Method for preparing functionalized graphene through Mannich reaction

A Mannich reaction and functional technology, applied in the preparation and application of modified graphene, achieves the effects of low price, excellent mechanical and electrical properties, and simple preparation process

Active Publication Date: 2013-05-22
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It aims to solve the problems of low-cost preparation of graphene, reactivity with polymers and easy processing of composite materials, and explore the preparation method of functionalized graphene suitable for industrial applications

Method used

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  • Method for preparing functionalized graphene through Mannich reaction

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Experimental program
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Embodiment 1

[0035] Graphene oxide was prepared by the Hummers method. Specific references: Hummers Jr, W. S.; Offeman, R. E. J Am Chem Soc 1958 , 80 , 1339.

[0036] Disperse 0.1 g of graphene oxide into water to make a 1 mg / mL dispersion. Dissolve epigallocatechin gallate in water (10 mg / mL). Mix the above two solutions in proportion (the amount of epigallocatechin gallate is 100 wt% of graphene oxide), mix well, and heat to 80 o C, reacted for 8 h. Mix 10 mL absolute ethanol, 0.9 g polyetheramine (molecular formula H 3 C-(OCH 2 CH 2 ) 31 -(OCH 2 CH–CH 3 ) 10 -NH 2 ), 0.03 g formaldehyde were sequentially added to the above solution, and the temperature was adjusted to 40 oCAfter reacting for 8 hours, the obtained solution was repeatedly washed to obtain the functionalized graphene modified by the Mannich condensate. The obtained functionalized graphene has good dispersibility in media such as water, alcohol, ester, ketone, haloalkane, dimethyl sulfoxide, dimethylformami...

Embodiment 2

[0040] Graphene oxide was prepared by the Staudenmaier method. Specific references: L. Staudenmaier, Ber. Dtsch. Chem. Ges. 1898, 31 , 1481.

[0041] Disperse 0.1 g of graphene oxide into water to make a 0.1 mg / mL dispersion. Dissolve gallic tannin in water (1 mg / mL), mix the above two solutions in proportion (the amount of gallic tannin is 100 wt% of graphene oxide), mix well, stir well, and heat to 80 o C, reacted for 8 h. Mix 50 mL methanol, 0.05 g polyetheramine (molecular formula: OH-(OCH 2 CH 2 ) 25 -(OCH 2 (CH 3 )CH) 18 -(OCH 2 CH 2 ) 10 -NH 2 ), 0.001 g formaldehyde was added to the above solution in turn, and the temperature was adjusted to 70 oC After reacting for 4 hours, the obtained solution was washed repeatedly to obtain the functionalized graphene modified by Mannich condensate. The obtained functionalized graphene has good dispersibility in media such as water, alcohol, ester, ketone, haloalkane, dimethyl sulfoxide, dimethylformamide, etc. ...

Embodiment 3

[0044] Graphene oxide was prepared by the Brodie method. Specific references: B.C. Brodie, Ann Chim Phys , 1860, 59 , pp. 466.

[0045] Disperse 0.1 g of graphene oxide into water to make a 5 mg / mL dispersion. Dissolve 0.05g epigallocatechin gallate (5 mg / mL) and 0.05g gallic tannin (5 mg / mL) in water, and mix the above three solutions in proportion (epigallocatechin gallate and The sum of the amount of gallnut tannin is 100 wt% of graphene oxide) mix evenly, after fully stirring, heat to 80 o C, reacted for 8 h. Mix 1 mL glycerin, 0.36 g polyetheramine (molecular formula: C 2 h 5 -(OCH 2 CH 2 ) 35 -(OCH 2 (CH 3 )CH) 6 -(OCH 2 CH 2 ) 10 -NH 2 ), 0.012 g formaldehyde were added to the above solution in turn, and the temperature was adjusted to 90 oC After reacting for 0.5 hours, the obtained solution was washed repeatedly to obtain the functionalized graphene modified by Mannich condensate. The obtained functionalized graphene has good dispersibility in med...

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Abstract

The invention discloses a method for preparing functionalized graphene through Mannich reaction. The method comprises the following steps of: reducing oxidized graphene by taking plant polyphenols and derivatives of the plant polyphenols as reducing agents to obtain the polyphenol modified graphene; and then preparing the functional graphene with amphipathy through Mannich reaction between polyphenol groups on the surface of the graphene and polyether amine. The method disclosed by the method has the advantages of mild preparation conditions, simple and efficient purification process and no-purification of intermediate products. Simultaneously, raw materials for preparation of the functionalized graphene comprise the reducing agents and a modifier and have the characteristics of rich sources and low cost, and therefore, the functionalized graphene and colloids thereof can be efficiently prepared on a large scale. The functionalized graphene can be used for directly preparing a graphene hybrid material with excellent electric conductivity and toughness, has very good solvent dispersivity and excellent storage stability, and is suitable for compounding with various polymers to prepare a polymer/graphene composite material with high performance.

Description

[0001] technical field [0002] The invention relates to the field of preparation and application of modified graphene, in particular to a method for preparing functionalized graphene by Mannich reaction. Background technique [0003] Graphene is a single-atom-thick layer of carbon atoms, a two-dimensional carbon atom crystal discovered only in recent years. It is considered to be the basic structural unit of fullerene, carbon nanotube (CNT) and graphite. Because of its special mechanical, quantum and electrical properties, it is highly valued by the physics and materials science circles. Free-state 2D crystal structures have long been considered thermodynamically unstable and cannot exist independently in ordinary environments. In 2004, Geim and other talents from the University of Manchester peeled off a small amount of graphene monoliths from graphite and studied its electrical properties. They found that it has special electronic properties and has great potential in th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C08K3/04C08K5/17C08K9/04
Inventor 郭宝春廖瑞娟唐征海
Owner SOUTH CHINA UNIV OF TECH
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