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Method for preparing graphene oxide based on high-concentration inorganic saline solution stripping

An inorganic salt solution and high-concentration technology, applied in the direction of inorganic chemistry, chemical instruments and methods, carbon compounds, etc., can solve the problems that hinder the mass production of graphene oxide, waste of water resources and energy, and non-recyclable utilization, etc., to achieve the realization of intercalation Effects of layers and puffing, change destruction, short preparation cycle

Inactive Publication Date: 2019-10-22
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

However, the preparation of graphene oxide in the above-mentioned preparation methods requires the introduction of a large amount of acid liquid and strong oxidant, resulting in a serious waste of water resources and energy in order to remove a large amount of acid liquid and strong oxidant in the purification stage, and these strong There are heavy metal ions in the oxidant, which is not recyclable, causing irreversible and serious pollution to the environment, thus hindering the mass production of graphene oxide

Method used

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  • Method for preparing graphene oxide based on high-concentration inorganic saline solution stripping
  • Method for preparing graphene oxide based on high-concentration inorganic saline solution stripping
  • Method for preparing graphene oxide based on high-concentration inorganic saline solution stripping

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Embodiment 1

[0041]Using sodium perchlorate as the electrolyte, weigh 17.2g of sodium perchlorate and add 5g of water and place it in an oven at 50°C for 30min. After the solution is clear and transparent, use it as electrolyte (concentration: 24.5mol / L) for electrochemical exfoliation of graphite . Add the prepared electrolyte in the electrolytic cell, choose graphite paper as the anode and connect it to the DC power supply, and use the platinum sheet as the cathode to connect it to the DC power supply. The distance between the two electrodes is 5 cm, and a DC voltage of 5 V is applied. Chemical peel reaction. After continuing for 30 hours, the electrode did not peel off, and graphene oxide aggregates were obtained. The actual figure is as follows figure 1 shown. After suction filtration and washing, disperse in an 80W ultrasonic cleaning machine for 30 minutes to obtain a two-dimensional sheet graphene oxide dispersion, and dry the dispersion at -20°C at 20 Pa for 72 hours to prepare g...

Embodiment 2

[0044] Using sodium perchlorate as the electrolyte, weigh 15g of sodium perchlorate and add 5g of water and place it in a 50°C oven for 30min. After the solution is clear and transparent, use it as the electrolyte (concentration: 21.4mol / L) for electrochemical exfoliation of graphite. Add the prepared electrolyte in the electrolytic cell, choose graphite paper as the anode and connect it to the DC power supply, and use platinum wire as the cathode to connect it to the DC power supply. The distance between the two electrodes is 6cm, and a 10V DC voltage is applied to conduct electrolysis at 15°C. Chemical peel reaction. After 10 hours, the electrodes did not peel off, and graphene oxide aggregates were obtained. After vacuum filtration and washing, they were dispersed in a 100W ultrasonic cleaner for 1 hour to obtain a two-dimensional sheet of graphene oxide dispersion. The dispersion was stored at -30°C Graphene oxide powder was prepared by drying under vacuum at 20 Pa for 24 ...

Embodiment 3

[0047] Using sodium perchlorate as the electrolyte, weigh 5g of sodium perchlorate and add 5g of water and place it in an oven at 50°C for 30min. After the solution is clear and transparent, use it as electrolyte (concentration: 7.1mol / L) for electrochemical exfoliation of graphite. Add the prepared electrolyte solution into the electrolytic cell, choose graphite paper as the anode and connect it to the DC power supply, and use platinum wire as the cathode to connect it to the DC power supply. The distance between the two electrodes is 10cm, and a voltage of 15V is applied, and the electrochemistry is carried out at 35°C. Stripping reaction. The electrode did not peel off for 1 hour, and graphene oxide aggregates were obtained. After vacuum filtration and cleaning, they were dispersed in a 150W ultrasonic cleaner for 2 hours to obtain a two-dimensional sheet of graphene oxide dispersion. The dispersion was vacuumed at -40°C Dry at 20Pa for 36h to prepare graphene oxide powder....

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Abstract

The invention provides a method for preparing graphene oxide based on high-concentration inorganic saline solution stripping, and belongs to the technical field of graphene oxide preparation. The method comprises the following steps: taking high-concentration inorganic saline solution as electrolyte, taking graphite as anode, taking inertia conductive precious metal material as the cathode, performing electrochemical stripping reaction to obtain the graphene oxide aggregation. By taking the high-concentration inorganic saline solution as the electrolyte, the quick decomposition of the water under low voltage can be inhibited, thereby realizing the continuous intercalation of the graphite; the damage on the graphite electrode integrity by the traditional low-concentration electrolyte is changed, thereby realizing the deep intercalation and bulking of the graphite; the anion in the high-concentration salt is used as the oxidation intercalation agent, the graphite can be oxidized while performing the intercalation and stripping the graphite, thereby preparing the graphene oxide; and meanwhile, the method for preparing graphene oxide disclosed by the invention is short in preparation cycle, low in cost, free from producing acid liquid, environment-friendly, simple and easy to realize industrial and large-batch production.

Description

technical field [0001] The invention relates to the technical field of graphene oxide preparation, in particular to a method for preparing graphene oxide based on exfoliation of a high-concentration inorganic salt solution. Background technique [0002] Since the concept of graphene was proposed by the research group led by A.K.Geim of the University of Manchester in 2004, graphene, as another bright star in the carbon family, has been highly valued by physics, chemistry and materials scientists. Among the current graphene preparation methods, the preparation of graphene oxide from graphite and then reduction to graphene is considered to be a large-scale preparation method for high-quality graphene. [0003] Graphene oxide is a derivative of graphene. Its structure is roughly the same as that of graphene. It is a two-dimensional planar structure. Compared with graphene, it not only has good hydrophilicity and dispersibility in water, but also can pass through Chemical modif...

Claims

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Application Information

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IPC IPC(8): C01B32/198
CPCC01B32/198
Inventor 阎兴斌杨娟王正军
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI