Preparation method for graphite oxide with low oxidizability

A technology of oxidation degree and graphite, applied in the field of materials, can solve the problems of no research on GO stripping behavior, long time, unfavorable production, etc.

Inactive Publication Date: 2017-05-31

QINGDAO ZHIXIN BIOLOGICAL TECH CO LTD

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Problems solved by technology

However, these reports did not study the exfoliation behavior of GO, nor did they characterize the exfoliated GONS. At...

Abstract

The invention relates to a preparation method for graphite oxide with low oxidizability. The preparation method comprises the following steps: adding 50 ml of concentrated sulfuric acid and 0.5 g of graphite powder into a three-neck flask, carrying out uniform mixing under stirring, then carrying out cooling to 0 DEG C in an ice-water bath, slowly adding 0.5 to 1.5 g of potassium permanganate, carrying out slow heating to 35 DEG C, allowing the above substances to undergo a reaction for 2 h, then carrying out slow heating to 70 DEG C, and carrying out a reaction for half an hour until potassium permanganate is completely consumed so as to obtain GO with low oxidizability; after completion of the reaction, adding a great amount of ice water and carrying out centrifugal sedimentation; then carrying out washing with an aqueous hydrochloric acid solution with a concentration of 10% six times and washing with deionized water three times; carrying out centrifugation and collecting a product; and drying the product in a vacuum drying oven at 60 DEG C so as to obtain graphite oxide with low oxidizability. Compared with the Brodie method and the Staudenmaier method, the preparation method has higher efficiency and does not give out toxic gas in the process of preparation. Since the speed of a reaction of potassium permanganate with graphite is fast, the purpose of reaching a low oxidation degree of GO is achieved by changing the usage amount of an oxidizing agent.

Application Domain

Graphite

Technology Topic

IonPotassium permanganate +9

Examples

Experimental program(3)

Example Embodiment

[0010] Example 1

[0011] A method for preparing graphite oxide with low oxidation degree. The steps are as follows: add 50ml concentrated sulfuric acid and 0.5g graphite powder into a three-necked flask, stir evenly, cool to 0°C in an ice water bath, and then slowly add 0.5g permanganic acid Potassium, slowly increase the temperature to 35°C, after 2 hours of reaction, slowly increase the temperature to 70°C, and react for half an hour until the potassium permanganate is consumed completely and GO with a low degree of oxidation is obtained. After the reaction is completed, pour into a large amount of ice water After centrifugation, it was washed 6 times with 10% hydrochloric acid aqueous solution and three times with deionized water. The product was collected by centrifugation, and finally dried in a vacuum oven at 60°C to obtain the product.

Example Embodiment

[0012] Example 2

[0013] A method for preparing low-oxidation graphite oxide, the steps are as follows: add 50ml concentrated sulfuric acid and 0.5g graphite powder into a three-necked flask, stir evenly, cool to 0°C in an ice water bath, and then slowly add 1.0g permanganic acid Potassium, slowly increase the temperature to 35°C, after 2 hours of reaction, slowly increase the temperature to 70°C, and react for half an hour until the potassium permanganate is consumed completely and GO with a low degree of oxidation is obtained. After the reaction is completed, pour into a large amount of ice water After centrifugation, it was washed 6 times with 10% hydrochloric acid aqueous solution and three times with deionized water. The product was collected by centrifugation, and finally dried in a vacuum oven at 60°C to obtain the product.

Example Embodiment

[0014] Example 3

[0015] A method for preparing low-oxidation graphite oxide, the steps are as follows: add 50ml concentrated sulfuric acid and 0.5g graphite powder into a three-necked flask, stir evenly, cool to 0°C in an ice water bath, and then slowly add 1.5g permanganic acid Potassium, slowly increase the temperature to 35°C, after 2 hours of reaction, slowly increase the temperature to 70°C, and react for half an hour until the potassium permanganate is consumed completely and GO with a low degree of oxidation is obtained. After the reaction is completed, pour into a large amount of ice water After centrifugation, it was washed 6 times with 10% hydrochloric acid aqueous solution and three times with deionized water. The product was collected by centrifugation, and finally dried in a vacuum oven at 60°C to obtain the product.

PUM

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