CN115532276A - Preparation and application of nickel-based carbon nanotube catalyst - Google Patents
Preparation and application of nickel-based carbon nanotube catalyst Download PDFInfo
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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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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 70
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 70
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 239000003054 catalyst Substances 0.000 title claims abstract description 57
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title abstract description 16
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 66
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 claims abstract description 44
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims abstract description 22
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 22
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 22
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 22
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 22
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 20
- 238000005229 chemical vapour deposition Methods 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 14
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000001354 calcination Methods 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 239000003153 chemical reaction reagent Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 239000001294 propane Substances 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 229910000000 metal hydroxide Inorganic materials 0.000 abstract description 3
- 150000004692 metal hydroxides Chemical class 0.000 abstract description 3
- 239000002244 precipitate Substances 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01J23/8878—Chromium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
- C01B32/162—Preparation characterised by catalysts
-
- 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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/22—Electronic 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
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
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.
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