CN115254133A - Preparation method of supported high-conductivity carbon nanotube catalyst - Google Patents

Preparation method of supported high-conductivity carbon nanotube catalyst Download PDF

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CN115254133A
CN115254133A CN202210531145.9A CN202210531145A CN115254133A CN 115254133 A CN115254133 A CN 115254133A CN 202210531145 A CN202210531145 A CN 202210531145A CN 115254133 A CN115254133 A CN 115254133A
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heating
flask
carbon nanotube
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张韬
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Hubei Guanyu New Material Technology Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/85—Chromium, molybdenum or tungsten
    • B01J23/88—Molybdenum
    • B01J23/887—Molybdenum containing in addition other metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
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    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
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    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/0201—Impregnation
    • B01J37/0213—Preparation of the impregnating solution
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    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/0236—Drying, e.g. preparing a suspension, adding a soluble salt and drying
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    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment
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    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
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    • C01B32/16—Preparation
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    • B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
    • C—CHEMISTRY; METALLURGY
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    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties

Abstract

The invention discloses a preparation method of a supported high-conductivity carbon nano tube catalyst, which comprises the steps of preparing a nitrate solution, adding an oxide carrier, heating and drying for the second time, roasting and screening. The conductivity of the carbon nano tube produced by the method is greatly improved from 4000s/m to 8000s/m, and the conductive effect is improved by 100%. Meanwhile, compared with a coprecipitation production method, the method for preparing the catalyst by using the load method has a simpler production process, can greatly improve the yield of the catalyst and reduce the production cost.

