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Method for preparing multi-walled carbon nanotubes from phthalocyanine iron polymer by high temperature solid-phase cracking

A technology of multi-wall carbon nanotubes and high-temperature solid phase, applied in the field of nanomaterials, can solve the problems of high yield, unguaranteed, low carbon residue rate, etc., and achieve the effect of simple preparation method, high production rate, and high carbon residue rate

Inactive Publication Date: 2011-03-16
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Most of the carbon sources mentioned above have the disadvantage of low carbon residue rate after high-temperature roasting, so that a high yield cannot be guaranteed.

Method used

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  • Method for preparing multi-walled carbon nanotubes from phthalocyanine iron polymer by high temperature solid-phase cracking
  • Method for preparing multi-walled carbon nanotubes from phthalocyanine iron polymer by high temperature solid-phase cracking
  • Method for preparing multi-walled carbon nanotubes from phthalocyanine iron polymer by high temperature solid-phase cracking

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1 Using bis-phthalonitrile as the initial carbon source and carbonyl iron powder as the catalyst, carbon nanotubes were prepared by a solid-phase cracking method.

[0033] 1. Weigh 10 grams of bisphthalonitrile monomer and 0.6 grams of carbonyl iron powder, put them into a three-necked bottle, pour 15ml of N-methylpyrrolidone as a solvent; heat up to 200°C, and reflux for 4 hours.

[0034] 2. Pour the solution into water, filter, wash the filtered solid with deionized water 2 to 3 times, dry and collect.

[0035] 3. The samples collected in step 2 were cured according to the following procedure at 50°C for 4 hours, at 280°C for 4 hours, and at 300°C for 50 hours.

[0036] 4. Introduce nitrogen, then step 3, the initial temperature is 300°C, and rise to 350°C at a heating rate of 5°C / min (constant temperature for 1 hour); 5°C / min to 400°C (constant temperature for 1 hour); 3°C / min to 500°C (constant temperature for 4 hours); 2°C / min to 800°C (constant temperatu...

Embodiment 2

[0039] Example 2 Using bis-phthalonitrile as the initial carbon source and nano-iron powder as the catalyst, carbon nanotubes were prepared by a solid-phase cracking method.

[0040] 1. Weigh 10 grams of bisphthalonitrile monomer and 0.2 grams of nano-iron powder, put them into a three-necked bottle, and pour 15ml of N-methylpyrrolidone as a solvent. Raise the temperature to 200°C and reflux for 4 hours.

[0041] 2. Pour the solution into water, filter, wash the filtered solid with deionized water 2 to 3 times, dry and collect.

[0042] 3. The samples collected in step 2 were cured according to the following procedure at 50°C for 4 hours, at 280°C for 4 hours, and at 300°C for 50 hours.

[0043] 4. Introduce nitrogen, then step 3, the initial temperature is 300°C, and rise to 350°C at a heating rate of 5°C / min (constant temperature for 1 hour); 5°C / min to 400°C (constant temperature for 1 hour); 3°C / min to 500°C (constant temperature for 4 hours); 2°C / min to 800°C (constant...

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Abstract

The invention discloses a method for preparing multi-walled carbon nanotubes from phthalocyanine iron polymer by high temperature solid-phase cracking, belongs to the technical field of nanomaterials, and provides a simple, high-efficiency and low-cost method for preparing the multi-walled carbon nanotubes. The method comprises the following steps of: performing reflux reaction on bisphthalonitrile and an iron-based catalyst in N-methylpyrrolidone solvent to generate a phthalocyanine iron oligomer; heating and curing the phthalocyanine iron oligomer to obtain the phthalocyanine iron polymer; and finally performing the high temperature solid-phase cracking on the phthalocyanine iron polymer under the protection of an inert gas to obtain the multi-walled carbon nanotubes. By using the two iron-based catalysts of carbonyl iron powder and iron nanopowder, the hollow carbon nanotubes and the carbon nanotubes of which the cores are filled with iron nanopowder can be obtained respectively. The multi-walled carbon nanotubes prepared by the method has high purity, uniform tube diameter and length and can be widely applied to the high-technology fields such as various composite materials, microelectronics and the like.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials and relates to a preparation method of carbon nanotubes. Background technique [0002] Nanomaterials, known as important materials in the 21st century, are also expected to be one of the four pillars of the future intelligent society. In 1991, Dr. S. Iijima, an electron microscope expert at the basic research laboratory of NEC Corporation of Japan, discovered some tubes formed by nano-scale coaxial carbon atoms in the deposits formed after the discharge of graphite cathodes. Iijinma named it carbon nanometers. Tubes (Carbon Nanotubes, CNTs). Since the carbon-carbon bond that constructs the carbon nanotube structure is one of the strongest chemical bonds known in nature, carbon nanotubes have extremely high mechanical strength. According to calculations, their theoretical tensile strength should be 100 times that of steel, and their density is only 100 times that of steel. It is 1 / 6 o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02
Inventor 雷雅杰赵睿詹迎清孟凡彬钟家春刘孝波
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA
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