CN115532276A - Preparation and application of nickel-based carbon nanotube catalyst - Google Patents

Preparation and application of nickel-based carbon nanotube catalyst Download PDF

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CN115532276A
CN115532276A CN202211250622.0A CN202211250622A CN115532276A CN 115532276 A CN115532276 A CN 115532276A CN 202211250622 A CN202211250622 A CN 202211250622A CN 115532276 A CN115532276 A CN 115532276A
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nickel
nitrate
catalyst
nano tube
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陈国顺
刘彦军
陈永胜
游启龙
吕家应
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Shandong Carbon Peak New Material Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002Mixed oxides other than spinels, e.g. perovskite
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76Catalysts 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
    • B01J23/84Catalysts 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
    • B01J23/85Chromium, molybdenum or tungsten
    • B01J23/88Molybdenum
    • B01J23/887Molybdenum containing in addition other metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/8878Chromium
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    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/158Carbon nanotubes
    • C01B32/16Preparation
    • C01B32/162Preparation characterised by catalysts
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2523/00Constitutive chemical elements of heterogeneous catalysts
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    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2202/00Structure or properties of carbon nanotubes
    • C01B2202/20Nanotubes characterized by their properties
    • C01B2202/22Electronic properties

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Abstract

The invention discloses a preparation method and application of a nickel-based carbon nanotube catalyst, which is prepared by dissolving nickel nitrate, aluminum nitrate, citric acid, ammonium molybdate and chromium nitrate; according to the preparation method of the catalyst, nickel nitrate, aluminum nitrate, citric acid, ammonium molybdate and chromium nitrate are stirred and mixed in deionized water, and then the metal hydroxide precipitate is calcined at high temperature to finally form the catalyst. The preparation method ensures that the prepared catalyst has high catalytic activity by strictly controlling the process conditions of each step and the proportion of each component, can obtain the carbon nano tube with higher multiplying power under the catalytic action of the catalyst, the multiplying power is 18-22 times, the prepared carbon nano tube has high conductivity, and the catalyst can effectively reduce the production cost of the carbon nano tube.

