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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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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these reports did not study the exfoliation behavior of GO, nor did they characterize the exfoliated GONS. At the same time, the preparation of GO by these methods is relatively long, which is not conducive to actual production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

Embodiment 2

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

Embodiment 3

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

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PUM

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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.

Description

technical field [0001] The invention belongs to the technical field of materials, and in particular relates to a preparation method of graphite oxide with low oxidation degree. Background technique [0002] The preparation of graphene has always been a hot and difficult topic in the scientific and industrial circles. Although many methods have successfully prepared graphene, each method has its own advantages, but there are also certain disadvantages. For example, the mechanical exfoliation method can prepare graphene sheets with the most complete structure, but it is too time-consuming and labor-intensive; chemical vapor deposition (CVD) can prepare high-quality graphene films, but this method requires high equipment and costs Higher; liquid-phase ultrasonic stripping has the advantages of simple operation and convenience, but it is highly dependent on the choice of solvent. Moreover, these methods also have a common shortcoming, that is, graphene cannot be prepared on a ...

Claims

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Application Information

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IPC IPC(8): C01B32/23
Inventor 孙国志
Owner QINGDAO ZHIXIN BIOLOGICAL TECH CO LTD
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