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Carbon nano-tube preparation method

A carbon nanotube, acetate technology, applied in nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problem of uneven diameter of carbon nanotubes, unfavorable industrial production, and length of carbon nanotubes. uncontrollable issues

Active Publication Date: 2015-12-23
WUXI DONGHENGNEWENERGYTECHNOLOGYCO LTD
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Problems solved by technology

In summary, the disadvantages of the above-mentioned method are mainly: 1. mainly use transition metal ions (Ni, Co, Mo) as catalysts, involving the use of multiple toxic substances; It is easy to cause environmental damage; 3. The diameter of carbon nanotubes is uneven, the diameter distribution is wide, and contains a large amount of amorphous carbon; 4. The oxidation resistance of carbon nanotubes is poor and the degree of graphitization is low; 5. The length of carbon nanotubes is uncontrollable 6. Carbon nanotubes have high ash content and low purity; 7. Carbon nanotubes contain insoluble catalyst supports such as silicon salts, making purification difficult; 8. Carbon nanotubes have low packing density and high production cost, which is not conducive to industrial production

Method used

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preparation example Construction

[0021] A method for preparing carbon nanotubes proposed by the present invention includes the following steps or operations.

[0022] In step 1, nitrate or acetate of Fe, Al, and Mg are used as raw materials, citric acid is used as complexing agent and pore-forming agent, and water is added and mixed to form a solution.

[0023] In one embodiment, this step can be specifically performed as follows: using nitrate or acetate of Fe, Al, and Mg as raw materials, using citric acid as a complexing agent and pore-forming agent, adding water and mixing to form a solution , wherein, the nitrate or acetate of Fe, the nitrate or acetate of Al, the nitrate or acetate of Mg, the molar ratio of these four kinds of substances of citric acid are Fe:Al:Mg=1: x:y, 0.1≤x≤3, 0.1≤y≤3; citric acid / (Fe+Al+Mg)=z, 1≤z≤3.

[0024] In step 2, the above solution is calcined to prepare a catalyst, the structural formula of which is FeAlxMgyO, x=0.1-3, y=0.1-3.

[0025] In one embodiment, this step can b...

Embodiment 1

[0030] Weigh 202kgFe(NO 3 ) 3 9H 2 O, 318.86kgAl (NO 3 ) 3 9H 2 O, 12.82kgMg(NO 3 ) 2 9H 2 0, 537.99kg anhydrous citric acid, 720kg deionized water, pour into the reactor and stir to make it fully dissolved. 100°C oil bath heating, 85r / min mechanical stirring. Stir and heat to evaporate until the viscosity of the solution reaches 100mPas, then roast the solution in a tunnel kiln at 500°C under air atmosphere for 3 hours to obtain FeAl 1.7 Mg 0.1 o 4.15 catalyst.

[0031] Use an automatic feeding system to push each crucible filled with 6g of catalyst powder continuously into the reaction zone of a tube furnace at 700°C, and adjust the ethylene flow rate by 5m 3 / h, hydrogen flow rate 1m 3 / h, set the program so that the residence time of each crucible in the reaction zone is 30min, push out the crucible and cool it under the protection of nitrogen atmosphere. see Figure 1-Figure 3 , figure 1 is made of FeAl1.7 Mg 0.1 o 4.15 A 100,000-fold scanning electron m...

Embodiment 2

[0034] Weigh 202kgFe(NO 3 ) 3 9H 2 O, 93.78kgAl(NO 3 ) 3 9H 2 O, 192.11kgMg (NO 3 )2·9H 2 O, 288.21kg anhydrous citric acid, 1620kg deionized water, pour into the reactor and stir to make it fully dissolved. 100°C oil bath heating, 85r / min mechanical stirring. Stir and heat to evaporate until the viscosity of the solution reaches 100mPas, then roast the solution in a tunnel kiln at 400°C under air atmosphere for 1 hour to obtain FeAl 0.1 Mg 1.5 o 3.15 catalyst.

[0035] Use an automatic feeding system to push each crucible filled with 6g of catalyst powder continuously into the reaction zone of a tube furnace at 500°C, and adjust the ethylene flow rate by 1m 3 / h, hydrogen flow rate 1m 3 / h, set the program so that the residence time of each crucible in the reaction zone is 20min, push out the crucible and cool it under the protection of nitrogen atmosphere. The yield of carbon nanotubes can be 2400%, the tube diameter is 15-20nm, and the ratio is 201-223㎡ / g.

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Abstract

The present invention discloses a carbon nano-tube preparation method, which comprises: adopting nitrates or acetates of three substances such as Fe, Al and Mg as raw materials, adopting citric acid as a complexing agent and a pore-forming agent, adding water, and mixing to form a solution; calcining the solution to prepare a catalyst, wherein the structure general formula of the catalyst is FeAlxMgyO, x is 1-3, and y is 0.1-1; and carrying out catalytic cracking on any one of methane, ethylene or propylene with the catalyst to obtain the carbon nano-tubes. The preparation method of the present invention has characteristics of carbon nano-tube bulk density improving, yield increase and production cost reducing.

Description

technical field [0001] The invention relates to the technical field of carbon nanotube production, in particular to a method for preparing carbon nanotubes. Background technique [0002] At present, the mainstream of industrial carbon nanotube products is multi-walled carbon nanotubes. The principle of its preparation is to use high-power energy input to make the carbon in the carbon-containing raw materials self-organize into regularly arranged tubes. According to factors such as energy input methods and carbon source materials, there are currently three mainstream preparation methods: graphite arc method, laser evaporation method and chemical vapor deposition method. Both the graphite arc method and the laser evaporation method use physical means such as electric arc or laser to locally introduce extremely high power to rearrange the atomic structure of carbon. Since the local temperature will be as high as 3000-4000°C during the action process, which is conducive to the ...

Claims

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Application Information

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IPC IPC(8): C01B31/02B82Y40/00B82Y30/00
Inventor 万仁涛沈宇栋
Owner WUXI DONGHENGNEWENERGYTECHNOLOGYCO LTD
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