CN116425146A - Method for growing carbon nanotube array by catalyzing propylene with Fe-Ni-Mo alloy - Google Patents
Method for growing carbon nanotube array by catalyzing propylene with Fe-Ni-Mo alloy Download PDFInfo
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- CN116425146A CN116425146A CN202310579124.9A CN202310579124A CN116425146A CN 116425146 A CN116425146 A CN 116425146A CN 202310579124 A CN202310579124 A CN 202310579124A CN 116425146 A CN116425146 A CN 116425146A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 67
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 67
- 239000000956 alloy Substances 0.000 title claims abstract description 55
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 53
- 229910003296 Ni-Mo Inorganic materials 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 33
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 title claims abstract description 32
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 26
- 239000003054 catalyst Substances 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 239000011261 inert gas Substances 0.000 claims abstract description 15
- 239000007789 gas Substances 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000003491 array Methods 0.000 claims description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000007605 air drying Methods 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000004050 hot filament vapor deposition Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 12
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 5
- 125000004432 carbon atom Chemical group C* 0.000 description 5
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- VAWNDNOTGRTLLU-UHFFFAOYSA-N iron molybdenum nickel Chemical compound [Fe].[Ni].[Mo] VAWNDNOTGRTLLU-UHFFFAOYSA-N 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 229910001182 Mo alloy Inorganic materials 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 229910021398 atomic carbon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001010 compromised effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000000539 dimer Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- -1 iron-silicon-aluminum Chemical compound 0.000 description 1
- 239000002048 multi walled nanotube Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 229910000702 sendust Inorganic materials 0.000 description 1
- 239000002109 single walled nanotube Substances 0.000 description 1
- 239000013638 trimer Substances 0.000 description 1
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
- C01B32/162—Preparation characterised by catalysts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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Abstract
The invention belongs to the field of new materials, relates to a carbon nanotube preparation technology, and particularly provides a method for catalyzing propylene to grow a carbon nanotube array by using Fe-Ni-Mo alloy, which comprises the following steps: step 1, taking Fe-Ni-Mo alloy as a catalyst, placing the Fe-Ni-Mo alloy in a CVD rotary furnace, and introducing inert gas to remove air in the furnace; and 2, heating the CVD rotary furnace to 650-750 ℃ by taking propylene gas as a carbon source, introducing the propylene gas at a gas flow rate of 20-150 ml/min for reaction for 5-60 min, cooling to room temperature along with the furnace, and finally purifying to remove the catalyst to obtain the carbon nanotube array. The technology can be applied to other Fe-based alloys in a expanding way. The invention takes propylene as a carbon source and Fe-Ni-Mo alloy as a catalyst, and utilizes a catalytic chemical vapor deposition method to realize the efficient mass production of the carbon nanotube array, has mild reaction conditions, simple process flow and high utilization rate of the carbon source, and lays an important application foundation for mass and low-cost production of the carbon nanotube array.
Description
Technical Field
The invention belongs to the field of new materials, relates to a carbon nanotube preparation technology, and particularly provides a method for growing a carbon nanotube array by catalyzing propylene with Fe-Ni-Mo alloy.
Background
Carbon element is one of the earliest elements which are contacted and utilized by human beings, plays a vital role in the development process of the human beings, and carbon-based compounds are indispensable substances in our daily life. Nanomaterial is also receiving extensive attention for its excellent physical and chemical properties, and nanomaterial with unique structure and excellent properties is continuously explored and developed; among them, carbon nanomaterials have excellent properties in various aspects such as mechanics, thermal, electricity, optics, etc., and are one of the most interesting objects among many nanomaterials. However, since the freely grown carbon nanotubes are easily entangled with each other, their application and development are limited; the aspect ratio of the carbon nano tubes in the array form is almost the same, the orientation is good, the purity is high, and the excellent performance is shown; even if the orientation of the carbon nanotube array is compromised, the carbon nanotube array still has better performance than agglomerated single-walled and multi-walled carbon nanotubes in terms of improving the electronic, mechanical, and thermal properties of the polymer.
