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Method for preparing primary amine carbon nano tube

A technology of carbon nanotubes and nanotubes, which is applied in the field of chemically modifying the surface of carbon nanotubes and carbon nanotubes. It can solve the problems of complex steps, harsh reaction conditions, and inability to guarantee amino groups, etc., and achieves simple steps, high reactivity, and extensive use. The effect of applying the foreground

Inactive Publication Date: 2008-05-14
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The present invention overcomes the shortcomings of harsh reaction conditions and complicated steps in the existing carbon nanotube modification technology, especially solves the problem that the current method cannot guarantee that the amino group on the modification must be a primary amino group

Method used

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  • Method for preparing primary amine carbon nano tube
  • Method for preparing primary amine carbon nano tube
  • Method for preparing primary amine carbon nano tube

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] as attached figure 1 Shown: the first step: mix 500mg SWNT (diameter 1~2nm, purity greater than 90%) with 150ml H 2 SO 4 with HNO 3 mixed solution (98%H 2 SO 4 : 68% HNO 3 = 3:1 vol / vol), and reflux reaction for 4 hours at 35-40° C. and 50 kHz ultrasonic oscillation. Then filter through a vinylidene fluoride membrane with a pore size of 0.45 μm, and wash with water until the pH is neutral. The product was placed in a vacuum oven and dried under vacuum at 40°C for 24h. The above carboxylated and washed product was placed in H 2 SO 4 with H 2 o 2 mixed solution (98%H 2 SO 4 : 30%H 2 o 2 =4:1vol / vol) at 70°C for 2h. Then filter through a vinylidene fluoride membrane with a pore size of 0.45 μm, and wash with water until the pH is neutral. The product was placed in a vacuum oven and dried under vacuum at 40°C for 24h. The infrared spectrum of the product is attached figure 2 shown.

[0021] The second step: take 85 mg of the above-mentioned carboxylated ...

Embodiment 2

[0024] See Example 1 for the first step, and the second step: take 85 mg of the above-mentioned acidified carbon nanotubes and place them in a reaction flask, add 120 mg of di-tert-butyl dicarbonate, 114 mg of sodium azide, and 24.15 mg of tetrabutylammonium bromide, Zinc bromide 7.425mg, tetrahydrofuran 100ml, stirred and refluxed at 40°C for 24h. Filtered and washed several times with THF. Carbon nanotubes bearing tert-butyl carbamate were obtained.

[0025] Step 3: Add 50 mg of carbon nanotubes with tert-butyl carbamate into a mixed solution of 10 ml of hydrochloric acid and 20 ml of ethyl acetate, stir, and react at room temperature for 2 hours to stop the reaction. Filter through a vinylidene fluoride membrane, wash with water, and filter through a fiber membrane with a pore size of 0.45 μm to obtain a black powder.

Embodiment 3

[0027] See Example 1 for the first step, and the second step: take 85 mg of the above-mentioned acidified carbon nanotubes and place them in a reaction flask, add 120 mg of di-tert-butyl dicarbonate, 114 mg of sodium azide, and 24.15 mg of tetrabutylammonium bromide, Zinc trifluoromethanesulfonate 12mg, tetrahydrofuran 100ml, stirred and refluxed at 40°C for 24h. Filtered and washed several times with THF. Carbon nanotubes bearing tert-butyl carbamate were obtained.

[0028]Step 3: Add 50 mg of carbon nanotubes with tert-butyl carbamate into a mixed solution of 10 ml of hydrochloric acid and 20 ml of ethyl acetate, stir, and react at room temperature for 2 hours to stop the reaction. Filter through a vinylidene fluoride membrane, wash with water, and filter through a fiber membrane with a pore size of 0.45 μm to obtain a black powder.

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Abstract

The invention relates to a preparation method for primary amine modified carbon nano-tubes (CNT). Firstly, the carbon nano-tubes (CNT) with carboxyl at surface are obtained after acid treatment of the carbon nano-tubes (CNT). Carboxyl carbon nano-tubes (CNT), di-tert-butyl dicarbonate and sodium azide are reacted under the composite catalysis of phase-transfer metal catalyst and Lewis acid to obtain the carbon nano-tubes (CNT) with carbamic tert-butyl. Then the tert-butyl group is lost in hydrochloric ethyl acetate solution to generate the carbon nano-tubes (CNT) with primary amine group. Compared with other methods, the carbon nano-tubes (CNT) prepared with the invention has higher primary amine level, and can be used as an important reaction intermediate as well as be compounded with polymers to obtain composite materials with high performance.

Description

technical field [0001] The invention belongs to the field of materials, and relates to carbon nanotubes, in particular to a method for chemically modifying the surface of carbon nanotubes. Background technique [0002] Since Lijima discovered carbon nanotubes in 1991, carbon nanotubes have been a research hotspot in recent years because of their unique structure, good electrical properties and mechanical properties. Carbon nanotubes have nanoscale diameters and micron-scale lengths, and the aspect ratio can reach 100-1000. They are extremely strong and have ideal elastic modulus. They are an excellent fiber material, and their performance is better than any current fiber. Therefore, it can be used as a superfiber for the reinforcement of advanced composite materials; because carbon nanotubes combine the semi-metallic properties of graphite with the quantum laws of energy levels and electronic waves, and have nanoscale dimensions, making them in the field of electronics The ...

Claims

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Application Information

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IPC IPC(8): C01B31/02B82B3/00
Inventor 王国建屈泽华
Owner TONGJI UNIV
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