Synthetic technology of graphite oxide

Abstract

A synthetic technology of graphite oxide comprises the following steps: placing graphite powder, concentrated sulfuric acid, a persulfate and an oxide in a reaction container according to a ratio of the graphite powder to the concentrated sulfuric acid to the persulfate to the oxide of 5-30g:50-300ml:5-30g:3-30g, stir-mixing, carrying out ultrasonic treatment for 3-25min, stirring in a 20-200DEG C water or oil bath for 2-24h, allowing to stand for 1-16h, filtering, drying, adding the concentrated sulfuric acid having an amount 2-7 times higher than the previous amount of the concentrated sulfuric acid, carrying out the ultrasonic treatment for 3-150min, slowly adding potassium permanganate having an amount 1-7 times higher than the addition amount of the graphite powder, continuously stirring for 2-24h, adding deionized water having an amount equal to the secondary addition amount of the concentrated sulfuric acid under an ice bath cooling condition, stirring for 5-h, adding hydrogen peroxide while stirring until no bubbles appear to obtain a graphite oxide solution, filtering the graphite oxide solution, and drying to obtain the graphite oxide. The synthetic technology has the advantages of no pollution, high raw material utilization rate, simple preparation process, high oxide insertion degree, and easy operation.

Description

technical field [0001] The invention belongs to a synthesis process of graphite oxide, in particular to a method for preparing graphite oxide by an intercalation method. Background technique [0002] Graphene is a two-dimensional carbon atom crystal with a thickness of one atom. It is the thinnest substance artificially produced at present. It is considered to be the basic structural unit of fullerene, carbon nanotube and graphite (Geim, A.K. et al. Nature Materials 6,183 (2007)). At present, the preparation methods of free-state graphene mainly include micromechanical splitting method (Novoselov, K.S. et al. Science 306,666 (2004)), epitaxial growth method (Berger, C. et al. Science 312,1191 (2006)) and mechanical exfoliation Graphite oxide method (Stankovich, S. et al. Carbon 45, 1558 (2007)). Among them, the first two methods are not suitable for large-scale preparation of graphene due to high cost and poor controllability, thus limiting the large-scale application of g...

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Problems solved by technology

The traditional Hummers method will generate red oily Mn during the reaction process 2 o 7 Intermediates, there are safety hazards such as combustion and explosion under water or high temperature conditions, the degree of oxygen intercalation of the obtained graphite oxide products is not high, it is difficult to achieve first-order intercalation, and the oxygen content is generally not higher than 40 wt%, thus limiting Its practical preparation and application

The three methods introduced above will produce NO and N during the reaction process. 2 o 4 , SO 2 and SO 3 Harmful gases such as gases are important pollution sources of the atmospheric environment, and thus are not suitable for large-scale industrial production

The published patent CN102275896A is a method for preparing graphite oxide by intercalation method. In the process of preparing graphite oxide, the insoluble matter obtained after filtration needs to be washed with acid and water for many times, and the consumption of raw materials is relatively large, and the operation steps are also very expensive. cumbersome

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