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Amino- and thiol-modified magnetic carbon nanotube composite material and preparation method

A technology of magnetic carbon nanotubes and carbon nanotubes, which is applied in the field of nanomaterials, can solve the problems of low efficiency of functional groups, poor dispersion of carbon nanotubes, and low degree of functionalization, and achieve simple process, favorable adsorption, and excellent magnetic properties. Effect

Active Publication Date: 2017-02-22
LANZHOU UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to solve the shortcomings of poor dispersion of carbon nanotubes, low efficiency of introducing functional groups, and low degree of functionalization

Method used

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  • Amino- and thiol-modified magnetic carbon nanotube composite material and preparation method
  • Amino- and thiol-modified magnetic carbon nanotube composite material and preparation method
  • Amino- and thiol-modified magnetic carbon nanotube composite material and preparation method

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preparation example Construction

[0017] The preparation method of the magnetic carbon nanotube composite material modified by amino group and thiol group, the steps are:

[0018] (1) Disperse the carbon nanotubes into the mixed acid solution, react at 60-80°C for 1-3 hours for pretreatment, then filter, wash and dry for later use;

[0019] (2) Add pretreated carbon nanotubes to the solution containing ferrous ions and ferric ions. After ultrasonic oscillation for 10-30 minutes, add ammonia water drop by drop to control the pH at 11-12. Stir for 30 to 60 minutes, wherein the mass ratio of the pretreated carbon nanotubes to ammonium ferrous sulfate is 1:2 to 1:10;

[0020] (3) Separate the generated magnetic carbon nanotubes with a magnet, and dry them in a vacuum oven at 60-120°C for 6-20 hours to obtain superparamagnetic carbon nanotube materials;

[0021] (4) Disperse the supermagnetic carbon nanotube material in absolute ethanol, stir mechanically under the protection of nitrogen, add acetic acid and 3-mer...

Embodiment 1

[0030] Step 1 carbon nanotube pretreatment:

[0031] Disperse 1g of original multi-walled carbon nanotubes (prepared by chemical vapor deposition) into a mixed acid solution of 60ml concentrated sulfuric acid and 20ml concentrated nitric acid, stir and react at 60°C for 3 hours, wash with distilled water until pH = 7, and vacuum dry at 80°C Reserve after 12 hours.

[0032] Step 2 Preparation of superparamagnetic carbon nanotube material MagCNTs:

[0033] 0.1 g of pretreated multi-walled carbon nanotubes were added to a mixed solution of 0.17 g ferrous ammonium sulfate and 0.25 g ferric ammonium sulfate, and ultrasonically oscillated for 10 minutes; 8 mol / L ammonia solution was added dropwise, and the mixed solution was The pH is controlled at 11-12; the generated superparamagnetic carbon nanotube material is separated from the suspension with a magnet, washed 5 times with distilled water; vacuum-dried at 80 degrees for 8 hours, dried and ground for later use to obtain superpa...

Embodiment 2

[0039] Step 1 carbon nanotube pretreatment:

[0040] Put 0.3g of original multi-wall carbon nanotubes (prepared by chemical vapor deposition) into a sand core funnel with a pore size of 20-30 microns, and place the sand core funnel with original multi-wall carbon nanotubes in a volume of 50 ml In the Teflon container, there is 3ml of concentrated nitric acid at the bottom of the Teflon container, put the Teflon container into a reaction kettle with a volume of 100ml, seal it, and then put it into the drying box, the temperature of the drying box is 200°C, duration is 5 hours. Take out the reaction kettle to cool to room temperature, open the reaction kettle and take out the sand core funnel, put the carbon nanotubes into a clean beaker, dilute with 100ml of distilled water, pour the diluted carbon nanotubes into a 10 cm diameter beaker with ordinary filter paper Wash the funnel 10 times with water and absolute ethanol until the pH of the washing water is close to neutral. Th...

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Abstract

The invention relates to an amino-modified and thiol-group-modified magnetic carbon nanotube composite material and a preparation method thereof and aims to overcome the defects of poor dispersity, low introduction efficiency of functional groups and low degree of functionalization of carbon nanotubes. The composite material adopts a tubular structure, ferroferric oxide particles with the diameters being 10-20nm are uniformly deposited on the surfaces of the carbon nanotubes, and the outer surfaces of the ferroferric oxide nano-particles and the carbon nanotubes are coated with a layer of 5-10nm of film containing amino and thiol groups. The method comprises the following steps: dispersing the carbon nanotubes into a solution containing ferrous and ferric iron ions, adding ammonia water, and thus obtaining a ferroferric oxide / carbon nanotube composite material with superparamagnetism; after magnetic separation, dispersing into a mixed solution containing acetic acid, acetone and trimethoxysilylpropanethiol; after reaction, centrifugally separating and drying, and then dispersing into an ethanol solution; adding hydrazine under the protection of nitrogen; after reaction, respectively washing with water and ethanol; after vacuum drying, obtaining the amino-modified and thiol-group-modified magnetic carbon nanotube composite material.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, and in particular relates to a magnetic carbon nanotube composite material modified by amino groups and thiol groups and a preparation method thereof. Background technique [0002] After the Japanese electron microscope scientist Iijima S first discovered carbon nanotubes in 1991, the material has a unique hollow tubular structure, excellent electrical conductivity, large specific surface area, light mass density, and strong interaction with pollutant molecules. It quickly attracted the attention of scholars in various fields at home and abroad. However, due to the surface hydrophobicity and ultra-high surface energy of carbon nanotubes, they are easy to agglomerate and entangle with each other, and are not easily soluble in various solvents, which greatly limits their application. In order to improve the dispersion of carbon nanotubes and improve their application ability, chemical ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/20B01J20/28B01J20/30
CPCB01J20/22B01J20/28009
Inventor 姜丽丽于海涛侯新刚李树军周晓蒙李传通姚夏妍
Owner LANZHOU UNIVERSITY OF TECHNOLOGY
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