CN110040718B - Preparation method of thiacalixarene-based multi-walled carbon nanotube derived from 16 nuclear molecular cluster - Google Patents
Preparation method of thiacalixarene-based multi-walled carbon nanotube derived from 16 nuclear molecular cluster Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000002048 multi walled nanotube Substances 0.000 title claims abstract description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 31
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 23
- 239000010453 quartz Substances 0.000 claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000758 substrate Substances 0.000 claims abstract description 13
- 238000004528 spin coating Methods 0.000 claims abstract description 8
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- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 6
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims abstract description 4
- 239000012018 catalyst precursor Substances 0.000 claims abstract description 4
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims abstract description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N CHCl3 Substances ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000013078 crystal Substances 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 239000012300 argon atmosphere Substances 0.000 claims description 6
- 239000002071 nanotube Substances 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 5
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
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- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 238000010926 purge Methods 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 2
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- 238000006555 catalytic reaction Methods 0.000 abstract description 3
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- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 4
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- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- -1 sodium cations Chemical class 0.000 description 2
- 238000004729 solvothermal method Methods 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241001330002 Bambuseae Species 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 229910006148 NiII Inorganic materials 0.000 description 1
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
- B01J31/063—Polymers comprising a characteristic microstructure
- B01J31/066—Calixarenes and hetero-analogues, e.g. thiacalixarenes
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/28—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of the platinum group metals, iron group metals or copper
-
- 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
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/06—Multi-walled nanotubes
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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
- C01B2202/32—Specific surface area
-
- 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
Abstract
The invention discloses a preparation method of a multi-walled carbon nanotube derived from thiacalixarene-16 nuclear molecular cluster, which adopts the technical scheme that the preparation method comprises the following steps: (1) preparation and spin-coating of M16 from t-butylthiacalixarene H4BTC4A(0.1mmol)，NiCl2·6H2O(0.4mmol)，Dy(OAc)3·6H2O (0.3mmol) and Na2CO3(0.2mmol) in DMA/CH3CN/Et3N, then transferred to a reaction kettle for 6 days at 130 ℃, then slowly cooled to room temperature, which was designated as M16: taking the macromolecular cluster M16 in a test tube, and adding 10mL of CHCl3The solution was dissolved and dispersed on a quartz substrate by a spin coating method to be used as a catalyst precursor. (2) The carbon nano tube is prepared by a chemical vapor deposition method. The method has the advantages of low cost of required materials, simple preparation process, short preparation period, simple reaction conditions, regular appearance of the prepared product, larger specific surface area, strong appearance controllability, good stability and repeatability, and strong operability and practicability, and has potential application value and strong practicability in the fields of electro-catalysis performance and the like.
Description
Technical Field
The invention belongs to the technical field of micro-nano material synthesis, and particularly relates to a preparation method of a multi-walled carbon nanotube derived from thiacalixarene-based 16-nucleus molecular cluster.
Background
The carbon nano tube is used as a one-dimensional nano material, has light weight, perfect connection of a hexagonal structure and a plurality of abnormal mechanical, electrical and chemical properties. In recent years, the extensive application prospect of the carbon nano-tube and the nano-material is continuously shown along with the research of the carbon nano-tube and the nano-material. The carbon nanotube can be regarded as a graphene sheet layer which is curled, and thus the number of layers of the graphene sheet can be divided into: single-walled Carbon nanotubes (or Single-walled Carbon nanotubes, SWCNTs) and Multi-walled Carbon nanotubes (or Multi-walled Carbon nanotubes, MWCNTs). The carbon nano tube has good mechanical property, the hardness of the carbon nano tube is equivalent to that of diamond, but the carbon nano tube has good flexibility and can be stretched. Furthermore, the melting point of carbon nanotubes is the highest of the known materials.
The commonly used methods for preparing carbon nanotubes mainly include arc discharge, laser ablation, chemical vapor deposition (pyrolysis of hydrocarbon gas), solid phase pyrolysis, glow discharge, gas combustion, and polymerization synthesis. Among them, the chemical vapor deposition method is an economical method due to its advantages of low preparation temperature, low cost, large-area preparation, etc., and thus has been widely studied. However, the method for preparing the carbon material still needs to be developed, and the preparation of the carbon material by using a synthesis method with simplicity, good repeatability and low cost still has great challenge.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of a multi-wall carbon nano-tube derived from thiacalixarene-16 nuclear molecular cluster. The method has the advantages of low material cost, simple preparation process, short preparation period, simple reaction conditions, regular product appearance, larger specific surface area, strong appearance controllability, good stability and repeatability, and strong operability and practicability, and has potential application value and strong practicability in the fields of electro-catalysis performance and the like.
