CN115608372B - Iron-cobalt-based catalyst, carbon nanotube and preparation process thereof - Google Patents
Iron-cobalt-based catalyst, carbon nanotube and preparation process thereof Download PDFInfo
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- CN115608372B CN115608372B CN202211121091.5A CN202211121091A CN115608372B CN 115608372 B CN115608372 B CN 115608372B CN 202211121091 A CN202211121091 A CN 202211121091A CN 115608372 B CN115608372 B CN 115608372B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 43
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 43
- 239000003054 catalyst Substances 0.000 title claims abstract description 31
- QVYYOKWPCQYKEY-UHFFFAOYSA-N [Fe].[Co] Chemical compound [Fe].[Co] QVYYOKWPCQYKEY-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 21
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims abstract description 20
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims abstract description 15
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims abstract description 15
- 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 12
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 12
- 235000012501 ammonium carbonate Nutrition 0.000 claims abstract description 12
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 12
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 12
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 12
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 12
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 12
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims abstract description 12
- 229940071125 manganese acetate Drugs 0.000 claims abstract description 12
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 238000007664 blowing Methods 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 238000012216 screening Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims 2
- 238000000034 method Methods 0.000 claims 1
- 238000000197 pyrolysis Methods 0.000 claims 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 10
- 229910017052 cobalt Inorganic materials 0.000 abstract description 5
- 239000010941 cobalt Substances 0.000 abstract description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 5
- 229910052742 iron Inorganic materials 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000005336 cracking Methods 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 9
- 230000001681 protective effect Effects 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
Classifications
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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
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8898—Manganese, technetium or rhenium containing also molybdenum
-
- 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
-
- 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
-
- 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
- C01B32/164—Preparation involving continuous processes
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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
- 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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- 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
- C01B2202/30—Purity
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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
- C01B2202/34—Length
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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
- C01B2202/36—Diameter
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- Materials Engineering (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention provides an iron-cobalt-based catalyst, a carbon nanotube and a preparation process thereof, wherein the iron-cobalt-based catalyst is prepared from the following raw materials in percentage by mass: 7-7.5wt% of ferric nitrate, and aluminum nitrate: 10-15wt%, ammonia water 4-8wt%, ammonium molybdate 0.1-0.5wt%, ammonium carbonate 1-5wt%, manganese acetate 0.5-0.9wt%, cobalt nitrate 1.5-2wt%, and H 2 62-75wt% of O; the preparation process of the carbon nano tube comprises the following steps: adding the iron-cobalt-based catalyst into a first main reactor, then introducing nitrogen and propylene, and performing expansion cracking on the propylene under the action of the iron-cobalt-based catalyst to obtain a carbon nano tube seed material; blowing the carbon nanotube seed material into a second main reactor, and then introducing nitrogen and propylene for reaction to obtain a carbon nanotube finished product. The iron-cobalt-based catalyst is beneficial to improving the purity of the carbon nano tube and reducing the impurity content of iron, cobalt and the like.
Description
Technical Field
The invention relates to the technical field of carbon nanotubes, in particular to an iron-cobalt-based catalyst, a carbon nanotube and a preparation process thereof.
Background
The preparation of the carbon nano tube by chemical vapor deposition is to add a catalyst into a furnace body, then introduce carbon source gas in the atmosphere of protective gas to grow the carbon nano tube, and the carbon nano tube prepared by the existing iron-cobalt-based catalyst has the problems of lower purity, higher impurity content of iron, cobalt and the like.
Disclosure of Invention
The invention provides an iron-cobalt-based catalyst, a carbon nanotube and a preparation process thereof, which are used for improving the purity of the carbon nanotube and reducing the impurity content of iron, cobalt and the like.
