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A method for preparing graphene oxide by electrocatalytic oxidation

A technology of electrocatalytic oxidation and fossilization, applied in the direction of electrolysis process, electrolysis components, etc., can solve the problems of production restriction and large-scale application, and achieve the effects of shortening the production cycle, low cost, and small structural damage

Active Publication Date: 2016-11-30
QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the yield problem has restricted the large-scale application of this method.

Method used

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  • A method for preparing graphene oxide by electrocatalytic oxidation
  • A method for preparing graphene oxide by electrocatalytic oxidation
  • A method for preparing graphene oxide by electrocatalytic oxidation

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Experimental program
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Effect test

Embodiment 1

[0035] Graphene oxide was obtained by electrolyzing spectroscopically pure graphite rods in an electrolyte solution containing 0.9 mol / L sodium chloride and 0.65 mol / L sodium sulfate at a voltage of 13 V and at a temperature of 29°C for 5 hours.

[0036] Adopt routine test method to test the graphene oxide that obtains, the result is as follows figure 2 and image 3 shown by figure 2 It can be seen from the Raman diagram that there are more obvious D peaks and 2D peaks in the exfoliated graphite oxide. The appearance of the 2D peak shows the existence of single-layer graphene in the product. In addition, the ratio of the D peak to the G peak is 0.33, which is much smaller than the ratio of the chemically synthesized graphite oxide (about 0.9). It proves that the structure of graphite oxide prepared by electrocatalysis is less damaged. Depend on image 3 The micro-area detection shows that the carbon-oxygen ratio of graphite oxide is about 3.8, which proves that graphite ...

Embodiment 2

[0039]Graphene oxide was obtained by electrolyzing spectroscopically pure graphite rods in an electrolyte solution containing 0.6 mol / L sodium chloride and 0.4 mol / L sodium sulfate, with a voltage of 20V and a temperature controlled at 35°C for 6 hours.

[0040] Adopt routine test method to test the graphene oxide that obtains, the result is as follows Figure 5 and Image 6 shown by Figure 5 It can be seen from the Raman diagram in , that there are also obvious D peaks and 2D peaks in the exfoliated graphite oxide. The ratio of D peak to G peak is 0.52, which is also smaller than the ratio (about 0.9) of graphite oxide synthesized by chemical method. It also proves that the graphite oxide prepared by electrocatalysis has a small degree of structural damage. Depend on Image 6 It can be seen from the micro-area detection that the carbon-to-oxygen ratio of graphite oxide can be obtained to be about 3.7, which proves that graphite has been oxidized to a certain extent.

[...

Embodiment 3

[0043] Graphene oxide was obtained by electrolyzing spectroscopically pure graphite rods in an electrolyte solution containing 1.2 mol / L sodium chloride and 0.8 mol / L sodium sulfate at a voltage of 15 V and at a temperature of 25 °C for 4 hours.

[0044] Adopt routine test method to test the graphene oxide that obtains, the result is as follows Figure 8 shown by Figure 8 It can be seen from the Raman diagram in , that there are also obvious D peaks and 2D peaks in the exfoliated graphite oxide. The ratio of D peak to G peak is 0.14, which is much smaller than that of chemically synthesized graphite oxide (about 0.9). It proves that the structure of graphite oxide prepared by electrocatalysis is less damaged. Graphene oxide was characterized by infrared spectroscopy, the results are as follows Figure 9 As shown, obvious oxygen-containing functional groups appeared in the infrared spectrum, which have been marked in detail in the infrared spectrum.

[0045] Graphene oxide...

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Abstract

The invention discloses a method for preparing graphene oxide through electrocatalytic oxidation. The method comprises the following steps: electrolyzing a graphite rod with a pure spectrum in electrolyte for 4-6 hours at the electrolysis voltage of 15+ / -5V and the electrolysis temperature of 30+ / -5 DEG C, and after the electrolysis is completed, peeling off the graphite rod, thereby obtaining the graphene oxide, wherein the electrolyte contains 0.4-0.8mol / L sulfate ions and 0.6-1.2mol / L chloride ions or hypochlorite ions. On the basis of electrochemical peeling, raw materials which are cheap and easy to obtain are adopted to prepare the electrolyte for peeling off the graphene oxide, and thus the method has the advantages of one-step synthesis, no pollution, simple operation and the like.

Description

technical field [0001] The invention belongs to the technical field of material preparation, in particular, the invention relates to a method for preparing graphene oxide by electrocatalytic oxidation. Background technique [0002] Graphene has unique physical properties and unparalleled electrical conductivity, which leads to its application in some fields as a substitute for some materials. Therefore, in recent years, it has attracted extensive attention of researchers in many fields such as material science, physics and chemistry, energy storage, and high-performance hybrid field emission. [0003] In 1959, Hummers et al. (Hummers, W.S.; Offeman, R.E., Preparation of GraphiticOxide. Journal of the American Chemical Society 1958, 80(6), 1339-1339.) added sodium nitrate and permanganate to graphite in a sulfuric acid environment. Oxidation of potassium, successfully prepared graphite oxide, this method is one of the most basic methods of chemical synthesis of graphite for ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B1/00
CPCC25B1/00
Inventor 房春晖杨子祥房艳周永全朱发岩
Owner QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI
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