Description

Preparation method of supported high-conductivity carbon nanotube catalyst
Technical Field
The invention relates to the technical field of preparation of carbon nanotubes, in particular to a preparation method of a supported high-conductivity carbon nanotube catalyst.
Background
The catalyst is an original material for producing the carbon nano tube, the carbon nano tube is a key raw material added in the composite material, and the electrical conductivity, the tensile resistance and the dispersion performance of the carbon nano tube in the composite material are important indexes for checking the carbon nano tube.
The prior art adopts a coprecipitation method to prepare the carbon nanotube catalyst, and has the defects of low catalyst yield, easy occurrence of a precipitation phenomenon of the catalyst during coprecipitation, and difficult control of mutual combination between an active substance and a carrier, so that the carbon nanotube produced by the catalyst has low quality and poor conductivity. In addition, the co-precipitation method requires a plurality of complicated steps, and the process is complex, thereby affecting the production efficiency.
Disclosure of Invention
The invention aims to overcome the problems and provides a preparation method of a supported high-conductivity carbon nanotube catalyst. In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a supported high-conductivity carbon nanotube catalyst comprises the following steps:
s1, preparing nitrate solution
Mixing 9.1g Co (NO)3)2·6H2O、0.89g(NH4)6Mo7O24、0.22gNH4VO3Completely dissolved in a flask A of 100ml of pure water;
s2, adding an oxide carrier
Flask A was charged with 12.5g of amorphous α -Al2O3Adding the mixture into a flask A;
s3, heating and dipping
Putting the flask A into a constant-temperature water bath kettle, heating and stirring for 60min to fully immerse the oxide carrier in the nitrate solution;
s4, secondary heating and drying
After the impregnation is finished, putting the mixture into a vacuum evaporation device, and heating, rotating and stirring for 60min;
s5, roasting
After evaporation, putting the material into a muffle furnace to be roasted for 60min at 350 ℃, then gradually increasing the temperature to 720 ℃ at the heating rate of 10 ℃/min, and roasting for 180min;
s6, screening
And screening the product, and sieving the product by a sieve of 60-200 meshes to obtain a finished product.
As an improvement, the amorphous α -Al2O3Average particle diameter D of50v=73 μm and a specific surface area of 0.5m2/g。
As a modification, the temperature of the water bath heating in the S3 step is 100 ℃.
As a modification, the temperature of the secondary heating in S4 is 60 ℃.
The invention has the advantages that:
the conductivity of the carbon nano tube produced by the method is greatly improved from 4000s/m to 8000s/m, and the conductive effect is improved by 100%. Meanwhile, compared with a coprecipitation production method, the method for preparing the catalyst by using the loading method has a simpler production process, can greatly improve the yield of the catalyst and reduce the production cost.
Drawings
FIGS. 1, 2 and 3 show the appearance of carbon nanotubes prepared by the present invention under different magnifications;
FIG. 4 is an appearance of a catalyst prepared according to the present invention.
Detailed Description
The present invention will be described in detail and specifically with reference to the following examples so as to facilitate the understanding of the present invention, but the following examples do not limit the scope of the present invention.
Example 1
The embodiment discloses a preparation method of a supported high-conductivity carbon nanotube catalyst, which comprises the following steps:
s1, preparing nitrate solution
Mixing 9.1g of Co (NO)3)2·6H2O、0.89g(NH4)6Mo7O24、0.22gNH4VO3Completely dissolved in a flask A of 100ml of pure water;
s2, adding an oxide carrier
Flask A was charged with 12.5g of amorphous α -Al2O3(average particle diameter D)50v=73 μm and a specific surface area of 0.5m2Per gram) is added into the flask A;
s3, heating and dipping
Putting the flask A into a constant-temperature water bath kettle, heating and stirring at 100 ℃ for 60min to fully impregnate the oxide carrier with the nitrate solution;
s4, secondary heating and drying
After the impregnation is finished, putting the mixture into a vacuum evaporation device, and heating, rotating and stirring the mixture for 60min at the temperature of 60 ℃;
s5, roasting
After evaporation, putting the material into a muffle furnace to be roasted for 60min at 350 ℃, then gradually increasing the temperature to 720 ℃ at the heating rate of 10 ℃/min, and roasting for 180min;
s6, screening
And screening the product, and sieving the product by a sieve with 60-200 meshes to obtain a finished product.
Comparative example 1
The embodiment discloses a preparation method of a supported high-conductivity carbon nanotube catalyst, which comprises the following steps:
s1, preparing nitrate solution
Mixing 9.1g Co (NO)3)2·6H2O、0.89g(NH4)6Mo7O24、0.22gNH4VO3Completely dissolved in a flask A of 100ml of pure water;
s2, adding an oxide carrier
Flask A was charged with 12.5g of amorphous α -Al2O3(average particle diameter D)50v=73 μm, specific surface area 0.5m2Per gram) is added into the flask A;
s3, heating and dipping
Putting the flask A into a constant-temperature water bath kettle, heating and stirring at 100 ℃ for 60min to fully impregnate the oxide carrier with the nitrate solution;
s4, secondary heating and drying
After the impregnation is finished, putting the mixture into a vacuum evaporation device, and heating, rotating and stirring the mixture for 60min at the temperature of 60 ℃;
s5, roasting
After the evaporation is finished, putting the material into a muffle furnace, roasting for 60min at 350 ℃, then gradually increasing the temperature to 500 ℃ at the heating rate of 10 ℃/min, and roasting for 180min;
s6, screening
And screening the product, and sieving the product by a sieve with 60-200 meshes to obtain a finished product.
Comparative example 2
The embodiment discloses a preparation method of a supported high-conductivity carbon nanotube catalyst, which comprises the following steps:
s1, preparing nitrate solution
Mixing 9.1g of Co (NO)3)2·6H2O、0.89g(NH4)6Mo7O24、0.22gNH4VO3Completely dissolved in a flask A of 100ml of pure water;
s2, adding an oxide carrier
Flask A was charged with 12.5g of amorphous α -Al2O3(average particle diameter D)50v=73 μm and a specific surface area of 0.5m2Per gram) is added into the flask A;
s3, heating and dipping
Putting the flask A into a constant-temperature water bath kettle, heating and stirring at 100 ℃ for 60min to fully impregnate the oxide carrier with the nitrate solution;
s4, secondary heating and drying
After the impregnation is finished, putting the mixture into a vacuum evaporation device, and heating, rotating and stirring the mixture for 60min at the temperature of 60 ℃;
s5, roasting
After the evaporation is finished, putting the material into a muffle furnace, roasting for 60min at 350 ℃, then gradually increasing the temperature to 600 ℃ at the heating rate of 10 ℃/min, and roasting for 180min;
s6, screening
And screening the product, and sieving the product by a sieve with 60-200 meshes to obtain a finished product.
Comparative example 3
The embodiment discloses a preparation method of a supported high-conductivity carbon nanotube catalyst, which comprises the following steps:
s1, preparing nitrate solution
Mixing 9.1g Co (NO)3)2·6H2O、0.89g(NH4)6Mo7O24、0.22gNH4VO3Completely dissolved in a flask A of 100ml of pure water;
s2, adding an oxide carrier
To flask A was added 12.5g of spherical alpha-Al2O3(average particle diameter D)50v=73 μm and a specific surface area of 1m2Per g) addition ofIn a flask A;
s3, heating and dipping
Putting the flask A into a constant-temperature water bath kettle, heating and stirring at 100 ℃ for 60min to fully impregnate the oxide carrier with the nitrate solution;
s4, secondary heating and drying
After the impregnation is finished, putting the mixture into a vacuum evaporation device, and heating, rotating and stirring the mixture for 60min at the temperature of 60 ℃;
s5, roasting
After evaporation, putting the material into a muffle furnace to be roasted for 60min at 350 ℃, then gradually increasing the temperature to 720 ℃ at the heating rate of 10 ℃/min, and roasting for 180min;
s6, screening
And screening the product, and sieving the product by a sieve with 60-200 meshes to obtain a finished product.
Comparative example 4
The embodiment discloses a preparation method of a supported high-conductivity carbon nanotube catalyst, which comprises the following steps:
s1, preparing nitrate solution
Mixing 9.1g of Co (NO)3)2·6H2O、0.89g(NH4)6Mo7O24、0.22gNH4VO3Completely dissolved in a flask A of 100ml of pure water;
s2, adding an oxide carrier
Flask A was charged with 12.5g of amorphous gamma-Al2O3(average particle diameter D)50v=73 μm and a specific surface area of 200m2Per gram) is added into the flask A;
s3, heating and dipping
Putting the flask A into a constant-temperature water bath kettle, heating and stirring at 100 ℃ for 60min to fully impregnate the oxide carrier with the nitrate solution;
s4, secondary heating and drying
After the impregnation is finished, putting the mixture into a vacuum evaporation device, and heating, rotating and stirring the mixture for 60min at the temperature of 60 ℃;
s5, roasting
After evaporation, putting the material into a muffle furnace to be roasted for 60min at 350 ℃, then gradually increasing the temperature to 720 ℃ at the heating rate of 10 ℃/min, and roasting for 180min;
s6, screening
And screening the product, and sieving the product by a sieve of 60-200 meshes to obtain a finished product.
The results obtained are shown in the following table:
Figure BDA0003646282550000051
it can be concluded from the above table that the baking temperature has a large influence on the yield of carbon nanotubes and a small influence on the conductivity of the produced carbon nanotubes, and that the large difference in the use of different carriers has a large influence on both the yield and the conductivity. The carrier and reaction conditions used in example 1 are most favorable.
The embodiments of the present invention have been described in detail above, but they are merely exemplary, and the present invention is not equivalent to the embodiments described above. Any equivalent modifications and substitutions to those skilled in the art are also within the scope of the present invention. Therefore, equivalent changes and modifications made without departing from the spirit and scope of the present invention should be covered in the present invention.

