to obtain a graphene dispersion.

[0032] The entire process of the method takes about 2.5 hours, which is at least 58 hours shorter than the traditional method, and greatly improves the dispersion efficiency of the graphene nanosheets. Characterize t...

Embodiment 2

[0034] A two-electrode electrochemical cell was used for intercalation reaction, and 40 mL of tetrapropylammonium bromide / acetonitrile solution with a concentration of 5 mg / mL was used as the electrolyte, and 2.0 g of graphene nanosheets were respectively fixed on copper wires with conductive copper strips. Apply a voltage of 5V to carry out the electrolysis reaction for 0.5h, rinse with 0.1mol / mL PVP / DMF solution for 0.5h, and ultrasonicate the rinsed graphene solution for 5min, then centrifuge the dispersion at a centrifugal speed of 1000rpm / min for 0.5 After h, wash twice with isopropanol IPA to remove PVP in the solution. The graphene dispersion was centrifuged again for 2 min at a centrifugation speed of 1000 rpm / min, and then the precipitate IPA was removed from the graphene solution to obtain a graphene dispersion.

[0035] The entire process of this method takes about 2.5 hours, which is the same as that of Example 1, and shortens nearly 58 hours compared to the tradit...

Embodiment 3

[0037] A two-electrode electrochemical cell is used for intercalation reaction. Take 40mL of electrolyte, the concentration of tetrabutylammonium bromide in the acetonitrile solution is 5mg / mL, and the concentration of tetradecylammonium bromide is 5mg / mL. Graphene nanosheets were fixed on copper wires, applied a voltage of 15V for electrolysis for 2.5h, rinsed with 0.5mol / mL PVP / DMF solution for 1.0h, ultrasonicated the rinsed graphene solution for 10min, and then centrifuged After the dispersion was centrifuged at 1000 rpm / min for 1.0 h, it was washed twice with isopropanol IPA to remove PVP in the solution. The graphene dispersion was centrifuged again for 5 min at a centrifugation speed of 1000 rpm / min, and then the precipitate IPA was removed from the graphene solution to obtain a graphene dispersion.

[0038] The entire process of this method takes about 3.5 hours, which is also shortened by nearly 58 hours compared with the traditional method, and greatly improves the d...

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Abstract

The invention belongs to the field of material preparation, and relates to a preparation method for preparing a graphene dispersion liquid by electrochemical swelling. The method comprises the following steps: (1) taking graphite sheets as a cathode and taking a graphite substrate as a cathode to carry out electrolysis on the electrodes in an electrolytic tank, wherein the electrolyte is an acetonitrile solution dissolved with a quaternary ammonium salt, and the concentration of the quaternary ammonium salt is 5-10 mg / mL; (2) rinsing the cathode by using a rinsing solution containing a dispersing agent, carrying out ultrasonic stripping on the solution subjected to rinsing to form a dispersion, then centrifuging the dispersion, washing the dispersion by using isopropyl alcohol to remove the excess dispersing agent; and (3) separating solid impurities to obtain the graphene dispersion liquid. According to the method, the graphene nanosheets are swelled and dispersed through an electrochemical method, quaternary ammonium salt cations are inserted into interlayers of the graphene, and then interlayer expansion is achieved, and preparation efficiency of the graphene dispersion liquid is improved.

Description

technical field [0001] The invention belongs to the field of material preparation, and in particular relates to a preparation method for preparing a graphene dispersion liquid by electrochemical swelling. Background technique [0002] Graphene materials are often added to polymer materials, metal materials or inorganic non-metallic materials as modifying additives to modify the matrix material through the excellent optical, electrical or mechanical properties of graphene. However, two-dimensional graphene cannot exist alone and needs to rely on a carrier. Therefore, the two-dimensional graphene materials used as additives all need to use graphene nanosheets as raw materials and obtain them by dispersing with a dispersant. Because two-dimensional graphene is easy to agglomerate, the dispersion effect and efficiency are very low. At present, the dispersion of graphene in the industry is mostly obtained by putting it into a dispersant, and then obtaining it through ultrasonic v...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/19
CPCC01B32/19
Inventor 田博王洪炜姜小川李俊竺董豪聪
Owner 厦门十一维科技有限公司
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