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Method for preparing multi-wall carbon nanotubes

A technology of multi-walled carbon nanotubes and active components, applied in the direction of multi-walled carbon nanotubes, carbon nanotubes, nanocarbons, etc., can solve the problems of inability to obtain high specific surface area and high-purity multi-walled carbon nanotubes, Achieve the effect of low cost, good effect and wide source of raw materials

Inactive Publication Date: 2019-04-23
CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The invention provides a method for preparing multi-walled carbon nanotubes to solve the problem that the existing multi-walled carbon nanotubes preparation process cannot obtain multi-walled carbon nanotubes with small diameter, high specific surface area and high purity characteristics

Method used

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  • Method for preparing multi-wall carbon nanotubes
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  • Method for preparing multi-wall carbon nanotubes

Examples

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Embodiment 1

[0056] Use Fe, Co, Al and Mg nitrates and urea to prepare 0.3mol / L mixed salt solution and 10mol / L alkaline solution, wherein the atomic ratio of Fe and Co is 10:1, and the atomic ratio of Mg and Al Ratio is at 2, and the consumption of urea is 15 times (mol ratio) of metal ion, and the content of active component is 15% of catalyst gross weight, and above-mentioned two kinds of solutions are mixed at room temperature, under stirring state, with 3 ℃ / The temperature was slowly raised to 103° C. at a rate of 1 min, and the stirring was continued for 12 h, and then the reaction was stopped. The resulting suspension was placed in an oven at 95° C. for 12 h, then cooled and filtered, washed three times with deionized water, and freeze-dried. The catalyst was loaded into a fixed-bed reactor, and first reduced with nitrogen containing 30% hydrogen at 800°C for 10 min. Then the gas was switched to 100% methane and reacted at 800 °C for 1 h. Switch the gas to nitrogen, and cool down...

Embodiment 2

[0058] Use Fe, Ni, Al and Mg sulfate and urea to prepare 0.2mol / L mixed salt solution and 10mol / L alkaline solution, wherein the atomic ratio of Fe and Ni is 12:1, and the atomic ratio of Mg and Al Ratio is at 3, and the consumption of urea is 18 times (molar ratio) of metal ion, and the content of active component is 12% of catalyst gross weight, and above-mentioned two kinds of solutions are mixed at room temperature, under agitation, with 3 ℃ / Slowly raise the temperature to 100°C at a rate of min, continue to keep stirring for 12 hours, and then stop the reaction. The resulting suspension was placed in an oven at 95° C. for 12 h, then cooled and filtered, washed three times with deionized water, and freeze-dried. The catalyst was loaded into a fixed-bed reactor, and first reduced with nitrogen containing 30% hydrogen at 760°C for 10 min. Then the gas was switched to 100% natural gas, and the reaction was carried out at 760° C. for 1 h. Switch the gas to nitrogen, and coo...

Embodiment 3

[0060] Use Fe, Co, Al and Mg nitrate and ammonium molybdate to make 0.15mol / L mixed salt solution, use ammonium bicarbonate and ammonium carbonate to make 2mol / L alkaline precipitant solution, in which Fe, Co The atomic ratio of Mo and Mo is 10:1:0.5, the atomic ratio of Mg and Al is 2, the consumption of ammonium bicarbonate and ammonium carbonate is 2 times (molar ratio) of metal ion, and the content of active component is 1% of the total weight of catalyst 15%, add the mixed salt solution dropwise to the stirring alkaline precipitant solution. After the dropwise addition, slowly raise the temperature to 80°C at a rate of 3°C / min, continue to keep warm and stir for 2h, and then stop the reaction. The suspension was left to stand in an oven at 90° C. for 12 h, then cooled and filtered, washed three times with deionized water, and freeze-dried. The catalyst was loaded into a fixed-bed reactor, and first reduced with nitrogen containing 20% ​​hydrogen at 780° C. for 5 minutes. ...

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Abstract

The invention relates to a preparation method of multi-wall carbon nanotubes, in particular to a method for directly preparing multi-wall carbon nanotubes with high specific surface area by using a chemical vapor deposition method. The method comprises the steps of preparing a catalyst with excellent catalytic performance by adopting a precipitation freeze-drying method, and cracking C1 hydrocarbon to grow carbon nanotubes in a reactor by using the catalyst. The specific surface area of the multi-walled carbon nanotubes directly prepared by the method is as high as 800-900 m<2> / g, the tube diameter distribution is in a range of 3-5 nm, the length distribution is in the range of several to dozens of micrometers, the purity of a crude product can be greater than or equal to 90 wt%, the purity can further be greater than or equal to 98 wt% after simple pickling, and the obtained carbon nanotubes have the advantages of high quality, low cost and easiness in operation and implementation.

Description

technical field [0001] The invention relates to the technical field of carbon nanotube preparation, in particular to a method for preparing multi-walled carbon nanotubes. Background technique [0002] Carbon nanotubes (Carbon Nanotube, CNT) have attracted much attention for their excellent electrical conductivity, thermal conductivity, mechanical properties and chemical stability. [0003] Similar to the sheet structure of graphite, the carbon atoms in the carbon nanotube structure are sp 2 Hybridization, each carbon atom has an unpaired electron located on the π orbital perpendicular to the sheet, so carbon nanotubes have good electrical properties. Theoretical calculations show that the electronic properties of carbon nanotubes are closely related to the structure of CNTs. The conductivity of carbon nanotubes depends on its diameter and the helix angle of the tube wall. Its conductivity can exhibit properties similar to metals (metallic carbon nanotubes), or it can exhib...

Claims

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Application Information

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IPC IPC(8): C01B32/162B01J23/755B01J23/75B01J27/236B01J37/32B01J37/08B01J35/02
CPCC01B32/162B01J23/75B01J23/755B01J27/236B01J37/08B01J37/32C01B2202/30C01B2202/36C01B2202/34C01B2202/32C01B2202/06B01J35/00B01J35/30
Inventor 姜锦锦张焕刘文静刘建平瞿美臻汪镭
Owner CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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