Claims (4)

1. A preparation method of a supported high-conductivity carbon nanotube catalyst is characterized by comprising the following steps:
s1, preparing nitrate solution
Mixing 9.1gCO (NO)3)2·6H2O、0.89g(NH4)6Mo7O24、0.22gNH4VO3Completely dissolved in a flask A of 100ml of pure water;
s2, adding an oxide carrier
Flask A was charged with 12.5g of amorphous α -Al2O3Adding the mixture into a flask A;
s3, heating and dipping
Putting the flask A into a constant-temperature water bath kettle, heating and stirring for 60min to fully immerse the oxide carrier in the nitrate solution;
s4, secondary heating and drying
After the impregnation is finished, putting the mixture into a vacuum evaporation device, and heating, rotating and stirring for 60min;
s5, roasting
After the evaporation is finished, putting the material into a muffle furnace, roasting for 60min at 350 ℃, then gradually increasing the temperature to 720 ℃ at the heating rate of 10 ℃/min, and roasting for 180min;
s6, screening
And screening the product, and sieving the product by a sieve of 60-200 meshes to obtain a finished product.
2. The method for preparing the supported high-conductivity carbon nanotube catalyst as claimed in claim 1, wherein the amorphous α -Al is2O3Average particle diameter D of50v=73 μm and a specific surface area of 0.5m2/g。
3. The method for preparing the supported highly conductive carbon nanotube catalyst according to claim 1, wherein the temperature of the water bath heating in the step S3 is 100 ℃.
4. The method as claimed in claim 1, wherein the secondary heating temperature of S4 is 60 ℃.
CN202210531145.9A 2022-05-16 2022-05-16 Preparation method of supported high-conductivity carbon nanotube catalyst Pending CN115254133A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060240974A1 (en) * 2002-08-02 2006-10-26 Nec Corporation Catalyst support substrate, method for growing carbon nanotubes using the same, and the transistor using carbon nanotubes
CN106102906A (en) * 2015-02-06 2016-11-09 Lg化学株式会社 The CNT catalyst for synthesizing comprising unsetting Alpha-alumina and the preparation method of the CNT utilizing described catalyst
CN106458593A (en) * 2015-04-21 2017-02-22 Lg化学株式会社 Large-diameter, low-density carbon nanotube, and preparation method therefor
CN112203978A (en) * 2018-07-27 2021-01-08 Lg化学株式会社 Method for preparing carbon nano tube

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060240974A1 (en) * 2002-08-02 2006-10-26 Nec Corporation Catalyst support substrate, method for growing carbon nanotubes using the same, and the transistor using carbon nanotubes
CN106102906A (en) * 2015-02-06 2016-11-09 Lg化学株式会社 The CNT catalyst for synthesizing comprising unsetting Alpha-alumina and the preparation method of the CNT utilizing described catalyst
CN106458593A (en) * 2015-04-21 2017-02-22 Lg化学株式会社 Large-diameter, low-density carbon nanotube, and preparation method therefor
CN112203978A (en) * 2018-07-27 2021-01-08 Lg化学株式会社 Method for preparing carbon nano tube

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