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A kind of method for preparing graphite oxide by intercalation method

A technology of fossil and graphite powder, which is applied in the field of preparing graphite oxide by intercalation method, can solve the problems of easy explosion and many process factors, and achieve the effect of high degree of oxygen intercalation and short reaction time.

Inactive Publication Date: 2011-12-14
THE SIXTH ELEMENT CHANGZHOU MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method uses KMnO 4 Instead of KClO 3 and KClO 4 , which relatively improves the safety of the experiment and reduces the generation of toxic gases, but KMnO 4 in NaNO 3 Concentrated H 2 SO 4 Improper temperature control in the system is still prone to explosion, and there are many process factors that need to be controlled during the reaction process

Method used

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  • A kind of method for preparing graphite oxide by intercalation method
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Effect test

Embodiment 1

[0022] The method for preparing graphite oxide by Haida 100 mesh flake graphite powder intercalation method comprises the following preparation steps:

[0023] 1. Weigh 2g of Haida 100 mesh flake graphite powder, pour it into a round bottom flask with a funnel, take 100ml of concentrated sulfuric acid with a weight percentage of 98% and slowly pour it into the round bottom flask, and then put in a stirring magnet;

[0024] 2. Set the stirring speed to 200 rpm, weigh 7g of potassium permanganate and add it evenly into the concentrated sulfuric acid graphite powder solution within 18 to 20 minutes;

[0025] 3. Soak the round bottom flask in a water bath, raise the temperature of the water bath to 35°C for 2 hours, and set the stirring speed to 500 rpm;

[0026] 4. After two hours, change the round-bottomed flask to an ice bath for cooling reaction in an ice bath. Slowly add 100ml of deionized water into the round-bottomed flask to dilute concentrated sulfuric acid. The stirring ...

Embodiment 2

[0032] The method for preparing graphite oxide by Haida 500 mesh flake graphite powder intercalation method comprises the following preparation steps:

[0033] 1. Weigh 2g of Haida 500 mesh flake graphite powder, pour it into a round bottom flask with a funnel, take 100ml of concentrated sulfuric acid with a weight percentage of 98% and slowly pour it into the round bottom flask, and then put in a stirring magnet;

[0034] 2. Set the stirring speed to 200 rpm, weigh 7g of potassium permanganate and evenly add it to the concentrated sulfuric acid graphite powder solution within 15 to 16 minutes;

[0035] 3. Soak the round bottom flask in a water bath, raise the temperature of the water bath to 35°C for 2 hours, and set the stirring speed to 500 rpm;

[0036] 4. After two hours, change the round-bottomed flask to an ice bath for cooling reaction in an ice bath. Slowly add 100ml of deionized water into the round-bottomed flask to dilute concentrated sulfuric acid. The stirring sp...

Embodiment 3

[0042] The method for obtaining graphite oxide by intercalation of Haida 100 mesh flake graphite powder comprises the following preparation steps:

[0043]1. Weigh 25g of Haida 100 mesh flake graphite powder, pour it into a round bottom flask with a funnel, take 1000ml of concentrated sulfuric acid with a weight percentage of 98% and slowly pour it into the round bottom flask, and then put in a stirring magnet;

[0044] 2. Set the stirring speed to 200 rpm, weigh 87.5g of potassium permanganate and add it evenly into the concentrated sulfuric acid graphite powder solution within 16-18 minutes;

[0045] 3. Soak the round bottom flask in a water bath, raise the temperature of the water bath to 35°C for 2 hours, and set the stirring speed to 500 rpm;

[0046] 4. After two hours, change the round-bottomed flask to an ice bath for cooling reaction in an ice bath. Slowly add 1000ml of deionized water into the round-bottomed flask to dilute concentrated sulfuric acid. The stirring sp...

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Abstract

The present invention relates to a method for preparing graphite oxide by intercalation, which comprises the following steps: firstly take graphite powder and place it in a reaction vessel, then add concentrated sulfuric acid and stir; then add potassium permanganate and stir; place the reaction vessel at 30 In a water bath at ~40°C; put the reaction vessel in an ice bath after heating in the water bath, add deionized water into the reaction vessel and stir; after cooling down in the ice bath, continue to add deionized water into the reaction vessel and stir; continue Stir, add hydrogen peroxide dropwise to the stepping container until no bubbles are generated; filter the insoluble matter in the suspension, wash with dilute hydrochloric acid and deionized water several times; filter the insoluble matter, and remove the The insoluble matter is placed in a vacuum oven and dried at room temperature for 1 to 2 days to obtain graphite oxide. The method of the invention has the advantages of short reaction time, high degree of oxygen intercalation, relatively safe synthesis process, suitable for large-scale production and the like.

Description

technical field [0001] The invention belongs to the technical field of graphite oxide preparation, in particular to a method for preparing graphite oxide by an intercalation method. Background technique [0002] The preparation of graphite oxide from graphite is considered to be a strategic starting point for large-scale synthesis of graphene. Graphite oxide can be further prepared by mechanical methods, such as pyrolytic expansion or ultrasonic dispersion in solvents, to prepare quasi-two-dimensional graphene oxide suspensions, and then through surface modification. Sexually increase its mechanical properties, and form graphene through reduction reaction. At present, the more commonly used methods for preparing graphite oxide mainly include the following. [0003] Brodie method: first use fuming HNO 3 Treat natural micropowder graphite, then use KClO 3 or KClO 4 As an oxygen intercalating agent, the temperature of the reaction system needs to be maintained at 0°C and th...

Claims

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Application Information

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IPC IPC(8): C01B31/00
Inventor 温祝亮蔡燕
Owner THE SIXTH ELEMENT CHANGZHOU MATERIALS TECH
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