At present, the most commonly used carbon sources in the growth process of the carbon nanotube array are methane, ethylene, acetylene and the like, the molecular structure of the carbon sources can influence the shape of the grown carbon nanotubes, and linear hydrocarbon (methane, ethylene and acetylene) is thermally decomposed into atomic carbon or linear dimers/trimers of carbon, so that straight and hollow carbon nanotubes can be grown generally; for example, chinese patent publication No. CN112875680a discloses a method for growing carbon nanotube arrays by catalytically cracking acetylene with flaky iron-silicon-aluminum, but because acetylene produces more byproducts at the reaction temperature, the carbon conversion rate is low and the carbon source utilization rate is low; another example is a method for improving acetylene utilization rate by modifying sendust with plasma as disclosed in chinese patent publication No. CN114644337a, but this method is more cumbersome. Therefore, a method for mass production of carbon nanotube arrays with high carbon source utilization rate, simple process and low cost is still an important research difficulty.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides a method for catalyzing propylene to grow a carbon nano tube array by using Fe-Ni-Mo alloy; according to the invention, propylene is used as a carbon source, and Fe-Ni-Mo alloy is used as a catalyst, so that the carbon nanotube array with good compactness and good growth vigor is prepared under the condition of high carbon source conversion rate.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the method for growing the carbon nanotube array by catalyzing propylene with the Fe-Ni-Mo alloy is characterized by comprising the following steps of:
and 2, heating the CVD rotary furnace to 650-750 ℃ by taking propylene gas as a carbon source, introducing the propylene gas at a gas flow rate of 20-150 ml/min for reaction for 5-60 min, cooling to room temperature along with the furnace, and finally purifying to remove the catalyst to obtain the carbon nanotube array.
In the step 1, the inert gas is nitrogen or argon, the flow rate of the inert gas is 30-100 ml/min, and the charging time is 10-30 min.
Further, in the step 1, the iron-nickel-molybdenum alloy adopts a sheet alloy, and the sheet alloy is FeNiMo.
Further, in the step 1, the Fe-Ni-Mo alloy adopts a sheet alloy FeNiMo, wherein the Fe accounts for 30-35%, the Ni accounts for 30-35% and the Mo accounts for 30-40%.
In the step 1, the using amount of the Fe-Ni-Mo alloy is 0.5-10 g, and the weighing process is carried out under the protection of inert gas.
In step 2, the temperature rising rate of the CVD rotary furnace is 1-15 ℃/min.
Further, in the step 2, the specific steps of purification are as follows: firstly, soaking Fe-Ni-Mo alloy growing with a carbon nano tube array in dilute nitric acid or dilute sulfuric acid for 10-24 h, filtering, and washing with deionized water to neutrality; then soaking in dilute hydrofluoric acid for 10-24 h, filtering, and washing with deionized water to neutrality; finally, drying in a forced air drying oven at 60-80 ℃ for 10-48 h.
In the step 2, the reaction process is carried out under the protection of inert gas, wherein the inert gas is nitrogen or argon, and the flow rate of the inert gas is 30-60 ml/min.
Based on the technical scheme, the invention has the beneficial effects that:
the invention provides a method for catalyzing propylene to grow a carbon nano tube array by using Fe-Ni-Mo alloy, which takes propylene as a carbon source and Fe-Ni-Mo alloy as a catalyst, and realizes the high-efficiency mass production of the carbon nano tube array by using a catalytic chemical vapor deposition method; according to the invention, propylene is cracked into hydrogen and carbon atoms at high temperature, the oxide on the surface of the iron-based catalyst is reduced by the hydrogen, the carbon atoms are dissolved, diffused and nucleated on the surface of the iron-based catalyst, carbon nano tubes are generated, the carbon source byproducts of propylene are fewer, and the carbon source conversion rate is up to 98.44%; the technology can be applied to other Fe-based alloys in a expanding way. In conclusion, the method for preparing the carbon nanotube array by catalyzing propylene based on the Fe-Ni-Mo alloy has the advantages of mild reaction conditions, simple process flow and high carbon source utilization rate, and lays an important application foundation for mass and low-cost production of the carbon nanotube array.
