Preparation method of aminated graphene

A technology of aminated graphene and carboxylated graphene, applied in chemical instruments and methods, inorganic chemistry, carbon compounds, etc., can solve problems such as physical health damage, environmental damage, and low amino content, and prevent structural changes. , the effect of avoiding agglomeration and preventing damage

Active Publication Date: 2017-07-14
山东金城石墨烯科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, although the traditional aminated graphene process route is simple to operate, the obtained amino content is low, no more than 10.0wt%.
Moreover, tetrahydrofuran and thionyl chloride used in the synthesis process are not only harmful to the environment, but also cause irreversible damage to the health of practitioners after long-term exposure
The ball milling process involved in the traditional method of synthesizing aminated graphene not only destroys the graphene sheet structure, but also mechanically incorporates amino groups so that most of the amino groups exist in the product in the form of physical adsorption, and only a small part of the amino groups are chemically bonded. The form of bonded graphene exists in the product, and the reactive sites of the aminated graphene obtained by this method will be reduced, and the expected effect cannot be achieved.

Method used

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Experimental program
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Embodiment 1

[0020] (1) Preparation of graphene oxide

[0021] The method for synthesizing graphene oxide in the present invention is a chemical oxidation method.

[0022] The source of the amino group in the present invention is the carboxyl group in the graphene oxide, so the carboxyl group content in the graphene oxide directly affects the doping amount of the amino group in the aminated graphene. Therefore, in the process of synthesizing graphene oxide, we changed the concentrated sulfuric acid into a mixed acid of concentrated sulfuric acid and concentrated phosphoric acid and prolonged the oxidation time to increase the oxidation degree of graphite and increase the reactive sites. The volume ratio of concentrated sulfuric acid to concentrated phosphoric acid is 1:1, and the oxidation time is 2 hours.

[0023] (2) Preparation of Aminated Graphene

[0024] Disperse graphene oxide uniformly in aqueous solution with a concentration of 1mol L -1 , then add NaOH and chloroacetic acid wi...

Embodiment 2

[0030] (1) Preparation of graphene oxide

[0031] The method for synthesizing graphene oxide in the present invention is a chemical oxidation method.

[0032] The source of the amino group in the present invention is the carboxyl group in the graphene oxide, so the carboxyl group content in the graphene oxide directly affects the doping amount of the amino group in the aminated graphene. Therefore, in the process of synthesizing graphene oxide, we changed the concentrated sulfuric acid into a mixed acid of concentrated sulfuric acid and concentrated phosphoric acid and prolonged the oxidation time to increase the oxidation degree of graphite and increase the reactive sites. The volume ratio of concentrated sulfuric acid to concentrated phosphoric acid is 3:1, and the oxidation time is 5 hours.

[0033] (2) Preparation of Aminated Graphene

[0034] Disperse graphene oxide uniformly in aqueous solution with a concentration of 0.5mol L -1 , then add NaOH and chloroacetic acid ...

Embodiment 3

[0040] (1) Preparation of graphene oxide

[0041] The method for synthesizing graphene oxide in the present invention is a chemical oxidation method.

[0042] The source of the amino group in the present invention is the carboxyl group in the graphene oxide, so the carboxyl group content in the graphene oxide directly affects the doping amount of the amino group in the aminated graphene. Therefore, in the process of synthesizing graphene oxide, we changed the concentrated sulfuric acid into a mixed acid of concentrated sulfuric acid and concentrated phosphoric acid and prolonged the oxidation time to increase the oxidation degree of graphite and increase the reactive sites. The volume ratio of concentrated sulfuric acid to concentrated phosphoric acid is 8:1, and the oxidation time is 3 hours.

[0043] (2) Preparation of Aminated Graphene

[0044] Disperse graphene oxide uniformly in aqueous solution with a concentration of 2mol L -1, then add NaOH and chloroacetic acid wit...

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Abstract

The invention relates to a preparation method of aminated graphene. The preparation method comprises the following steps: synthesizing graphene oxide by means of a chemical oxidation process; adjusting the volume ratio of concentrated sulfuric acid and strong phosphoric acid to change the oxidizing degree of graphene oxide; then treating the graphene oxide with sodium chloroacetate to obtain carboxylated graphene; then adjusting the pH to 10-12 with ammonia water; performing a reaction on the carboxylated graphene and ammonia water to generate amidated graphene; then dehydrating the amidated graphene with phosphorus oxychloride to generate cyanated graphene; then performing catalytic hydrogenation to obtain the aminated graphene; and lyophilizing the obtained aminated graphene obtain aminated graphene powder. Through representation and detection, the content of amino in the aminated graphene is 15.0-25.0wt%. The preparation method provided by the invention is simple in process, and can be used for synthesizing aminated graphene with a high doping amount.

Description

technical field [0001] The invention belongs to the field of modification of functional materials, and in particular relates to a preparation method of aminated graphene. Background technique [0002] As an emerging material, graphene has experienced rapid development since its discovery due to its excellent properties. Graphene has good electrical conductivity, mechanical properties and optical properties, and graphene has a large specific surface area, but it is difficult for single-layer graphene to exist stably in aqueous solution, and it is easy to agglomerate. This problem limits the development and application of graphene. , so developing a well-dispersed hydrophilic graphene becomes a thorny problem. [0003] Aminated graphene not only retains the good electrical conductivity, mechanical properties and optical properties of graphene, but also has a large specific surface area. In addition, the amino group has good adsorption capacity for heavy metals, and the amina...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/192C01B32/194
CPCC01P2004/03C01P2004/80
Inventor 李欣郑庚修曲良体张忠政张志旭于卫昆张敏王丽波
Owner 山东金城石墨烯科技有限公司
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