Method for amination of carbon nano tube

A carbon nanotube and amination technology, applied in the field of amination, can solve the problems of complex process and low efficiency of nitrogen-containing functional groups, and achieve the effect of simple process and high efficiency

Inactive Publication Date: 2010-07-14

HARBIN INST OF TECH

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AI-Extracted Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a method for the amination of carbon nanotubes in order to solve the problems of ...

Method used

Use Nicolet-Nexus 670 infrared spectrometer, characterize and analyze the carbon nanotube after the amination of the present embodiment, infrared spectrogram as shown in Figure 1, as can be seen from the figure at 1515cm-1 corresponds to- The NH bending vibration absorption peak shows that the method of this embodiment grafts ethylenediamine to carbon nanotubes with nitrogen atoms as amide groups. Use the PHI5700ESCA X-ray photoelectron spectrometer to characterize and analyze the aminated carbon nanotubes in this embodiment. The X-ray photoelectron spectrogram is shown in Figure 2. The Cls peak appears at the electron binding energy of 532eV, the O1s peak appears at the electron binding energy of 532eV, and the N1s peak appears at the electron binding energy of 399eV. The high temperature and high pressure reaction conditions of 350°C and 6.28MPa can break and decompose a large amount of -OH and -COOH, and some carboxyl groups are converted into amides, thereby greatly reducing the surface oxygen content and improving the efficiency of introducing nitrogen-containing functional groups. Wherein the content of C atoms in the carbon nanotubes obtained in this embodiment is 94.11%, the content of O atoms is 2.65%, and the content of N atoms is 3.24%, and the content of N atoms in the carbon nanotubes after amination in this embodiment is high.

Use Nicolet-Nexus 670 infrared spectrometer, characterize and analyze the ...

Abstract

The invention discloses a method for amination of a carbon nano tube, relating to a method for amination and solving the problems of complicated process and low nitrogenous functional group introduction efficiency of the existing method for modification of the carbon nano tube. The method is as follows: first, putting the pre-treated carbon nano tube into a supercritical reactor for reaction; and second, washing the products from the first step through distilled water and then vacuum drying under 55-65 DEG C. In this way, an aminated carbon nano tube can be prepared. The method is simple in process, and the analysis of the infrared spectrum diagram and infrared X-ray electron spectrum diagram of the aminated carbon nano tube prepared through the method shows that the nitrogenous functional group introduction efficiency through the method is high.

Application Domain

Bulk chemical production

Technology Topic

ChemistryCarbon nanotube +8

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Experimental program(8)

Example Embodiment

[0009] Specific embodiment 1: The method of amination of carbon nanotubes in this embodiment is carried out according to the following steps: 1. 0.2~0.5g of pretreated carbon nanotubes are put into a supercritical reactor, and then 20~24ml of Ammonia or 20-24ml of ethylenediamine, control the temperature of the supercritical reactor at 340~350℃, the pressure at 6~11MPa, and the reaction time at 2~4min. Cool the reactor with water; 2. Use the product after step 1 reaction After washing with distilled water, vacuum drying is carried out at 55-65°C to obtain aminated carbon nanotubes.

[0010] The method of this embodiment has a simple process. The aminated carbon nanotubes of this embodiment can be known by infrared spectroscopy, and there is obvious -CH on the carbon nanotubes infrared spectrogram. 2 , -C=O, -CNH absorption peaks, it can be inferred that the amine group is grafted onto the carbon nanotubes, and the aminated carbon nanotubes in this embodiment can be known from the red X-ray photoelectron spectroscopy. N appears in the red X-ray photoelectron spectrum 1s It can be seen that nitrogen atoms have been introduced on the surface of the carbon nanotubes, and the content of nitrogen atoms in the carbon nanotubes obtained in this embodiment has reached more than 3%. The nitrogen-containing functional groups introduced by the method of the present invention are efficient.

Example Embodiment

[0011] Specific embodiment two: This embodiment is different from specific embodiment one in that the pretreatment method in step one adopts purification treatment, and the specific operation is: burning carbon nanotubes at 300-400°C for 5-7h, namely The pretreated carbon nanotubes are obtained. Other steps and parameters are the same as in the first embodiment.

Example Embodiment

[0012] Specific embodiment three: this embodiment is different from specific embodiments one to two in that: in step one, the pretreatment of carbon nanotubes adopts an acid treatment method, and the specific operations are: a. The carbon nanotubes are burnt at 300-400°C 5~7h; b. Mix 250ml of mixed acid and 0.3~0.6g of the carbon nanotubes treated in step one under the conditions of frequency 80~100Hz and temperature 45~55℃ for 5~7h, where the mixed acid is concentrated H 2 SO 4 With concentrated HNO 3 The composition is in accordance with the volume ratio of 3:1; c. Wash with distilled water after ultrasound, and then filter with 0.45μm microporous membrane. The precipitate obtained by the suction filter is vacuum dried at 55~65℃ to obtain the pretreated For carbon nanotubes, the number of cleaning with distilled water is 3 to 5 times, and the standing time for each cleaning is 22 to 26 hours. The other steps and parameters are the same as those in the first to second embodiments.

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Classification and recommendation of technical efficacy words

Simple process
Improve efficiency

Method for amination of carbon nano tube

A carbon nanotube and amination technology, applied in the field of amination, can solve the problems of complex process and low efficiency of nitrogen-containing functional groups, and achieve the effect of simple process and high efficiency

AI-Extracted Technical Summary

Problems solved by technology

Method used

Abstract

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Examples

Example Embodiment

Example Embodiment

Example Embodiment

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Description & Claims & Application Information

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