A kind of carbon nanotube produced in situ and its preparation method and application

A technology of carbon nanotubes and reactions, applied in the field of carbon nanotubes generated in situ and its preparation, to achieve good dispersion, good catalytic reduction effect, and high mechanical strength

Active Publication Date: 2019-11-22
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

A large number of literatures report that carbon nanotubes are excellent catalysts for this type of reaction, but the price of carbon nanotubes makes their use as a catalyst daunting

Method used

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  • A kind of carbon nanotube produced in situ and its preparation method and application
  • A kind of carbon nanotube produced in situ and its preparation method and application
  • A kind of carbon nanotube produced in situ and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Embodiment 1: the synthesis of cross-linked polymer

[0062] In a 250mL beaker, add 100mL of cross-linking agent acetylacetone, and then add metal donor nickel acetylacetonate 0 / 50 / 100 / 250 / 500 / 1000 / 2000mg, fully sonicate until the nickel acetylacetonate is completely dissolved, then shake it vigorously at room temperature The reaction was stirred and 15 g NaOH was added rapidly. After 30 min, when the reaction solution became viscous, the stirring reaction was stopped. After the reaction, the reaction solution was left at room temperature for one week.

[0063] The reaction formula is as follows:

[0064]

[0065] figure 1 It is a Fourier transform infrared spectrum (FT-IR) figure of the polymer precursor; As can be seen from the figure, the reaction mechanism of the polymer precursor obtained meets the mechanism of assumption;

[0066] figure 2 is a scanning electron microscope (SEM) image of the polymer precursor; it can be seen from the figure that the obtai...

Embodiment 2

[0067] Embodiment 2: the preparation of carbon nanotube

[0068] The cross-linked polymer obtained in Example 1 is transferred to a porcelain boat, dried in an oven at 80°C for 12 hours, and then placed in a tube furnace. / 5 / 10 min -1 The heating rate is increased to the annealing temperature (respectively 400 / 500 / 600 / 700 / 800 / 900°C) under the protection of high-purity nitrogen for annealing, the annealing time is 0.5 / 1 / 2 / 4 / 6h, and then cooled to 50℃, the cooling rate is 5℃min -1 . Afterwards, the obtained carbon material was ground and ultrasonically dispersed in deionized water, filtered with suction, and rinsed with a large amount of deionized water. Afterwards, the filter cake was dried in an oven at 80° C. for 12 hours to obtain a carbon material with a purity of 80%. It can be seen from Table 1-3 that the inner diameter of the obtained carbon nanotubes is 5-30nm, the outer diameter is 10-50nm, the length is 20-200um, and the specific surface area is 50-200m 2 g -1 ,...

Embodiment 3

[0077] Embodiment 3: the reduction of p-nitrophenol

[0078] 13 mg of p-nitrophenol was dissolved in 2 mL of deionized water, and then 4 mg of the carbon nanotubes prepared in Example 2 were added as a catalyst. After sufficient ultrasonication for 15 min, 50 mg of sodium borohydride was added. To measure the rate of the reaction, pipette the reaction solution at 10uL min -1 Dilute it in 10 mL of deionized water, and then use a UV-visible spectrophotometer to measure the reaction effect.

[0079] Figure 8 It is the UV spectrum of in situ generated carbon nanotubes catalyzing the reduction of 4-nitrophenol; it can be seen from the figure that after 12 minutes, the reaction is complete. , to obtain pure 4-aminophenol. White crystals, melting point: 189-189.6°C. NMR spectrum (such as Figure 11 shown): 1 H NMR (600 MHz, DMSO) δ8.33 (s, 1H), 6.53–6.45 (m, 2H), 6.45–6.37 (m, 2H), 4.37 (s, 2H). Figure 12 shown): 13 C NMR (151MHz, DMSO) δ148.43, 140.52, 115.70, 115.54. GC-MS...

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Abstract

The invention discloses in-situ generated carbon nanotubes as well as a preparation method and application thereof. A carbon nanotube material is generated in situ by annealing a cross-linked polymerobtained by taking acetylacetone and acetylacetone nickel to be subjected to aldol condensation reaction under the action of strong alkali, i.e., sodium hydroxide. The carbon nanotube material has theinner diameter of 5 to 30nm, the outer diameter of 10 to 50nm, the length of 20 to 200mu m, the specific surface area of 50 to 200m<2>g<-1> and the electrical conductivity of 30 to 400Scm<-1>. By utilizing the method disclosed by the invention, the carbon nanotubes with a long size, good dispersity in a solution and excellent electron conduction effect can be produced in a large batch. Furthermore, the prepared carbon nanotubes have a very good effect of catalyzing the reduction of 4-nitrophenol.

Description

technical field [0001] The invention belongs to the field of carbon materials, and relates to an in-situ generated carbon nanotube and its preparation method and application. Background technique [0002] Since the first observation of carbon nanotubes in 1991 by Japan's NEC Electric Company using a high-resolution transmission electron microscope, research on carbon nanotubes has flourished. Carbon nanotubes are hollow tubular carbon nanomaterials with a high aspect ratio. From a structural point of view, carbon nanotubes are formed by two-dimensional graphene curling along a certain direction, and different layers of graphene will be rotated to obtain Carbon nanotubes with different wall numbers. With its unique hollow tubular structure and excellent mechanical, thermal, electrical and optical properties, carbon nanotubes are widely used in many fields such as chemistry, chemical engineering, physics, biology, medicine, and environmental science. After more than 20 years...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/16C07C213/02C07C215/76B01J21/18
CPCB01J21/185C01B32/16C01B2202/22C01B2202/32C01B2202/34C01B2202/36C07C213/02C07C215/76
Inventor 梁琼麟艾永建
Owner TSINGHUA UNIV
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