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Catalyst for preparing carbon nanometer pipe with small pipe diameter

A technology of carbon nanotubes and single-walled carbon nanotubes, which is applied in the field of inorganic material synthesis, can solve the problems of high degree of graphitization, changing the preparation conditions of carbon nanotubes, and inability to improve the yield and purity of single-walled carbon nanotubes

Inactive Publication Date: 2004-09-22
CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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  • Application Information

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Problems solved by technology

Changing the preparation conditions of carbon nanotubes cannot improve the yield and purity of single-walled carbon nanotubes
[0003] Small-diameter multi-walled carbon nanotubes (referring to carbon nanotubes with an outer diameter of less than 8 nanometers) have a high degree of graphitization and few defects, and have important application prospects in material reinforcement, electrical conductivity, or static electricity conduction. There is no catalytic cracking method yet. Literature Reports on Small Diameter Multi-walled Carbon Nanotubes

Method used

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  • Catalyst for preparing carbon nanometer pipe with small pipe diameter
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Embodiment 1

[0020] Catalyst composed of Co 0.1 Sr 0.04 Mo 0.05 Mg 0.94 O. Weigh 0.100 g of the catalyst and place it in a molybdenum boat, and the molybdenum boat is placed in the middle of a tubular reactor (35 mm in diameter). First pass nitrogen to remove the air, half an hour later, under the protection of nitrogen, start to heat up, and switch to the mixed gas of hydrogen and methane after reaching 750 °C, H 2 Flow 100ml / min, CH 4 The flow rate is 40ml / min. The heating rate was 5°C per minute. After reacting for 50 minutes, switch the mixed gas of hydrogen and methane to nitrogen, and cool to room temperature. Weighed 0.218 g of black product, yield 118%. After purification with nitric acid, the purity of the single-walled carbon nanotubes reaches 98% (weight percentage), and the yield is 0.106g. After Raman spectrum analysis, the diameters of the obtained single-wall carbon nanotubes are mainly concentrated in 1.1-1.5nm. The transmission electron microscope photo of the ob...

Embodiment 2

[0022] Catalyst composed of Co 0.04 Cu 0.02 Mo 0.01 Fe 0.01 Mg 0.94 O. Weigh 0.100 g of the catalyst and place it in a molybdenum boat, and the molybdenum boat is placed in the middle of a tubular reactor (35 mm in diameter). First pass nitrogen to remove the air, and after half an hour, start to heat up under the protection of nitrogen, and switch to pure methane after reaching 900°C, CH 4 The flow rate is 60ml / min. Cool to room temperature after reacting for 60 minutes. Weighed 0.233 g of black product, yield 133%. After purification with nitric acid, the purity of the single-walled carbon nanotubes reaches 95% (weight percentage), and the yield is 0.113g. After Raman spectrum analysis, the diameters of the obtained single-wall carbon nanotubes are mainly concentrated in 0.9-1.3nm.

Embodiment 3

[0024] Catalyst composed of Co 0.1 Ca 0.05 Mo 0.01 Mg 0.94 O. Weigh 0.100 g of the catalyst and place it in a molybdenum boat, and the molybdenum boat is placed in the middle of a tubular reactor (35 mm in diameter). First pass nitrogen to remove the air, half an hour later, under the protection of nitrogen, start to heat up, and switch to the mixed gas of hydrogen and methane after reaching 800°C. 2 Flow 40ml / min, CH 4 The flow rate is 80ml / min. The heating rate was 4°C per minute. After reacting for 50 minutes, switch the mixed gas of hydrogen and methane to nitrogen, and cool to room temperature. Weighed 0.603 g of black product, yield 503%. The purity of the small-diameter multi-walled carbon nanotubes obtained after purification with nitric acid reaches 96% (weight percentage), and the yield is 0.483g. Through transmission electron microscope observation, the outer diameter of carbon nanotubes is mainly concentrated in 3-8nm.

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Abstract

A catalyst for preparing the small-diameter single-wall or multi-wall carbon nanotubes from C-contained micro-molecular gas at 700-1100 deg.C contains carrier (magnesium oxide or aluminium oxide), active component (metal Co), the first cocatalyst (molybdenum oxide), and the second cocatalyst (the oxide of alkali-earth element, rare-earth element, or other elements). Its advantages are high output rate and high purity of nanotube (more than 90%).

Description

technical field [0001] The invention discloses a catalyst for preparing small-diameter carbon nanotubes (the outer diameter of the carbon nanotubes is less than 8 nanometers), belongs to the field of inorganic material synthesis, and is particularly suitable for preparing high-purity single-wall carbon nanotubes by a catalytic cracking method. Background technique [0002] Carbon nanotubes are a new type of high-tech nano-carbon material that has emerged since the 1990s. Among them, single-walled carbon nanotubes can best reflect the excellent performance of carbon nanotubes. At present, there are three main methods for preparing single-walled carbon nanotubes in the world: laser ablation method, arc method and catalytic cracking method. Only the catalytic cracking method has the most industrial application prospects, and its development research has attracted the most attention. The existing catalyst system for preparing single-walled carbon nanotubes by catalytic crackin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/882C01B31/02
Inventor 赵社涛瞿美臻周固民
Owner CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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