In order to achieve the purpose, the invention adopts the technical scheme that
(1) Preparation and spin coating of M16
From 0.1mmol of tert-butylthiacalixarene H4BTC4A, 0.4mmol of NiCl2·6H2O, 0.3mmol of Dy (OAc)3·6H2O and 0.2mmol of Na2CO3In DMA/CH with volumes of 6, 3 and 0.5mL respectively3CN/Et3Mixing with N, transferring to a reaction kettle, reacting at 130 deg.C for 6 days, slowly cooling to room temperature to obtain green block crystal named M16, adding 1mg of macromolecular cluster M16 into a test tube, and adding 10ml of CHCl3Dissolving, and taking a drop of prepared solution to be dispersed on a quartz substrate by a spin coating method to be used as a catalyst precursor;
(2) obtaining the carbon nano tube M16-CNT by using a chemical vapor deposition method
And (2) growing the carbon nano tubes in a furnace with a 1-inch tube, placing the quartz substrate dispersed with the M16 substance obtained in the step (1) on a quartz boat, placing the quartz boat in the tube, calcining the quartz substrate in a chemical vapor deposition tube furnace in an argon atmosphere of 300 standard cubic centimeters per minute, raising the temperature of the furnace to 800 ℃ at a heating rate of 10 ℃/min, purging the system with argon, introducing a hydrogen flow of 100scc/min and ethylene of 50scc/min, and growing the carbon nano tubes at 800 ℃ for 30 minutes to obtain the carbon nano tubes densely distributed on the surface of the quartz substrate.
It is further set that M16 has a molecular weight of 1357 in said step (1).
A further arrangement is that the diameter of the carbon nanotubes produced is about 20 nm.
The further arrangement is that the carbon nanotubes are bamboo-like, and the tip of each nanotube is attached with M16 catalyst particles.
The carbon nano tube has the characteristics of micropores and mesopores, and the specific surface area of the carbon nano tube is 66.2m through a BET test2g-1。
The lattice stripe spacing of the obtained carbon nanotube is further set to be 0.31nm, corresponding to the (002) crystal face of the C atom.
The invention relates to a preparation method of a multi-walled carbon nanotube derived from thiacalixarene-16 nuclear molecular cluster. The method has the advantages of low cost of required materials, simple preparation process, short preparation period, simple reaction conditions, regular appearance of the prepared product, larger specific surface area, strong appearance controllability, good stability and repeatability, and strong operability and practicability, and has potential application value and strong practicability in the fields of electro-catalysis performance and the like.
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 description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is within the scope of the present invention for those skilled in the art to obtain other drawings based on the drawings without inventive exercise.
FIG. 1 is a crystal structure diagram of macromolecular cluster M16 synthesized by solvothermal method according to the present invention;
FIG. 2 is a gel permeation chromatogram of M16;
FIG. 3 is a powder X-ray diffraction (PXRD) pattern of M16;
FIG. 4 is a thermogravimetric analysis (TGA) profile of M16 under an argon atmosphere;
FIG. 5 is a Scanning Electron Microscope (SEM) image of a chemical vapor deposition process to synthesize M16-CNT; wherein, the sizes of scales corresponding to the SEM images are respectively 20 μm and 5 μm;
FIG. 6 is a Transmission Electron Microscope (TEM) image of a chemical vapor deposition method to synthesize M16-CNT; wherein the sizes of scales corresponding to the TEM image are 200nm and 10nm respectively;
FIG. 7 is a Raman plot of M16-CNT obtained by Chemical Vapor Deposition (CVD);
FIG. 8 shows N of M16-CNT obtained by Chemical Vapor Deposition (CVD)2Adsorption-desorption curves.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings.
The invention discloses a preparation method of a multi-walled carbon nanotube derived from thiacalixarene-based 16-nucleus molecular cluster. The method takes macromolecular clusters M16 as raw materials, and adopts a chemical vapor deposition method (CVD) to obtain multi-wall carbon nano-tubes M16-CNT; in other words, the present invention provides a method for preparing a novel multi-walled carbon nanotube. The preparation method of the multi-wall carbon nanotube M16-CNT comprises the following steps:
(1) preparation and spin coating of M16. From tert-butylthiacalixarenes H4BTC4A(0.1mmol，72mg)， NiCl2·6H2O(0.4mmol，95mg)，Dy(OAc)3·6H2O (0.3mmol, 132mg) and Na2CO3(0.2mmol, 21mg) in DMA/CH3CN/Et3N (6/3/0.5mL), then transferred to a reaction kettle for 6 days at 130 ℃ and then slowly cooled to room temperature to give green blocky crystals, which are designated M16: [ Na ]2NiII 12LnIII 2(BTC4A)3(μ7-CO3)3(μ3-OH)4(μ3-Cl)2-(OAc)6(dma)4] 2OAc 0.5dma 3MeCN 8DMA(Ln＝Dy；H4BTC4A＝p-tert-butylthiacalix[4]arene; DMA and DMA) are N, N' -dimethylacetamide). 1mg of macromolecular cluster M16 was placed in a test tube, 10mL of CHCl was added3The dissolution was carried out, and one drop of the prepared solution was dispersed on a quartz substrate by a spin coating method to be used as a catalyst precursor.
