Preparation method of aminated magnetic graphene

A magnetic graphene, amination technology, applied in chemical instruments and methods, inorganic chemistry, carbon compounds, etc., can solve problems such as reducing the saturation magnetization of composite materials, achieve good superparamagnetic properties, good application prospects, synthesis The effect of high safety

Inactive Publication Date: 2013-07-03
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Graphene has good electrical conductivity, mechanical strength, catalytic performance, optical performance, adsorption performance, etc. It is currently the fastest conductive at room temperature, the largest mechanical strength, thermal conductivity The most powerful material, due to these physical properties, graphene is widely used in many fields, such as: sensors, catalysis, energy materials, etc.; magnetic materials are ancient and widely used functional materials, magnetic iron oxide nanoparticles smaller than 20 nm The particles have superparamagnetism at room temperature and produce magnetic responses under the action of an external magnetic field; according to these characteristics, magnetic iron oxide nanoparticles have shown attractive properties in magnetic separation, magnetic monitoring, nuclear magnetic resonance, and drug controlled release. The application prospect of magnetic graphene has attracted the interest of many research groups due to the combination of the advantages of graphene and magnetic nanoparticles; Chen Yongsheng's research group [Journal of Materials Chemistry 19 (2009) 2710-2714] prepared magnetic Nanoparticle-graphene composite materials; Yu Shuhong's research group [Small 6 (2010) 169-173] Preparation of magnetic nanoparticles-graphene composites by pyrolysis of iron acetylacetonate in graphene oxide solution wrapped in sodium polystyrene sulfonate Materials, so that the surface of the composite material is connected with different amounts of magnetic nanoparticles; Chan et al [Carbon 48 (2010) 3139-3144] synthesized magnetic nanoparticles-graphene composites by chemical cross-linking, but they used silica Coating magnetic nanoparticles greatly reduces the saturation magnetization of composite materials; although there have been many reports on magnetic graphene, aminated magnetic graphene with positive charges on the surface has rarely been reported

Method used

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  • Preparation method of aminated magnetic graphene
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  • Preparation method of aminated magnetic graphene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) Add 3 millimoles of ferric chloride to 40 milliliters of graphene oxide solution with a concentration of 4 mg / ml, and stir for 1 hour to prepare a graphene oxide solution containing ferric chloride.

[0018] (2) Add 9 millimoles of dimethylaminoethyl methacrylate to the graphene oxide solution containing ferric chloride prepared in step (1), stir for 30 minutes, and obtain dimethylaminoethyl methacrylate and Graphene oxide mixed solution of ferric chloride.

[0019] (3) the graphene oxide mixed solution containing dimethylaminoethyl methacrylate and ferric chloride that step (2) makes is transferred in the hydrothermal reaction kettle of 100 milliliters, reacts 8 hours at 150 ℃, Then cooled to room temperature, centrifuged and washed with water, then vacuum-dried at 60° C. for 24 hours to prepare aminated magnetic graphene.

Embodiment 2

[0021] (1) Add 4 mmoles of iron sulfate to 40 milliliters of graphene oxide solutions with a concentration of 0.5 mg / ml, and stir for 1.5 hours to obtain a graphene oxide solution containing iron sulfate.

[0022] (2) Add 12 millimoles of diethylaminoethyl methacrylate to the graphene oxide solution containing ferric sulfate prepared in step (1), and stir for 45 minutes to obtain a solution containing diethylaminoethyl methacrylate. and graphene oxide mixed solution of ferric sulfate.

[0023] (3) the graphene oxide mixed solution containing diethylaminoethyl methacrylate and ferric sulfate that step (2) makes is transferred in the hydrothermal reaction kettle of 100 milliliters, reacts 12 hours at 200 ℃, Then cooled to room temperature, centrifuged and washed with water, then vacuum-dried at 60° C. for 24 hours to prepare aminated magnetic graphene.

Embodiment 3

[0025] (1) Add 6 mmoles of ferric nitrate to 40 milliliters of graphene oxide solution with a concentration of 6 mg / ml, and stir for 2 hours to prepare a graphene oxide solution containing ferric nitrate.

[0026] (2) Add 25 millimoles of dimethylaminoethyl acrylate to the graphene oxide solution containing ferric nitrate prepared in step (1), stir for 120 minutes to obtain dimethylaminoethyl acrylate and ferric nitrate Graphene oxide mixed solution.

[0027] (3) Transfer the graphene oxide mixed solution containing dimethylaminoethyl acrylate and ferric nitrate prepared in step (2) into a 100 ml hydrothermal reactor, react at 160°C for 16 hours, and then cool to room temperature, centrifuged and washed with water, then vacuum-dried at 60° C. for 24 hours to prepare aminated magnetic graphene.

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Abstract

The invention discloses a preparation method of aminated magnetic graphene. The preparation method comprises the following steps of: adding 3-6mmol of ferric iron salt into 40ml of a 0.5-6mg / ml graphene oxide solution, and stirring for 1-2 hours until the ferric iron salt is completely dissolved; adding 9-25mmol of organic base, and stirring for 30-120 minutes to obtain a graphene oxide mixing solution containing the organic base and the ferric iron salt; and transferring the prepared mixing solution into a hydrothermal reaction kettle, reacting for 8-24 hours at 150-200 DEG C, cooling to room temperature, centrifuging and washing, and carrying out vacuum drying for 24hours at 60 DEG C to obtain the amino magnetic graphene. The method disclosed by the invention has the advantages of moderate reaction, simple operation, convenient separation, high synthesis safety, low environmental pollution and the like; and the prepared aminated magnetic graphene has excellent superparamagnetism performance, and has a good application prospect on absorption, bioseparation, magnetic catalysis and other aspects.

Description

technical field [0001] The invention belongs to the technical field of nanocomposite materials, in particular to a preparation method of aminated magnetic graphene. Background technique [0002] Graphene has good electrical conductivity, mechanical strength, catalytic performance, optical performance, adsorption performance, etc. It is currently the material with the fastest electrical conductivity, the highest mechanical strength, and the strongest thermal conductivity at room temperature. Due to these physical properties, graphene is widely used Used in many fields, such as: sensors, catalysis, energy materials, etc.; magnetic materials are ancient and widely used functional materials, and magnetic iron oxide nanoparticles smaller than 20 nm have superparamagnetism at room temperature. According to these characteristics, magnetic iron oxide nanoparticles have shown attractive application prospects in magnetic separation, magnetic monitoring, nuclear magnetic resonance, dru...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/194
Inventor 周立何本钊黄佳昌
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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