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Preparation method of organic modified graphene

A graphene and modification technology, applied in the field of two-dimensional nanomaterial graphene preparation, can solve the problems of difficult to separate morphology, long preparation period, low degree of graphene exfoliation, etc., to achieve efficient exfoliation, controllability and stability sexual effect

Active Publication Date: 2017-05-17
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chen Guohua (Journal of Materials Chemistry, 2010, 20 (28): 5817-5819) realized the shear exfoliation of the graphite structure at a low speed (300 rpm) by adding a strong polar solvent DMF into the ball milling system, which can be lower Cost-effective preparation of graphene, but the obtained graphene sheets are too large and easy to reunite, and the organic solvent in the reaction process is difficult to remove
León V (ACS nano, 2014, 8(1): 563-571.) successfully prepared graphene with fewer layers by using melamine as a friction agent and intercalation agent to exfoliate the graphite structure by ball milling. Melamine and graphene sheets are non-covalently cross-linked. The presence of melamine will affect the structure of graphite sheets and reduce its related properties. At the same time, it is difficult to separate excess melamine from graphite after ball milling.
Dai Liming (Proceedings of the National Academy of Sciences, 2012,109 (15): 5588-5593.) has studied adding dry ice in ball milling system and comes the method that exfoliates graphite and prepares graphene, and the graphene edge prepared by this method contains a certain amount of Carboxyl groups, but the obtained graphene has a low exfoliation degree, is difficult to separate and has uncontrollable morphology, and there are still problems such as poor graphene dispersion and interface bonding in further applications.
Generally speaking, due to the problems of easy agglomeration and difficult dispersion in the application of graphene at this stage, in order to meet the requirements of uniform dispersion in the process, graphene oxide is mostly used in practical applications, but the large number of oxygen-containing functional groups between the sheets will cause its sheet The increase of interlayer spacing and the destruction of structural integrity make the performance of graphene itself unable to be fully utilized.
Therefore, there is an urgent need to develop a low-cost and efficient method for preparing graphene with an organic surface and a complete bulk structure to solve the problems of high cost, long preparation cycle, difficult dispersion and poor interface bonding of graphene in large-scale applications.

Method used

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Experimental program
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Effect test

Embodiment 1

[0020] Original graphite, nitrogen-containing organic matter are as 10:1 as in ball mill jar with mass fraction, and selected original graphite is the graphite powder of common graphite ore processing; Nitrogen-containing organic matter monomer is aromatic amine solidifying agent diaminodiphenylmethane ( DDM) and aliphatic amine curing agent ethylenediamine in a mass ratio of 1:1; the buffer solution is a Tris (HCl) solution with pH=8. Fill in carbon dioxide gas to make the pressure 15MPa, then close the air valve to seal the ball mill tank, set the ball mill speed to 600rpm for continuous ball milling for 48h, then add 5 parts by mass of buffer solution (calculated as 1 part by mass of nitrogen-containing organic matter, the following examples Same) and continue ball milling for 24 hours. After degassing, the resulting product was diluted with acetone and then ultrasonically treated for 60 minutes. After being centrifuged at 8000 rpm for 20 minutes, it was dialyzed for one day...

Embodiment 2

[0025]Original graphite, nitrogen-containing organic matter are as 10:5 as in the ball mill jar with mass fraction, and selected original graphite is the graphite powder of common graphite ore processing; Nitrogen-containing organic matter monomer is aromatic amine solidifying agent diaminodiphenylmethane ( DDM) and aliphatic amine curing agent ethylenediamine in a mass ratio of 1:1. ; The buffer solution is a Tris (HCl) solution with pH=8. Fill the carbon dioxide gas to make the pressure 10MPa, then close the air valve to seal the ball mill tank, set the speed of the ball mill to 600rpm and continue ball milling for 48 hours, then add 5 parts by mass of buffer solution and continue ball milling for 24 hours, after deflation, dilute the obtained product with acetone Sonicate for 60 minutes, centrifuge at 8000rpm for 20 minutes and then dialyze for one day using a dialysis bag with a molecular weight cut-off of 6000-10000, and freeze-dry the solution to obtain a black powder. ...

Embodiment 3

[0030] Original graphite, nitrogen-containing organic matter are as 10:5 as in the ball mill jar with mass fraction, and selected original graphite is the graphite powder of common graphite ore processing; Nitrogen-containing organic matter monomer is aromatic amine solidifying agent diaminodiphenylmethane ( DDM) and aliphatic amine curing agent ethylenediamine in a mass ratio of 1:1; the buffer solution is the polar solvent acetone. Fill the carbon dioxide gas to make the pressure 10MPa, then close the air valve to seal the ball mill tank, set the speed of the ball mill to 600rpm and continue ball milling for 48 hours, then add 5 parts by mass of buffer solution and continue ball milling for 24 hours, after deflation, dilute the obtained product with acetone Sonicate for 60 minutes, centrifuge at 8000rpm for 20 minutes and then dialyze for one day using a dialysis bag with a molecular weight cut-off of 6000-10000, and freeze-dry the solution to obtain a black powder. The obta...

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Abstract

The invention discloses a preparation method of organic modified graphene and belongs to the field of preparation of two-dimension nano material graphene. The method is characterized by taking low-cost raw graphite as the raw material, adding different masses of dry ice for creating high-pressure and high-energy environment, preparing graphene via a ball milling method, simultaneously introducing nitrogenous organic matters in the ball milling process, taking nitrogenous organic matters as friction agents and modifiers for simultaneously preparing graphene and carrying out in-situ modification to prepare a nitrogenous organic matter modified graphene structure. Through the preparation method of organic modified graphene, graphene with a circular microstructure is prepared by controlling reaction time, reaction pressure and the ratio of the raw graphite to the nitrogenous organic matters; a low-cost and high-efficiency method for preparing graphene with organic modified surface and complete body structure is developed; the problems of high cost, long preparation cycle, low dispersibility and poor interfacial adhesion caused in large-scale application of graphene are solved; the method has a great significance in industrial production and application of graphene.

Description

technical field [0001] The invention belongs to the field of preparation of two-dimensional nanometer material graphene, and in particular relates to the preparation of an organically modified graphene with a special circular microstructure through a high-pressure high-energy ball milling method. Background technique [0002] Graphene is a honeycomb two-dimensional nanomaterial whose carbon atoms are sp 2 The hybrid form exists, because of its good mechanical properties, thermal properties and electrical properties, it has a wide range of applications in many fields such as composite materials, electrode materials, thermal conductive materials and biological materials. However, the traditional graphene preparation methods all have inevitable shortcomings, which limit the further engineering application of graphene. Such as the mechanical exfoliation method is to obtain graphene by peeling graphite sheets layer by layer by physical methods. The integrity and quality of the r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/19C01B32/194
CPCC01P2002/82C01P2002/85C01P2002/88C01P2004/04
Inventor 贾晓龙杨文刚王润亭杨小平
Owner BEIJING UNIV OF CHEM TECH
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