Drawings
FIG. 1 is an SEM image of an Fe-Ni-Mo alloy flake used in examples 1-4 of the present invention.
FIG. 2 is an SEM image of a catalytically grown carbon nanotube array according to examples 1-4 of the present invention; wherein a to d represent the carbon nanotube arrays obtained in examples 1 to 4 in this order.
Fig. 3 is an XRD pattern of the carbon nanotube array obtained in example 3 of the present invention.
Fig. 4 is a Raman diagram of an iron-nickel-molybdenum sheet alloy material with carbon nanotubes grown in examples 1 to 2 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantageous effects of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings and examples.
Example 1
The embodiment provides a method for growing a carbon nano tube array by catalyzing propylene with Fe-Ni-Mo alloy, which comprises the following steps:
Example 2
The only difference between this embodiment and embodiment 1 is that: in step 2, the CVD rotary furnace (i.e., growth temperature) is 700 ℃; the resulting carbon nanotube array was labeled CNT-700 ℃.
Example 3
The only difference between this embodiment and embodiment 1 is that: in step 2, the CVD rotary furnace (i.e., growth temperature) is 725 ℃; the resulting carbon nanotube array was labeled CNT-725 ℃.
Example 4
The only difference between this embodiment and embodiment 1 is that: in step 2, the CVD rotary furnace (i.e., growth temperature) is 750 ℃; the resulting carbon nanotube array was labeled CNT-750 ℃.
The iron-nickel-molybdenum sheet alloy (catalyst), the iron-nickel-molybdenum sheet alloy with the carbon nanotube array grown and the prepared carbon nanotube array in examples 1 to 4 were tested, and the corresponding results were as follows:
as shown in fig. 1, which is an SEM image of the iron-nickel-molybdenum sheet alloy used in examples 1 to 4, it can be seen that the catalyst is a sheet alloy, and many nanoparticles exist on the surface of the catalyst, which plays a catalytic role in the growth process of the carbon nanotube array.
FIG. 2 is an SEM image of the carbon nanotube arrays prepared in examples 1 to 4; wherein a is the carbon nanotube array obtained in example 1, b is the carbon nanotube array obtained in example 2, c is the carbon nanotube array obtained in example 3, and d is the carbon nanotube array obtained in example 4; the graph shows that the Fe-Ni-Mo flaky alloy has good catalytic effect, and the ordered carbon nanotube array is successfully prepared on the surface of the Fe-Ni-Mo flaky alloy. Propylene is cracked into hydrogen and carbon atoms at high temperature, the hydrogen reduces oxide on the surface of the iron-based catalyst, the carbon atoms are dissolved, diffused and nucleated on the surface of the iron-based catalyst to generate carbon nanotubes, the directionally grown carbon nanotubes interact, and an array is formed under the action of Van der Waals force; the yields and carbon source conversions of the Fe-Ni-Mo alloy catalyzed propylene-grown carbon nanotube arrays in examples 1-4 are shown in Table 1, wherein the theoretical carbon supply amounts are: (3×12×40×30)/(1000×22.4) = 1.9286g, and the carbon source conversion is defined as the ratio of the carbon nanotube array yield to the theoretical carbon supply; in particular example 2, the carbon conversion rate of the Fe-Ni-Mo alloy catalyzed propylene growing carbon nano-tube array is as high as 98.44% at 700 ℃.
