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Method and device for preparing carbon nano tube by taking high-sulfur heavy oil as carbon source

A carbon nanotube and content technology, applied in nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of catalyst agglomeration, low carbon nanotube purity, and reduced product purity, etc. The effect of poisoning the catalyst

Active Publication Date: 2016-07-20
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, it has been reported that heavy oil residues similar to heavy oil, asphalt, etc., are used as carbon sources to prepare carbon materials such as carbon nanotubes or carbon microspheres, but there are many problems: the complexity of the carbon source components leads to low purity of the prepared carbon nanotubes, When carbon nanotubes are prepared by chemical vapor deposition, the high deposition temperature will easily lead to catalyst agglomeration and the presence of sulfur in the components will easily deactivate the catalyst.
However, there is a problem with this conventional tube furnace, that is, only one direction of ventilation is allowed, which inevitably leads to the entry of carbon source gas into the deposition area during the heating and cooling process, and the generation of impurities such as carbon deposits at non-preset temperatures , reducing the purity of the product
[0005] Catalysts used for traditional gaseous carbon sources, such as the silicon or copper sheet substrate catalysts of nickel-magnesium loaded as announced by a low-temperature preparation method of carbon nanotubes (application number CN201110187600.X), are not suitable for heavy oil carbon sources with high sulfur content, and Pre-desulfurization treatment of heavy oil with high sulfur content will increase the production cost and complicate the production process

Method used

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  • Method and device for preparing carbon nano tube by taking high-sulfur heavy oil as carbon source
  • Method and device for preparing carbon nano tube by taking high-sulfur heavy oil as carbon source
  • Method and device for preparing carbon nano tube by taking high-sulfur heavy oil as carbon source

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Experimental program
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Effect test

Embodiment 1

[0030] (1) 0.7275g (0.0025mol) of nickel nitrate hexahydrate and 4.8g (0.01875mol) of magnesium nitrate hexahydrate were dissolved in 50mL (0.8563mol) of absolute ethanol to obtain a catalyst precursor;

[0031] (2) Add the catalyst precursor at 2 μL / cm 2 The density is evenly sprayed on the 304 stainless steel substrate after ultrasonic cleaning with deionized water, and dried at 20 ° C to obtain a nickel-magnesium catalyst substrate;

[0032](3) The nickel-magnesium catalyst substrate is placed in the center of the high-temperature deposition area of ​​a dual-temperature zone horizontal tube furnace, and a small porcelain boat containing 0.1282g of Kuwait vacuum residue is placed in the dual-temperature zone horizontal tube furnace. In the center of the low-temperature vaporization zone of the type furnace, flanges with pipelines are used to close the two ends of the dual-temperature zone tube furnace; the composition of the vacuum residue in Kuwait is shown in Table 1;

[...

Embodiment 2

[0040] (1) 0.7275g (0.0025mol) nickel nitrate hexahydrate and 3.2g (0.0125mol) magnesium nitrate hexahydrate were dissolved in 40mL (0.6851mol) absolute ethanol to prepare a catalyst precursor;

[0041] (2) Add the catalyst precursor at 20 μL / cm 2 The density is evenly sprayed on the 304 stainless steel substrate after ultrasonic cleaning with deionized water, and dried at 30 ° C to obtain a nickel-magnesium catalyst substrate;

[0042] (3) Place the nickel-magnesium catalyst substrate in the center of the high-temperature deposition zone of a dual-temperature zone horizontal tube furnace, and place a small porcelain boat containing 0.35g of Tahe atmospheric residue in the dual-temperature zone horizontal furnace. In the center of the low-temperature vaporization zone of the tube furnace, flanges with pipelines are used to close both ends of the tube furnace with dual temperature zones; the composition of Tahe atmospheric residue oil is shown in Table 2;

[0043] (4) Use the ...

Embodiment 3

[0050] (1) 0.7275g (0.0025mol) of nickel nitrate hexahydrate and 3.84g (0.015mol) of magnesium nitrate hexahydrate were dissolved in 70mL (1.1988mol) of absolute ethanol to obtain a catalyst precursor;

[0051] (2) Add the catalyst precursor at 10 μL / cm 2 The density is evenly sprayed on the 304 stainless steel substrate after ultrasonic cleaning with deionized water, and dried at 35 ° C to obtain a nickel-magnesium catalyst substrate;

[0052] (3) The nickel-magnesium catalyst substrate is placed in the center of the high-temperature deposition area of ​​a dual-temperature zone horizontal tube furnace, and a small porcelain boat containing 0.1282g of Kuwait vacuum residue is placed in the dual-temperature zone horizontal tube furnace. In the center of the low-temperature vaporization zone of the tube furnace, use flanges with pipelines to close the two ends of the dual-temperature zone tube furnace;

[0053] (4) Use the hydrogen-argon mixed gas to discharge the closed air in...

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Abstract

The invention provides a method and device for preparing a carbon nano tube by taking high-sulfur heavy oil as a raw material, and belongs to the technical field of petrochemical industry and carbon materials.The invention provides a method for preparing the carbon nano tube by taking the heavy oil of which the mass fraction of sulfur ranges from 2.11% to 4.9% as a carbon source and taking a 304 stainless steel substrate of which the surface is loaded with nickel and magnesium oxide as a catalyst through a chemical vapor deposition method, and provides the device needed in preparing the carbon nano tube by taking the high-sulfur heavy oil as the carbon source simultaneously.The method and device for preparing the carbon nano tube by taking the high-sulfur heavy oil as the carbon source have the advantages that the prepared catalyst is suitable for directly preparing the carbon nano tube by taking the high-sulfur heavy oil as the raw material, the diameter of the prepared carbon nano tube ranges from 30 nm to 90 nm, the tube cavity is large, the tube wall is smooth, and the purity and the degree of graphitization are high; the method has the advantages that the raw materials are low in price and rich in source, the problem that high sulfur content in the carbon source makes the catalyst inactivated is solved, and a new way is provided for high value added utilization of the heavy oil.

Description

technical field [0001] The invention relates to the technical fields of petrochemical industry and carbon materials, in particular to a method and equipment for preparing carbon nanotubes by using heavy oil with high sulfur content as a carbon source. Background technique [0002] In 1991, Iijima, a scientist at the NEC Basic Laboratory in Japan, discovered a one-dimensional carbon nanotube with a seamless concentric cylindrical structure made of single-layer or multi-layer graphene. Due to their unique one-dimensional structure, carbon nanotubes have excellent mechanical, electrical, thermal, optical and reactive properties, and have great applications in the fields of energy storage and conversion, composite materials, heterogeneous catalysis, environmental protection and biomedicine. use potential. At present, gases such as methane and acetylene are usually used as carbon sources in the commercial preparation of carbon nanotubes. These carbon sources have disadvantages s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02B82Y30/00B82Y40/00B01J23/755B01J21/10
CPCB01J21/10B01J23/755C01P2002/82C01P2004/03C01P2004/04C01P2004/64
Inventor 陈旭申建洲杨文胜
Owner BEIJING UNIV OF CHEM TECH
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