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Superparamagnetic composite material of carbon nanotube coated coupling agent and preparation method thereof

A carbon nanotube and superparamagnetic technology, which is applied in the manufacture of magnetic materials, magnetic objects, inductors/transformers/magnets, etc., can solve the problems of difficult recycling of carbon nanotubes, high cost, and expensive medicines, and achieve excellent adsorption. and separation process, excellent magnetic properties, beneficial effect of adsorption

Inactive Publication Date: 2014-12-03
LANZHOU UNIVERSITY OF TECHNOLOGY
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Problems solved by technology

[0003] At present, it has been reported that the method of using precursor reduction to obtain ferric oxide has the disadvantages of expensive medicines, difficult control of the operation process, and high cost.
However, the reported method of directly loading MTPs directly with carbon nanotubes purified by hydrofluoric acid has the disadvantages that carbon nanotubes are not easy to recycle, and ferroferric oxide is easy to oxidize and change color in aqueous solution, causing environmental pollution and other hazards.

Method used

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  • Superparamagnetic composite material of carbon nanotube coated coupling agent and preparation method thereof
  • Superparamagnetic composite material of carbon nanotube coated coupling agent and preparation method thereof

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preparation example Construction

[0018] The preparation method of the superparamagnetic composite material of the above-mentioned carbon nanotube coating coupling agent, its steps are:

[0019] (1) Disperse carbon nanotubes CNTs in a mixed acid solution with a ratio of concentrated sulfuric acid and concentrated nitric acid of 3:1, react at 60-80°C for 1-3 hours for pretreatment, then filter, wash and dry for later use;

[0020] (2) Add pretreated multi-walled carbon nanotubes to a solution of ferrous ammonium sulfate and ferric ammonium sulfate with a mass ratio of 0.68. After ultrasonic oscillation for 10 minutes, add ammonia water drop by drop to control the pH at 11-12. Stir at a temperature of 40-60°C for 30-60 minutes, and the mass ratio of pretreated multi-walled carbon nanotubes to ferrous ammonium sulfate is 1:2-1:10;

[0021] (3) After the reaction, use a magnet to separate the generated magnetic multi-walled carbon nanotubes, and dry them in a vacuum oven at 60-100°C for 6-10 hours to obtain MagCNT...

Embodiment 1

[0026] Step 1 carbon nanotubes (CNTs) pretreatment:

[0027] Disperse 2g of carbon nanotubes CNTs into a mixed acid solution of 60ml of concentrated sulfuric acid and 20ml of concentrated nitric acid, stir and react at 60-80°C for 1-3 hours; wash with distilled water until pH = 7; vacuum dry at 80°C for 12 hours before use.

[0028] Step 2 Preparation of superparamagnetic carbon nanotube material MagCNTs:

[0029] Add 0.5 g of pretreated carbon nanotubes to a solution of 0.85 g ferrous ammonium sulfate and 1.25 g ferric ammonium sulfate, vibrate and sonicate for 10 minutes; add 8 mol / L ammonia solution dropwise, and control the pH of the mixed solution at 11-12; The generated superparamagnetic carbon nanotube material was separated from the suspension with a magnet, washed 5 times with distilled water; vacuum-dried at 80°C for 8 hours, and ground for later use to obtain the superparamagnetic carbon nanotube material MagCNTs. Such as figure 1 As shown, about 20nm ...

Embodiment 2

[0033] Step 1 Carbon Nanotubes (CNTs) Pretreatment:

[0034] Disperse 1g of carbon nanotubes CNTs into a mixed acid solution of 30ml of concentrated sulfuric acid and 10ml of concentrated nitric acid, stir and react at 60-80°C for 1-3 hours; wash with distilled water until pH = 7; vacuum dry at 80°C for 12 hours before use.

[0035] Step 2 Preparation of superparamagnetic carbon nanotube material MagCNTs:

[0036] Add 1 g of pretreated carbon nanotubes to a solution of 1.7 g of ferrous ammonium sulfate and 2.5 g of ferric ammonium sulfate, oscillate and sonicate for 10 minutes; add 6 mol / L ammonia solution dropwise, and control the pH of the mixed solution at 11 -12; use a magnet to separate the generated superparamagnetic carbon nanotube material from the suspension, wash 5 times with distilled water; vacuum-dry at 90°C for 8 hours, grind for later use after drying, and obtain superparamagnetic carbon nanotube material MagCNTs.

[0037] Step 3 Preparation of supe...

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Abstract

Provided are a superparamagnetic composite material of a carbon nanotube coated coupling agent and a preparation method thereof. The surfaces of CNTs (carbon nanotubes) are covered with a superparamagnetic iron oxide nanoparticle layer respectively, and the surface of the magnetic nanoparticle layer is modified with a silane coupling agent film. The preparation method includes the steps of (1) dispersing the CNTs in a mixed acid solution of concentrated sulfuric acid and concentrated nitric acid at the ratio of 3:1 for pretreatment reaction at the temperature of 60 DEG C to 80 DEG C; (2) adding the pre-treated multi-walled CNTs in an ammonium iron sulfate solution, dropwise adding aqueous ammonia and stirring at the temperature of 40 DEG C to 60 DEG C; (3) separating the generated magnetic multi-walled CNTs with a magnet after the reaction and drying in vacuum at the temperature of 60 DEG C to 100 DEG C; (4) dispersing the magnetic carbon nanotube material in anhydrous ethanol, adding acetic acid and 3-mercaptopropyl trimethoxysilane, stirring at the temperature of 30 DEG C to 60 DEG C, adding acetone for reacting for 3 hours, performing centrifugal separation and drying in vacuum at the temperature of 40 DEG C to 80 DEG C to obtain the material.

Description

technical field [0001] The invention belongs to the field of nanocomposite materials, in particular to a method for preparing a superparamagnetic composite material in which carbon nanotubes are coated with a coupling agent. Background technique [0002] Carbon nanotubes with excellent adsorption properties have been used to remove environmental pollutants. However, the possible nanotoxic effects of carbon nanotubes have attracted widespread attention from scholars. Therefore, the effective separation of carbon nanotubes from media is a key issue that cannot be ignored. Conventional centrifugation and filtration methods cannot achieve good solid-liquid separation, and magnetic separation technology has attracted more and more attention because of its high efficiency, rapidity, and economy. Carbon nanotube / iron oxide composites have attracted much attention due to their dual properties of carbon nanotubes and iron oxide magnetic nanoparticles. Cheng Zhang, Jiehe Sui, Jing Li...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01F1/00H01F41/00
Inventor 姜丽丽侯新刚李树军周晓蒙于海涛
Owner LANZHOU UNIVERSITY OF TECHNOLOGY
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