Preparation method for aminated graphene oxide

A technology of graphene and amination, applied in chemical instruments and methods, inorganic chemistry, carbon compounds, etc., can solve problems affecting graphene performance, graphene curling and agglomeration, high temperature, etc.

Inactive Publication Date: 2019-01-22
SHANDONG OBO NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, higher temperatures and longer reaction times are usually required, which will inevitably cause graphene to curl and agglomerate, affecting the properties of graphene itself.

Method used

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  • Preparation method for aminated graphene oxide
  • Preparation method for aminated graphene oxide
  • Preparation method for aminated graphene oxide

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preparation example Construction

[0062] The invention provides a kind of preparation method of aminated graphene oxide, comprises the following steps:

[0063] A) After the activated graphene oxide solution, ammonia source and organic solvent are mixed and reacted, aminated graphene is obtained;

[0064] The activated graphene oxide includes graphene oxide activated by surface hydroxyl groups.

[0065] The present invention does not have special limitation to the definition of described graphene, can get final product with the concept of graphene well-known to those skilled in the art, those skilled in the art can select and adjust according to actual application situation, product requirement and quality requirement, the present invention Described graphene is preferably graphene in a broad sense, that is, a graphene-like material, preferably including one or more of graphene, graphene oxide and reduced graphene oxide, more preferably single-layer graphene, multi-layer graphene, Graphene oxide or reduced gr...

Embodiment 1

[0157] Graphene oxide after surface hydroxyl activation

[0158] ①Add 0.75g graphene oxide slurry (mass fraction 28%) in a single-necked flask, add 100mL DMF, and ultrasonically stir for 30min to obtain a graphene oxide dispersion;

[0159] ②Add 9g of activated 5A molecular sieve to the graphene oxide dispersion in step ①, soak the dispersion for 24 hours and filter the dispersion into a three-necked flask;

[0160] ③Weigh 1.14g p-toluenesulfonyl chloride (the molar ratio of p-toluenesulfonyl chloride and graphene oxide is 3:1), add 10mL DMF to dissolve;

[0161] ④Under stirring condition, the solution obtained in step ③ is slowly added dropwise to the graphene oxide dispersion obtained in step ②;

[0162] ⑤Transfer the three-necked flask containing the dispersion liquid in step ④ to the oil bath, connect the condenser tube and double-row tube, and pass nitrogen for 20 minutes;

[0163] ⑥Weigh 1.212g of triethylamine (the molar ratio of triethylamine to graphene oxide is 6:1...

Embodiment 2

[0177] Aminated graphene oxide

[0178] ①Add 0.212g of GOTs prepared in Example 1 into a single-necked flask, add 100mL of DMF, and stir ultrasonically for 30min to obtain a GOTs / DMF dispersion;

[0179] ② Weigh 1.3g of triethylenetetramine (the mass fraction of triethylenetetramine is 68%, and the molar ratio of triethylenetetramine to GOTs is 3:1) into a three-necked flask, and add 50mL of DMF to dissolve;

[0180] ③ Slowly add the GOTs / DMF dispersion obtained in step ① to the solution obtained in step ② under the condition of stirring in an ice bath (0°C);

[0181] ④ Add the reaction solution obtained in step ③ into a microwave reactor, and react for 10 minutes at a power of 800W;

[0182] ⑤ After the reaction is completed, the product is suction-filtered, washed with absolute ethanol, and vacuum-dried at 60° C. for 12 hours to obtain aminated graphene oxide.

[0183] see image 3 , image 3 It is a schematic diagram of the process flow for preparing aminated graphene o...

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Abstract

The invention provides a preparation method for aminated graphene oxide. The preparation method comprise a step of subjecting an activated graphene oxide solution, an ammonia source and an organic solvent to mixing and a reaction so as to obtain the aminated graphene oxide, wherein the activated graphene oxide comprises graphene oxide having undergone surface hydroxyl activation. According to theinvention, the graphene oxide having undergone surface hydroxyl activation is used as a raw material, and the ammonia source is directly added for amination modification; after a hydroxyl group on thesurface of the graphene oxide is activated, a carbon-oxygen bond becomes easy to break, so the desired temperature and time of amination are greatly reduced, and a modification reaction can be carried out under mild conditions at a low temperature; and thus, the lamellar structure of the graphite oxide can be well maintained and original characteristics can be reserved. Compared with a two-step-reaction amination process, the method of the invention has the following advantages: the surface-activated graphene oxide is directly utilized as the reaction raw material, so one step of reaction isomitted, and reaction time and energy consumption are reduced.

Description

technical field [0001] The invention belongs to the technical field of modified graphene, and relates to a preparation method of aminated graphene oxide, in particular to a preparation method of surface aminated graphene oxide. Background technique [0002] Graphene is a new material with a single-layer sheet structure composed of carbon atoms. It is a planar film composed of carbon atoms with sp2 hybrid orbitals forming a hexagonal honeycomb lattice, a two-dimensional material with a thickness of only one carbon atom. As a two-dimensional crystal composed of carbon atoms with only one atomic thickness, it is the thinnest material and the strongest material in the application field; at the same time, graphene has a huge theoretical specific surface area and stable physical and chemical properties , can maintain good structural stability under high working voltage and high current rapid charge and discharge; graphene also has excellent conductivity, which can reduce internal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/198B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01P2002/82
Inventor 蔡婷婷张在忠赵永彬吴开付刘海波
Owner SHANDONG OBO NEW MATERIAL CO LTD
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