The technical scheme of the invention is realized as follows: an iron-cobalt-based catalyst is prepared from the following raw materials in percentage by mass: 7-7.5wt% of ferric nitrate, and aluminum nitrate: 10-15wt%, ammonia water 4-8wt%, ammonium molybdate 0.1-0.5wt%, ammonium carbonate 1-5wt%, manganese acetate 0.5-0.9wt%, cobalt nitrate 1.5-2wt%, and H 2 O62-75wt％。
Further, 7-7.5wt% of ferric nitrate, and aluminum nitrate: 11 to 12 weight percent, 5 to 6 weight percent of ammonia water, 0.2 to 0.3 weight percent of ammonium molybdate, 3 weight percent of ammonium carbonate, 0.7 to 0.8 weight percent of manganese acetate, 1.5 to 2 weight percent of cobalt nitrate and H 2 O 70-72wt％。
Further, 7.28wt% of ferric nitrate, aluminum nitrate: 11.3wt%, ammonia water 5.61wt%, ammonium molybdate 0.26wt%, ammonium carbonate 3wt%, manganese acetate 0.71wt%, cobalt nitrate 1.64wt%, H 2 O 70.2wt％。
A process for preparing carbon nanotubes, comprising the steps of:
(1) Adding the iron-cobalt-based catalyst into a first main reactor, then introducing nitrogen and propylene, and performing expansion cracking on the propylene under the action of the iron-cobalt-based catalyst in a nitrogen environment to obtain a carbon nano tube seed material;
(2) And blowing the carbon nano tube seed material into the second main reactor through nitrogen, and then introducing nitrogen and propylene for reaction to obtain a carbon nano tube finished product.
The carbon nano tube is prepared by adopting the preparation process.
The invention has the beneficial effects that:
the preparation of the carbon nano tube by the iron-cobalt-based catalyst is beneficial to reducing the content of metal impurities such as iron, cobalt and the like, reducing the resistivity of carbon nano tube powder and improving the purity of the carbon nano tube.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a TEM image of a carbon nanotube according to example 5 of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without any inventive effort, are intended to be within the scope of the invention.
The invention adopts nitrogen with the purity of 99.999 percent as protective gas, and the purity of propylene is 99.6 percent.
Example 1
An iron-cobalt-based catalyst is prepared from the following raw materials in percentage by mass: 7wt% of ferric nitrate and aluminum nitrate: 15wt%, ammonia water 6wt%, ammonium molybdate 0.2wt%, ammonium carbonate 4wt%, manganese acetate 0.8wt%, cobalt nitrate 1.5wt%, H 2 O 65.5wt％。
Example 2
An iron-cobalt-based catalyst is prepared from the following raw materials in percentage by mass: 7.5wt% of ferric nitrate, aluminum nitrate: 10wt%, ammonia water 5wt%, ammonium molybdate 0.5wt%, ammonium carbonate 3wt%, manganese acetate 0.5wt%, cobalt nitrate 2wt%, H 2 O 71.5wt％。
Example 3
An iron-cobalt-based catalyst is prepared from the following raw materials in percentage by mass: 7.28wt% of ferric nitrate, aluminum nitrate: 11.3wt%, ammonia water 5.61wt%, ammonium molybdate 0.26wt%, ammonium carbonate 3wt%, manganese acetate 0.71wt%, cobalt nitrate 1.64wt%, H 2 O 70.2wt％。
Example 4
An iron-cobalt-based catalyst is prepared from the following raw materials in percentage by mass: 7wt% of ferric nitrate and aluminum nitrate: 12wt%, ammonia water 8wt%, ammonium molybdate 0.3wt%, ammonium carbonate 5wt%, manganese acetate 0.9wt%, cobalt nitrate 1.5wt%, H 2 O 65.3wt％。
The preparation method of the iron-cobalt-based catalyst in the embodiments 1-4 comprises the steps of uniformly stirring the raw materials, dehydrating, baking (550 ℃) and then crushing and screening to obtain the iron-cobalt-based catalyst.
