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Controllable preparation method of carboxyl functionalized carbon nanotube

A carboxyl-functionalized, carbon nanotube technology, applied in the fields of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of low concentration of functional groups, difficult processing steps, and damage to the structure of carbon nanotubes, etc. To achieve the effect of uniform pipe diameter distribution, easy expansion of scale, and simple and easy-to-obtain raw materials

Inactive Publication Date: 2014-11-05
BEIJING WANYUAN IND +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

First, the carbon nanotube internal sp 2 The hybridized lattice structure is destroyed, and the introduction of a large number of lattice defects leads to a great decrease in the conductivity of carbon nanotubes; secondly, the truncated carbon nanotubes pile up together, which increases the contact resistance between carbon nanotubes, and the electrode The internal resistance increases; again, the carbon nanotubes treated with strong oxidizing acid are very easy to agglomerate during the drying process, which brings difficulties to the subsequent processing steps; finally, even if the carbon nanotubes are treated with a strong oxidant for a long time, the functional groups on the surface Concentrations are still low (10 -9 ~10 -7 mol / m 2 ) (Langmuir, 2009, Vol 25, Pages: 7573-7577; Energy & Environmental Science, 2011, Vol 4, Pages: 4220-4229)
Attempts to increase the concentration of functional groups on the surface of carbon nanotubes by prolonging the oxidation time will seriously damage the structure of carbon nanotubes (J. Power Sources, 2006, 158, Pages: 1517-1522), thereby further improving the capacitance of carbon nanotube electrodes. come difficult

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  • Controllable preparation method of carboxyl functionalized carbon nanotube
  • Controllable preparation method of carboxyl functionalized carbon nanotube
  • Controllable preparation method of carboxyl functionalized carbon nanotube

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031]Weigh 2.741 grams of ferrocenedicarboxylic acid, add 100 grams of tetrachlorethylene and stir to form a uniform solution, transfer the solution into a stainless steel reaction kettle with a polytetrafluoroethylene substrate, and then raise the temperature to 160°C for 24 hours of constant temperature reaction. After the reaction, the filtered black product was washed three times with distilled water and ethanol in sequence, and finally placed in a vacuum drying oven at 100° C. for 12 hours to obtain the final product.

[0032] The scanning electron microscope (SEM) image of the final product is as Figure 1a As shown, under low magnification, the product is composed of a large number of one-dimensional fibrous structures, the thickness of which is between 30-50 nm and the distribution is relatively uniform. Figure 1a The upper right inset is a high magnification view of the port of the 1D fiber structure, showing that the 1D fiber structure is a hollow tubular structure i...

Embodiment 2

[0036] Weigh 0.372 grams of ferrocene and 2.193 grams of ferrocene dicarboxylic acid, add 100 grams of tetrachloroethylene and stir to form a uniform solution, transfer the solution into a stainless steel reaction kettle with a polytetrafluoroethylene substrate, and then heat up to 160 ° C for constant temperature reaction 24 hours. After the reaction, the filtered black product was washed three times with distilled water and ethanol in sequence, and finally placed in a vacuum drying oven at 100° C. for 12 hours to obtain the final product.

[0037] Similar to Example 1, SEM and TEM observations show that the final product is composed of a large number of one-dimensional tubular nanostructures, and FT-IR characterization results show that there are a large number of carboxyl groups in the product. The carboxyl concentration on the surface of the prepared carboxyl-modified carbon nanotubes was further determined by fluorescent labeling titration, Figure 2b Medium 0.8C 0 The ...

Embodiment 3

[0040] Weigh 0.744 grams of ferrocene and 1.645 grams of ferrocene dicarboxylic acid, add 100 grams of tetrachlorethylene and stir to form a uniform solution, transfer the solution into a stainless steel reaction kettle with a polytetrafluoroethylene substrate, and then heat up to 160°C for constant temperature reaction 24 hours. After the reaction, the filtered black product was washed three times with distilled water and ethanol in sequence, and finally placed in a vacuum drying oven at 100° C. for 12 hours to obtain the final product.

[0041] Similar to Example 1, SEM and TEM observations show that the final product is composed of a large number of one-dimensional tubular nanostructures, and FT-IR characterization results show that there are a large number of carboxyl groups in the product. Figure 2b Medium 0.6C 0 Curve corresponds to the fluorescence spectrum of the product obtained in Example 3, and the corresponding carbon tube surface carboxyl concentration is 2.06nm...

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Abstract

The invention discloses a controllable preparation method of a carboxyl functionalized carbon nanotube. The highest carboxyl concentration can reach 3.45nmol / cm<2> and can be randomly adjusted by changing the proportion of reactants. The method comprises the following concrete steps: weighing a cyclopentadienyl complex and carboxyl derivatives of the cyclopentadienyl complex; dissolving in an organic solvent; hermetically heating; filtering; washing; drying in vacuum and the like. The carboxyl modified carbon nanotube prepared by adopting the method is relatively high in purity and uniform in tube diameter distribution, and both the specific surface area and the carbon nanotube surface carboxyl concentration of the carboxyl modified carbon nanotube greatly exceed those of a carbon nanotube treated with a strong oxidant. The method for preparing the carboxyl modified carbon nanotube is low in energy consumption, high in efficiency, free of an additional catalyst and easy and feasible; raw materials are simple and easily available; the carboxyl modified carbon nanotube can be subjected to large-scale continuous production and is easy for large-scale production and suitable for industrialized production.

Description

technical field [0001] The invention belongs to the technical field of preparation of energy storage materials, and in particular relates to a bottom-up controllable method for preparing carboxyl-functionalized carbon nanotubes. Background technique [0002] The development of modern society depends on the supply of energy. At present, the main sources of energy in human society, such as coal, oil and other fossil energy sources, are increasingly depleted and the serious climate and environmental problems caused by large-scale use force people to turn to solar energy, Development and utilization of "clean energy" represented by wind energy and biomass energy. As a result, a new energy industry with broad market prospects and huge scale has emerged. Among them, electrochemical supercapacitors have attracted much attention due to their high-efficiency and fast charge-discharge performance. Unlike the energy conversion mechanism of the battery, which is mainly based on the sl...

Claims

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Application Information

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IPC IPC(8): C01B31/02B82Y40/00B82Y30/00
Inventor 沈健民马锐曹炬方臻
Owner BEIJING WANYUAN IND
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