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Method for purification of low-purity single-wall carbon nano-tubes

A technology of single-walled carbon nanotubes and a purification method, which is applied in the field of purification of low-purity single-walled carbon nanotubes, can solve the problems of low purification efficiency, long purification period, and difficulty in SWNTs purification, etc., and achieves the effect of small structural damage.

Inactive Publication Date: 2012-06-27
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these methods can obtain SWNTs with high purity, they have the disadvantages of severe SWNTS structural damage, low purification efficiency, and long purification cycle.
Especially in terms of the purification degree of SWNTs, it is difficult to achieve effective purification of SWNTs using existing purification techniques

Method used

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  • Method for purification of low-purity single-wall carbon nano-tubes
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  • Method for purification of low-purity single-wall carbon nano-tubes

Examples

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Effect test

Embodiment 1

[0028] according to figure 1 In the flow chart shown, 0.5g of low-purity SWNTs initial product was oxidized in air at 370°C for 30 minutes, then added to 2wt% SDS solution for 30 minutes of ultrasonication, and then the uniformly dispersed SWNTs aqueous solution was centrifuged at 9000rpm for 30 minutes; The supernatant was supernatant and ultrasonicated again for 10min, and then centrifuged at 12000rpm for 60min; the obtained single-walled carbon nanotube scanning electron microscope picture was as follows Figure 6 shown. Next, the centrifuged SWNTs supernatant hydraulic filter was washed to remove the SDS surfactant; then the SWNTs product that was filtered out was mixed with 100ml H 2 o 2 Mix and heat at 100°C for 5h. Finally, the SWNTs solution was suction-filtered to neutral and dried to obtain pure SWNTs. Figure 2-5 They are scanning electron microscope photos and transmission electron microscope photos before and after purification, respectively. It can be seen fr...

Embodiment 2

[0030] according to figure 1 In the flow chart shown, 1 g of low-purity SWNTs initial product was oxidized in air at 360°C for 60 minutes, then added to 2wt% SDBS solution for 60 minutes of ultrasonication, and then the uniformly dispersed SWNTs aqueous solution was centrifuged at 6000 rpm for 50 minutes; after centrifugation, the supernatant was taken out liquid and supernatant was ultrasonicated again for 15min, and then centrifuged at 14000rpm for 30min; Figure 7 shown. Next, the SWNTs supernatant hydraulic filter after centrifugation is washed to remove SDBS surfactant; then the SWNTs product that is filtered out is mixed with 200ml 2 o 2 Mix and heat at 100°C for 4h. Finally, the SWNTs solution was suction-filtered to neutral and dried to obtain pure SWNTs. It can be seen from the scanning electron microscope photos of the products obtained under different centrifugation speeds that choosing different centrifugation speeds can effectively remove impurity particles, w...

Embodiment 3

[0032] according to figure 1 In the flow chart shown, 1.2g of low-purity SWNTs initial product was oxidized in air at 400°C for 30 minutes, then added to 1wt% SDS solution for 30 minutes of ultrasonication, and then the uniformly dispersed SWNTs aqueous solution was centrifuged at 6000rpm for 40 minutes; Supernatant and supernatant were sonicated again for 20min, and then centrifuged at 12000rpm for 30min; then the centrifuged SWNTs supernatant was hydraulically filtered to remove the SDS surfactant; 2 o 2 Mix and heat at 100°C for 8h. Finally, the SWNTs solution was suction-filtered to neutral and dried to obtain pure SWNTs.

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Abstract

The invention relates to a method for purification of low-purity single-wall carbon nano-tubes. The method provided by the invention can realize purification of low-purity single-wall carbon nano-tubes by atmospheric oxidation, ultrasonic dispersion, centrifugal separation at different speeds, and hydrogen peroxide refluxing. Concretely, the method provided by the invention comprises the following steps of adding single-wall carbon nano-tube products subjected to atmospheric oxidation into a surfactant solution, carrying out ultrasonic dispersion, carrying out low-speed centrifugal separation and high-speed centrifugal separation to remove impurity particles, carrying out pressure filtration of the supernatant obtained by the high-speed centrifugal separation, mixing the filtrate and hydrogen peroxide, carrying out addition refluxing of the mixture, and carrying out vacuum filtration, flushing and drying to obtain the low-purity single-wall carbon nano-tubes. Compared with the prior art, the method provided by the invention avoids that waste liquid pollution is produced because of single utilization of hydrochloric acid in catalyst removal, and realizes removal of a catalyst according to a principle that the increasing of the weight of an oxidized catalyst is conducive to centrifugal separation. In purification, the centrifugal separation is a main process and oxidation adopting a weak oxidant H2O2 is an auxiliary process and thus the damage on a structure of the single-wall carbon nano-tube is small.

Description

technical field [0001] The invention belongs to the technical field of carbon nanotube technology, and in particular relates to a method for purifying low-purity single-walled carbon nanotubes. Background technique [0002] Carbon Nanotubes (CNTs) is a new type of hollow tubular nanostructure formed by bending two-dimensional graphene sheets, and is the fourth important allotrope of carbon besides graphite, diamond, and fullerene. Multi-walled carbon nanotubes (MWNTs) were first discovered by Professor Iijima Sumio (Iijima) in arc discharge cathode deposits in 1991, especially two years later single-walled carbon nanotubes (Single- The discovery of walled carbon nanotubes (SWNTs) has aroused widespread attention in many fields including physics, chemistry, and materials science. [0003] DC arc discharge method is a high-efficiency preparation technology of high-quality SWNTs. The prepared SWNTs have the advantages of high crystallinity, less defects, and high electron mobi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02B82Y40/00C01B32/159C01B32/17
Inventor 张亚非苏言杰张丽玲魏浩杨志
Owner SHANGHAI JIAO TONG UNIV
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