Description

Preparation and application of nickel-based carbon nanotube catalyst
Technical Field
The invention relates to the technical field of catalysts, in particular to a preparation method and application of a nickel-based carbon nanotube catalyst.
Background
The carbon nano tube has the characteristics of excellent conductivity, ultrahigh mechanical strength, extremely high chemical stability and thermal stability and the like, and can be widely applied to the fields of high-performance composite materials, capacitors, hydrogen storage, electromagnetic wave-absorbing materials and the like.
At present, the carbon nanotubes are mainly prepared by arc discharge, laser evaporation, and Chemical Vapor Deposition (CVD). In addition to these three common methods, there are electron beam irradiation, electrolysis, and pyrolysis polymerization.
Among them, the chemical vapor deposition method has the advantages of low cost, large yield, easy control of test conditions, etc., and is the most suitable method for industrial mass production at present. The principle of the CVD method is that a gas containing a carbon source is decomposed while flowing over the surface of a catalyst, and a carbon nanotube structure is induced to be formed on the side where the catalyst is present. Therefore, in the synthesis process of the carbon nanotubes, the key point is to select a proper catalyst, but the conversion rate and the yield of the carbon nanotubes prepared by the existing catalyst are low.
Disclosure of Invention
The present invention aims to provide a preparation method and an application of a nickel-based carbon nanotube catalyst, so as to solve the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: a nickel-based carbon nanotube catalyst comprises the following components: 8-12 parts of nickel nitrate, 7-12 parts of aluminum nitrate, 8-13 parts of citric acid, 0.6-1.2 parts of ammonium molybdate and 0.8-1.2 parts of chromium nitrate.
A preparation method of a nickel-based carbon nanotube catalyst comprises the following steps:
step one, according to parts by weight, 8-12 parts of nickel nitrate, 7-12 parts of aluminum nitrate, 8-13 parts of citric acid, 0.6-1.2 parts of ammonium molybdate and 0.8-1.2 parts of chromium nitrate for later use;
step two, dissolving the nickel nitrate, the aluminum nitrate, the citric acid, the ammonium molybdate and the chromium nitrate weighed in the step one into 300 parts by weight of deionized water, and uniformly stirring to completely dissolve the reagent to form a clear solution;
and step three, calcining the mixed solution of the solution at 600 ℃ for 1h to obtain the catalyst.
Preferably, in step two, the solution is stirred for 1h, wherein the stirring speed is 500r/min.
Preferably, step three further comprises grinding the calcined material to a fine powder.
The application of the nickel-based carbon nanotube catalyst comprises the following steps of preparing a carbon nanotube by a chemical vapor deposition method;
the chemical vapor deposition method for preparing the carbon nano tube comprises the following steps: putting the prepared nickel-based carbon nano tube catalyst into a horizontal furnace, heating to 800 ℃, and controlling the temperature to be 16m 3 And introducing propane as a carbon source for reaction for 3 hours to prepare the carbon nano tube, wherein the multiplying power of the prepared carbon nano tube is 18-22 times.
Has the advantages that: the invention has the beneficial effects that: the preparation method of the nickel-based carbon nanotube catalyst comprises the steps of stirring and mixing nickel nitrate, aluminum nitrate, citric acid, ammonium molybdate and chromium nitrate deionized water, and then calcining a metal hydroxide precipitate at high temperature to finally form the catalyst. The preparation method ensures that the prepared catalyst has high catalytic activity by strictly controlling the process conditions of each step and the proportion of each component, can obtain the carbon nano tube with higher multiplying power under the catalytic action of the catalyst, the multiplying power is 18-22 times, the prepared carbon nano tube has high conductivity, and the catalyst can effectively reduce the production cost of the carbon nano tube.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the prior art descriptions will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is an optical diagram of a nickel-based carbon nanotube catalyst according to the present invention.
Detailed Description
The technical solution of the present patent will be further described in detail with reference to the following embodiments.
A nickel-based carbon nanotube catalyst comprises the following components: 8-12 parts of nickel nitrate, 7-12 parts of aluminum nitrate, 8-13 parts of citric acid, 0.6-1.2 parts of ammonium molybdate and 0.8-1.2 parts of chromium nitrate.
A preparation method of a nickel-based carbon nanotube catalyst comprises the following steps:
step one, according to the parts by weight, 8-12 parts of nickel nitrate, 7-12 parts of aluminum nitrate, 8-13 parts of citric acid, 0.6-1.2 parts of ammonium molybdate and 0.8-1.2 parts of chromium nitrate are used for standby;
step two, dissolving the nickel nitrate, the aluminum nitrate, the citric acid, the ammonium molybdate and the chromium nitrate weighed in the step one into 300 parts by weight of deionized water, and uniformly stirring to completely dissolve the reagent to form a clear solution;
and step three, calcining the mixed solution of the solution at 600 ℃ for 1h to obtain the catalyst.
In the invention, in the second step, the solution is stirred for 1h, wherein the stirring speed is 500r/min.
In the invention, the third step also comprises grinding the calcined substance into fine powder.
The application of the nickel-based carbon nanotube catalyst comprises the following steps of preparing a carbon nanotube by a chemical vapor deposition method;
the chemical vapor deposition method for preparing the carbon nano tube comprises the following steps: putting the prepared nickel-based carbon nano tube catalyst into a horizontal furnace, heating to 800 ℃, and controlling the temperature to be 16m 3 And introducing propane as a carbon source for reaction for 3 hours to prepare the carbon nano tube, wherein the multiplying power of the prepared carbon nano tube is 18-22 times.
Example 1
A nickel-based carbon nanotube catalyst comprises the following components: 8 parts of nickel nitrate, 7 parts of aluminum nitrate, 8 parts of citric acid, 0.6 part of ammonium molybdate and 0.8 part of chromium nitrate.
A preparation method of a nickel-based carbon nanotube catalyst comprises the following steps:
step one, 8 parts of nickel nitrate, 7 parts of aluminum nitrate, 8 parts of citric acid, 0.6 part of ammonium molybdate and 0.8 part of chromium nitrate in parts by weight for later use;
step two, dissolving the nickel nitrate, the aluminum nitrate, the citric acid, the ammonium molybdate and the chromium nitrate weighed in the step one into 300 parts by weight of deionized water, and uniformly stirring to completely dissolve the reagent to form a clear solution;
and step three, calcining the mixed solution of the solution at 600 ℃ for 1h to obtain the catalyst.
In the second step of the invention, the solution is stirred for 1 hour, wherein the stirring speed is 500r/min.
In the invention, the third step also comprises grinding the calcined substance into fine powder.
The application of the nickel-based carbon nanotube catalyst comprises the following steps of preparing a carbon nanotube by a chemical vapor deposition method;
the chemical vapor deposition method for preparing the carbon nano tube comprises the following steps: putting the prepared nickel-based carbon nanotube catalyst into a horizontal furnace, heating to 800 ℃, and controlling the temperature to be 16m 3 And introducing propane as a carbon source, reacting for 3 hours, and preparing the carbon nano tube, wherein the multiplying power of the prepared carbon nano tube is 18 times.
Example 2
A nickel-based carbon nanotube catalyst comprises the following components: 12 parts of nickel nitrate, 12 parts of aluminum nitrate, 13 parts of citric acid, 1.2 parts of ammonium molybdate and 1.2 parts of chromium nitrate.
A preparation method of a nickel-based carbon nanotube catalyst comprises the following steps:
step one, 12 parts of nickel nitrate, 12 parts of aluminum nitrate, 13 parts of citric acid, 1.2 parts of ammonium molybdate and 1.2 parts of chromium nitrate in parts by weight for later use;
step two, dissolving the nickel nitrate, the aluminum nitrate, the citric acid, the ammonium molybdate and the chromium nitrate weighed in the step one into 300 parts by weight of deionized water, and uniformly stirring to completely dissolve the reagent to form a clear solution;
and step three, calcining the mixed solution of the solution at 600 ℃ for 1h to obtain the catalyst.
In the invention, in the second step, the solution is stirred for 1h, wherein the stirring speed is 500r/min.
In the invention, the third step also comprises grinding the calcined substance into fine powder.
The application of the nickel-based carbon nanotube catalyst comprises the following steps of preparing a carbon nanotube by a chemical vapor deposition method;
the chemical vapor deposition method for preparing the carbon nano tube comprises the following steps: putting the prepared nickel-based carbon nanotube catalyst into a horizontal furnace, heating to 800 ℃, and controlling the temperature to be 16m 3 And introducing propane as a carbon source for reaction for 3 hours to prepare the carbon nano tube, wherein the multiplying power of the prepared carbon nano tube is 22 times.
Example 3
A nickel-based carbon nanotube catalyst comprises the following components: 10 parts of nickel nitrate, 9 parts of aluminum nitrate, 11 parts of citric acid, 0.9 part of ammonium molybdate and 1.0 part of chromium nitrate.
A preparation method of a nickel-based carbon nanotube catalyst comprises the following steps:
step one, according to the parts by weight, 10 parts of nickel nitrate, 9 parts of aluminum nitrate, 11 parts of citric acid, 0.9 part of ammonium molybdate and 1.0 part of chromium nitrate are used for standby;
step two, dissolving the nickel nitrate, the aluminum nitrate, the citric acid, the ammonium molybdate and the chromium nitrate weighed in the step one into 300 parts by weight of deionized water, and uniformly stirring to completely dissolve the reagent to form a clear solution;
and step three, calcining the mixed solution of the solution at 600 ℃ for 1h to obtain the catalyst.
In the invention, in the second step, the solution is stirred for 1h, wherein the stirring speed is 500r/min.
In the invention, the third step also comprises grinding the calcined substance into fine powder.
The application of the nickel-based carbon nanotube catalyst comprises the following steps of preparing a carbon nanotube by a chemical vapor deposition method;
the chemical vapor deposition method for preparing the carbon nano tube comprises the following steps: putting the prepared nickel-based carbon nanotube catalyst into a horizontal furnace, heating to 800 ℃, and controlling the temperature to be 16m 3 And introducing propane as a carbon source, reacting for 3 hours, and preparing the carbon nano tube, wherein the multiplying power of the prepared carbon nano tube is 20 times.
The preparation method of the catalyst comprises the steps of stirring and mixing nickel nitrate, aluminum nitrate, citric acid, ammonium molybdate and chromium nitrate deionized water, and then calcining the metal hydroxide precipitate at high temperature to finally form the catalyst. The preparation method ensures that the prepared catalyst has high catalytic activity by strictly controlling the process conditions of each step and the proportion of each component, can obtain the carbon nano tube with higher multiplying power under the catalytic action of the catalyst, the multiplying power is 18-22 times, the prepared carbon nano tube has high conductivity, and the catalyst can effectively reduce the production cost of the carbon nano tube.
TABLE 1
Figure BDA0003887356120000051
Figure BDA0003887356120000061
As is clear from table 1, the carbon nanotube ratios in examples 1 to 3 are significantly improved as compared with comparative example 1.
The embodiments described above are preferred embodiments of the present invention, and not all embodiments. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Claims (5)