TABLE 1
| Sample of | Yield (g) | Conversion of carbon source (%) |
| CNT-675℃ | 1.57 | 81.35 |
| CNT-700℃ | 1.90 | 98.44 |
| CNT-725℃ | 1.75 | 90.77 |
| CNT-750℃ | 1.61 | 83.41 |
As shown in FIG. 3, which shows XRD patterns of the carbon nanotube array prepared in example 3, the diffraction peak 2 at CNT-700℃is a sample θ Diffraction peaks at=31.38°, 44.88 °, 65.34 ° and 82.86 ° represent the (200), (220), (400) and (422) planes, respectively, of the iron-based alloy, at 2 θ Diffraction peak at=26.12°, representing the diffraction peak of the carbon material.
As shown in FIG. 4, which shows the Raman diagrams of the Fe-Ni-Mo sheet alloy material with carbon nanotubes grown in examples 1-4, it is apparent from the diagrams that the Fe-Ni-Mo alloy after the formation of the carbon nanotube array has two distinct characteristic peaks of carbon nanotubes, one is at 1300cm -1 About D peak, another at 1580cm -1 The left and right G peaks, with increasing growth temperature and increasing temperature, the carbon atoms generated by the cleavage of linear propylene molecules tend to form SP 2 Less defects of the grown carbon nanotubes, I in Raman spectrum D /I G This is indicated by the decrease in value with increasing temperature.
While the invention has been described in terms of specific embodiments, any feature disclosed in this specification may be replaced by alternative features serving the equivalent or similar purpose, unless expressly stated otherwise; all of the features disclosed, or all of the steps in a method or process, except for mutually exclusive features and/or steps, may be combined in any manner.
Claims (7)
1. The method for growing the carbon nanotube array by catalyzing propylene with the Fe-Ni-Mo alloy is characterized by comprising the following steps of:
step 1, taking Fe-Ni-Mo alloy as a catalyst, placing the Fe-Ni-Mo alloy in a CVD rotary furnace, and introducing inert gas to remove air in the furnace;
and 2, heating the CVD rotary furnace to 650-750 ℃ by taking propylene gas as a carbon source, introducing the propylene gas at a gas flow rate of 20-150 ml/min for reaction for 5-60 min, cooling to room temperature along with the furnace, and finally purifying to remove the catalyst to obtain the carbon nanotube array.
2. The method for growing the carbon nanotube array by catalyzing propylene with the Fe-Ni-Mo alloy according to claim 1, wherein in the step 1, the inert gas is nitrogen or argon, the flow rate of the inert gas is 30-100 ml/min, and the introducing time is 10-30 min.
3. The method for catalyzing propylene to grow the carbon nanotube array by using the Fe-Ni-Mo alloy according to claim 1, wherein in the step 1, the Fe-Ni-Mo alloy adopts a sheet alloy, and the sheet alloy is FeNiMo, wherein the Fe accounts for 30-35%, the Ni accounts for 30-35% and the Mo accounts for 30-40%.
4. The method for growing carbon nanotube arrays by catalyzing propylene with Fe-Ni-Mo alloy according to claim 1, wherein in the step 1, the Fe-Ni-Mo alloy is used in an amount of 0.5-10 g, and the weighing process is performed under the protection of inert gas.
5. The method for growing the carbon nanotube array by catalyzing propylene with the Fe-Ni-Mo alloy according to claim 1, wherein in the step 2, the heating rate of the CVD rotary furnace is 1-15 ℃/min.
6. The method for growing carbon nanotube arrays by catalyzing propylene with Fe-Ni-Mo alloy according to claim 1, wherein in the step 2, the specific steps of purification are as follows: firstly, soaking Fe-Ni-Mo alloy growing with a carbon nano tube array in dilute nitric acid or dilute sulfuric acid for 10-24 h, filtering, and washing with deionized water to neutrality; then soaking in dilute hydrofluoric acid for 10-24 h, filtering, and washing with deionized water to neutrality; finally, drying in a forced air drying oven at 60-80 ℃ for 10-48 h.
7. The method for growing the carbon nanotube array by catalyzing propylene with the Fe-Ni-Mo alloy according to claim 1, wherein in the step 2, the reaction process is carried out under the protection of inert gas, the inert gas is nitrogen or argon, and the flow rate of the inert gas is 30-60 ml/min.
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