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Method for preparing nitrogen-phosphorus codoped multi-walled carbon nanotube

A technology of multi-walled carbon nanotubes and co-doping, which is applied in the direction of nanotechnology, can solve the problem of preparation of multi-walled carbon nanotubes without nitrogen and phosphorus co-doping, does not involve nitrogen-phosphorus co-doped multi-walled carbon nanotubes, does not involve Chemical vapor deposition and other problems, to achieve the effect of simple method, high output and strong operation controllability

Inactive Publication Date: 2011-05-18
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

Japanese Invention Patent Publication No. 101450799 discloses a graphite arc discharge method for preparing nitrogen-doped carbon nanotubes. This patent does not involve the preparation of nitrogen-phosphorous co-multiwalled carbon nanotubes, nor does it involve the chemical vapor deposition method used in the present invention (CVD method); there is no report on the preparation of nitrogen and phosphorus co-doped multi-walled carbon nanotubes

Method used

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  • Method for preparing nitrogen-phosphorus codoped multi-walled carbon nanotube
  • Method for preparing nitrogen-phosphorus codoped multi-walled carbon nanotube
  • Method for preparing nitrogen-phosphorus codoped multi-walled carbon nanotube

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Embodiment 1

[0027] 1) Pave the bottom with 0.1g of FeMo / Al 2 o 3 Put the catalyst quartz boat into the high-temperature part of the quartz tube in the tube furnace, and raise the temperature of the high-temperature part of the quartz tube to 700°C under the protection of argon inert gas with a flow rate of 1.0L / min;

[0028] 2) Add 8mL of toluene to the container bottle, and then slowly add triphenylphosphine, wherein the amount of triphenylphosphine is 2.5wt% toluene; after the triphenylphosphine is completely dissolved, replace the argon gas with a flow rate of 200ml / min Ammonia, under the ammonia atmosphere, inject the mixed solution into the quartz tube through a constant flow pump at a flow rate of 2mL / h. After the solution is vaporized, it is brought to the high temperature area by the ammonia gas. Carbon source toluene, nitrogen source ammonia and phosphorus The source triphenylphosphine is decomposed, and the solid catalyst FeMo / Al 2 o 3 Under the action, nitrogen and phosphoru...

Embodiment 2

[0031] 1) Pave the bottom with 0.1g of FeMo / Al 2 o 3 Put the catalyst quartz boat into the high-temperature part of the quartz tube in the tube furnace, and raise the temperature of the high-temperature part of the quartz tube to 700°C under the protection of argon inert gas with a flow rate of 1.0L / min;

[0032] 2) Add 10mL of toluene to the container bottle, and then slowly add triphenylphosphine, wherein the amount of triphenylphosphine is 5wt% toluene; after the triphenylphosphine is completely dissolved, replace the argon gas with a flow rate of 400ml / min Ammonia, under an ammonia atmosphere, inject the mixed solution into the quartz tube through a constant flow pump at a flow rate of 3mL / h. After the solution is vaporized, it is brought to the high temperature area by argon. Carbon source toluene, nitrogen source ammonia and phosphorus The source triphenylphosphine is decomposed, and the solid catalyst FeMo / Al 2 o 3 Under the action, nitrogen and phosphorus co-doped m...

Embodiment 3

[0035] 1) Pave the bottom with 0.1g of FeMo / Al 2 o 3 Put the catalyst quartz boat into the high-temperature part of the quartz tube in the tube furnace, and raise the temperature of the high-temperature part of the quartz tube to 800°C under the protection of argon inert gas with a flow rate of 1.3L / min;

[0036] 2) Add 12mL of toluene to the container bottle, and then slowly add triphenylphosphine, wherein the amount of triphenylphosphine is 10wt% toluene; after the triphenylphosphine is completely dissolved, replace the argon gas with a flow rate of 500ml / min ammonia Under the atmosphere of ammonia gas, inject the mixed solution into the quartz tube at a flow rate of 3mL / h through a constant flow pump. After the solution is vaporized, it is brought to the high temperature area by ammonia gas. Triphenylphosphine decomposes on the solid catalyst FeMo / Al 2 o 3 Under the action, nitrogen and phosphorus co-doped multi-walled carbon nanotubes began to grow;

[0037] 4) After t...

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Abstract

The invention provides a method for preparing a nitrogen-phosphorus codoped multi-walled carbon nanotube, comprising the following steps: putting a quartz boat in which a FeMo / Al2O3 catalyst is laid on the bottom into the high temperature zone of a quartz tube in a tube furnace and heating the high temperature zone of the quartz tube to the reaction temperature in the presence of argon gas; adding toluene and triphenylphosphorus to a container bottle; after the triphenylphosphorus is dissolved completely, injecting the mixed solution into the quartz tube by a constant flow pump in the presence of ammonia; after the solution is gasified, taking the gasified solution to the high temperature zone by ammonia; decomposing carbon source toluene, nitrogen source ammonia and phosphorus source triphenylphosphorus in the presence of a solid catalyst FeMo / Al2O3; starting to grow the nitrogen-phosphorus codoped multi-walled carbon nanotube; after the solution is completely injected, stopping introducing the ammonia into the quartz tube; cooling the quartz tube to room temperature in the presence of argon; and taking out samples from the quartz boat to obtain the prepared nitrogen-phosphorus codoped multi-walled carbon nanotube.

Description

technical field [0001] The invention relates to a preparation method of nitrogen and phosphorus co-doped multi-wall carbon nanotubes. Background technique [0002] Since the discovery of carbon nanotubes (CNTs) in 1991, it has become a research hotspot of nanomaterials worldwide. Most of the research is focused on exploring various new technologies to prepare high-purity carbon nanotubes with controllable structure. Studies have shown that chemical vapor deposition (CVD) is currently the most valuable preparation method for industrial applications. This quasi-one-dimensional nanomaterial not only has the high specific surface area of ​​traditional carbon materials, relative chemical inertness, surface modification, and easy recovery of loaded metals, but also due to the confinement effect produced by its unique nanotube lumen, it can be used in catalytic field has attracted widespread attention. For example, due to the catalytic effect of special functional groups on the ...

Claims

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Application Information

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IPC IPC(8): C01B31/02B82Y40/00
Inventor 刘滋武彭峰王红娟余皓杨剑
Owner SOUTH CHINA UNIV OF TECH
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