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Method of production of graphite oxide and uses thereof

一种石墨、用途的技术

Inactive Publication Date: 2015-08-05
BELENOS CLEAN POWER HLDG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, none of the aforementioned methods provide a method for preparing graphite oxide, and thus GO, suitable for industrial scale, because of explosive chlorine dioxide generation by methods derived from the Brodie reaction, poor oxidation degrees by methods derived from the Staudenmaier method, and The washing step requires the use of large amounts of water and handling (filtering) of the final product
Currently, GO is mainly prepared based on the method proposed by Hummers and Offeman, but the final product is difficult to purify due to the presence of manganese residues
Therefore, the method of Hummers and Offeman is not suitable for the preparation of GO for electronic device applications, where any metal residues in graphene would be problematic.

Method used

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  • Method of production of graphite oxide and uses thereof
  • Method of production of graphite oxide and uses thereof
  • Method of production of graphite oxide and uses thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0105] Example 1: Synthesis of graphite oxide from sulfate-intercalated graphite flakes by the method of the present invention

[0106] A mixture of 2.0 g of sulfate intercalated sheets (ASBURY 1721: 300 μm) and 30 ml of nitric acid (Merck 100% fuming nitric acid) was cooled to 0° C. in a 100 ml glass reactor. A purge flow of 250 liters / hour of air was initiated through the reactor and maintained throughout the reaction. Acid vapor is visible at room temperature, but is no longer visible at 0°C.

[0107] Then 17.0 g of sodium chlorate (oxidizing agent) was added in 1 g portions over 2 hours while stirring. Green vapour appeared after adding a few grams, indicating ClO 2 The presence. will contain the formed ClO 2 The gaseous effluent of C is continuously neutralized by blowing into sodium bisulfite solution (about 40%), and then the gaseous chlorine produced by this neutralization step is neutralized by sodium hydroxide before being released to the atmosphere.

[0108] Th...

Embodiment 2

[0111] Example 2: Synthesis of graphite oxide by standard Brodie method

[0112] In order to compare the graphite oxide obtained by the method of the present invention and the known methods of preparing graphite oxide, the standard Brodie method was applied to graphite powder as follows: 2.0 g (0.16 moles) of graphite powder (Timcal SFG6) and 17.0 g (0.16 moles) of chlorine The sodium mixture was cooled to -20°C in a 50ml Schlenk tube. A 15 ml volume (2.78 moles) of nitric acid (Merck 100% fuming nitric acid) was added slowly over 2 hours. At the beginning, only acid vapour is visible, after a few milliliters the vapour turns green, indicating ClO 2 The presence. The reaction was then allowed to reach room temperature over 12 hours. The color of the mixture turned turquoise during the previous 12 hours. The mixture was warmed to 60°C over 1 hour 30 minutes and held for 30 minutes. During heating, ClO 2 The release is especially severe (b.p.ClO 2 11°C). The reaction was...

Embodiment 3

[0115] Example 3: Synthesis of graphite oxide by standard Staudenmaier method (comparative example: non-inventive)

[0116] The Staudenmaier method as described in Staudenmaier, 1898 (see above) was applied to graphite powder (Timcal SFG6). The resulting graphite oxide was of poor quality, with a very low degree of oxidation (C / O ratio of 9.8-12.8). These results indicate that the staudenmaier method is not suitable for the large-scale production of graphite oxide.

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Abstract

The present invention is related to a new scalable method of forming graphite oxide (only one or few layers of carbon atoms) of high purity (notably without metallic residues) and high oxidation degree from graphite flakes in a cost-effective and reduced environmental impact.

Description

technical field [0001] The present invention relates to the field of preparing graphite oxide, especially graphite oxide with high oxidation degree. Background of the Invention [0002] Graphene is a two-dimensional (monoplanar) crystal of carbon that forms graphite by stacking, which is stable at ambient temperature. Thus, graphene can be described as a single-atom-thick layer of graphite. It should be noted that in the literature the term boundary between graphite and graphene is not always clearly defined, but it is generally accepted that a 3D arrangement of graphene layers is referred to as "graphite" when there is no 3D arrangement It is called "graphene" (Park et al., 2011, Carbon, 49, 3019-3023). Graphene has attracted great interest due to its excellent mechanical, electrical, thermal and optical properties, and has been used in several fields including bioengineering, composite materials, energy technology and nanotechnology, and is considered an energy storage ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
CPCC01B31/0476C01B31/043C01B32/23C01B32/192C01B32/198Y10T428/2982
Inventor B·普罗姆J·日诺兹R·马蒂E·瓦诺里J-P·布儒瓦
Owner BELENOS CLEAN POWER HLDG
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