1. A nickel-based carbon nanotube catalyst is characterized by comprising the following components: 8-12 parts of nickel nitrate, 7-12 parts of aluminum nitrate, 8-13 parts of citric acid, 0.6-1.2 parts of ammonium molybdate and 0.8-1.2 parts of chromium nitrate.
2. The method for preparing a nickel-based carbon nanotube catalyst according to claim 1, comprising the steps of:
step one, according to parts by weight, 8-12 parts of nickel nitrate, 7-12 parts of aluminum nitrate, 8-13 parts of citric acid, 0.6-1.2 parts of ammonium molybdate and 0.8-1.2 parts of chromium nitrate for later use;
step two, dissolving the nickel nitrate, the aluminum nitrate, the citric acid, the ammonium molybdate and the chromium nitrate weighed in the step one into 300 parts by weight of deionized water, and uniformly stirring to completely dissolve the reagent to form a clear solution;
and step three, calcining the mixed solution of the solution at 600 ℃ for 1h to obtain the catalyst.
3. The method of claim 2, wherein in the second step, the solution is stirred for 1 hour, wherein the stirring speed is 500r/min.
4. The method of claim 2, wherein the step three further comprises grinding the calcined substance into a fine powder.
5. The use of the nickel-based carbon nanotube catalyst according to claim 1, wherein: preparing the carbon nano tube by the nickel-based carbon nano tube catalyst through a chemical vapor deposition method;
the chemical vapor deposition method for preparing the carbon nano tube comprises the following steps: putting the prepared nickel-based carbon nanotube catalyst into a horizontal furnace, heating to 800 ℃, and controlling the temperature to be 16m 3 And introducing propane as a carbon source for reaction for 3 hours to prepare the carbon nano tube, wherein the multiplying power of the prepared carbon nano tube is 18-22 times.
CN202211250622.0A 2022-10-12 2022-10-12 Preparation and application of nickel-based carbon nanotube catalyst Pending CN115532276A (en)

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Application publication date: 20221230