Example 5
A process for preparing carbon nanotubes, comprising the steps of:
(1) Firstly, blowing protective gas into a main reactor and a gas preheating furnace, and starting to heat, wherein the protective gas is nitrogen with the purity of 99.999%; after the temperature of the main reactor is raised to 600 ℃, adding 3kg of the iron-cobalt-based catalyst prepared in the embodiment 3 into the main reactor, then introducing nitrogen and propylene, and under the nitrogen environment, performing expansion cracking on the propylene under the action of the iron-cobalt-based catalyst to obtain a carbon nano tube seed material, and blowing the carbon nano tube seed material into a transfer tank through nitrogen after cooling the carbon nano tube seed material;
(2) Blowing the carbon nanotube seed material into a second main reactor through nitrogen, then introducing nitrogen and propylene for reaction, blowing the carbon nanotube seed material into a cooling tank through nitrogen after the reaction is completed, cooling to 80 ℃, and blowing the carbon nanotube seed material into a finished product tank through nitrogen to obtain a carbon nanotube finished product.
In the steps (1) and (2), the gas is introduced into ten stages, wherein the gas comprises high-temperature propylene, low-temperature propylene, high-temperature nitrogen and low-temperature nitrogen, and the introduced amount is shown in the following table 1:
TABLE 1 gas inflow at each stage
Comparative example 1
This embodiment is substantially the same as embodiment 5 except that: an iron-cobalt-based catalyst is prepared from the following raw materials in percentage by mass: 7.6wt% of ferric nitrate, aluminum nitrate: 11.3wt%, ammonia water 5.61wt%, ammonium molybdate 0.26wt%, ammonium carbonate 3wt%, manganese acetate 0.71wt%, cobalt nitrate 1.32wt%, H 2 O 70.2wt％。
The carbon nanotube finished product prepared in example 5 was tested as shown in the following table 2:
TABLE 2 detection results of carbon nanotube finished products of example 5 and comparative example 1
As can be seen from table 2 above, the carbon nanotube finished product prepared by example 5 of the present invention has lower contents of iron and cobalt in metal impurities, lower powder resistivity and higher purity.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (5)
1. An iron-cobalt-based catalyst for preparing carbon nanotubes is characterized by being prepared from the following raw materials in percentage by mass: 7-7.5wt% of ferric nitrate, and aluminum nitrate: 10-15wt%, ammonia water 4-8wt%, ammonium molybdate 0.1-0.5wt%, ammonium carbonate 1-5wt%, manganese acetate 0.5-0.9wt%, cobalt nitrate 1.5-2wt%, and H 2 O 62-75wt%；
The preparation method of the iron-cobalt-based catalyst comprises the steps of uniformly stirring the raw materials, dehydrating, baking, crushing and screening to obtain the iron-cobalt-based catalyst.
2. An iron-cobalt-based catalyst for the preparation of carbon nanotubes according to claim 1, wherein the iron nitrate is 7-7.5wt%, aluminum nitrate: 11-12wt%, ammonia water 5-6wt%, ammonium molybdate 0.2-0.3wt%, ammonium carbonate 3wt%, manganese acetate 0.7-0.8wt%, cobalt nitrate 1.5-2wt%, and H 2 O 70-72wt%。
3. An iron-cobalt-based catalyst for the preparation of carbon nanotubes according to claim 2, characterized in that the iron nitrate is 7.28wt%, aluminum nitrate: 11.3wt%, ammonia water 5.61wt%, ammonium molybdate 0.26wt%, ammonium carbonate 3wt%, manganese acetate 0.71wt%, cobalt nitrate 1.64wt%, H 2 O 70.2wt%。
4. The preparation process of the carbon nano tube is characterized by comprising the following steps of:
(1) Adding the iron-cobalt-based catalyst in one of claims 1-3 into a first main reactor, then introducing nitrogen and propylene, and performing expansion pyrolysis on the propylene under the action of the iron-cobalt-based catalyst in a nitrogen environment to obtain a carbon nanotube seed material;
(2) And blowing the carbon nano tube seed material into the second main reactor through nitrogen, and then introducing nitrogen and propylene for reaction to obtain a carbon nano tube finished product.
5. A carbon nanotube prepared by the process according to claim 4.
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| CN202211121091.5A CN115608372B (en) | 2022-09-15 | 2022-09-15 | Iron-cobalt-based catalyst, carbon nanotube and preparation process thereof |
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| CN115608372B true CN115608372B (en) | 2024-03-26 |
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