(2) Carbon nanotube growth was performed in a furnace with a 1 inch tube. The quartz substrate with the well-dispersed M16 substance was placed on a quartz boat and placed in a tube and subjected to Chemical Vapor Deposition (CVD) tube furnace calcination under an argon atmosphere of 300 standard cubic centimeters per minute (scc/min) with the furnace temperature being raised to 800 ℃ at a ramp rate of 10 ℃/min. After purging the system with argon, a stream of hydrogen (100scc/min) and ethylene (50 scc/min) was introduced and the carbon nanotubes were grown at 800 ℃ for 30 minutes. The resulting M16-CNT was allowed to cool to room temperature. The resulting carbon nanotubes M16-CNT were characterized by FE-SEM, TEM, EDX and PXRD. SEM images showed that densely distributed carbon nanotubes were formed on the surface of the quartz substrate after calcination. The diameter of the nanotubes is about 10 nm. The obtained multi-walled carbon nanotubes were confirmed to be bamboo-like by TEM, and the tip of each nanotube was attached with nano-catalytic particles. The lattice fringe spacing was 0.31nm, corresponding to the (002) crystal plane of C.
FIG. 1 is a crystal structure diagram of macromolecular cluster M16 synthesized by solvothermal method according to the present invention, and it can be seen from the diagram that: it is a feather-like molecular cluster with 16 cores, which is respectively composed of two sodium cations, two lanthanide cations, twelve nickel ions and three tert-butyl thiacalixarenes;
fig. 2 is a gel permeation chromatogram of M16, from which GPC results are shown in which the number average molecular weight Mn is 1152, the weight average molecular weight Mw is 1357, and pdi (polydispersity) Mw/Mn is 1.17.
FIG. 3 is a powder X-ray diffraction (PXRD) pattern of M16, from which it can be seen that: the resulting M16 compares well with the simulated data.
FIG. 4 is a thermogravimetric analysis (TGA) of M16 under an argon atmosphere, from which it can be seen that: the resulting M16 had already begun to lose weight at lower temperatures under an argon atmosphere.
FIG. 5 is a Scanning Electron Microscope (SEM) image of the chemical vapor deposition method to synthesize M16-CNT, from which it can be seen that: after calcination, densely distributed multi-wall carbon nanotubes are formed on the surface of the quartz substrate. The diameter of the nanotubes is about 10 nm.
FIG. 6 is a Transmission Electron Microscope (TEM) image of the chemical vapor deposition method to synthesize M16-CNT, from which it can be seen that: the obtained multi-wall carbon nano-tube is in a bamboo joint shape, and the tip of each nano-tube is attached with nano-catalytic particles. The lattice fringe spacing was 0.31nm, corresponding to the (002) crystal plane of C.
FIG. 7 is a Raman plot of M16-CNT obtained by Chemical Vapor Deposition (CVD), from which it can be seen that: the D peak/G peak is 1.2, the degree of graphitization is not high, and amorphous carbon is mainly used.
FIG. 8 shows N of M16-CNT obtained by Chemical Vapor Deposition (CVD)2The adsorption-desorption curve, as can be seen from the figure: has the characteristics of mesopores and macropores, and the specific surface area is 66.2m by the BET test2g-1。
The above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention, and it is therefore to be understood that the invention is not limited by the scope of the appended claims.
Claims (6)
1. A preparation method of a multi-walled carbon nanotube derived from thiacalixarene-based 16-nuclear molecular cluster is characterized by comprising the following steps:
(1) preparation and spin coating of M16
From 0.1mmol of tert-butylthiacalixarene H4BTC4A, 0.4mmol of NiCl2·6H2O, 0.3mmol of Dy (OAc)3·6H2O and 0.2mmol of Na2CO3In DMA/CH with volumes of 6, 3 and 0.5mL respectively3CN/ Et3Mixing in N, transferring to a reaction kettle, reacting at 130 deg.C for 6 days, and reactingSlowly cooling to room temperature to obtain green block crystal, which is named as M16, taking 1mg of macromolecular cluster M16 in a test tube, and adding 10ml of CHCl3Dissolving, and taking a drop of prepared solution to be dispersed on a quartz substrate by a spin coating method to be used as a catalyst precursor;
(2) obtaining the carbon nano tube M16-CNT by using a chemical vapor deposition method
And (2) growing the carbon nano tubes in a furnace with a 1-inch tube, placing the quartz substrate dispersed with the M16 substance obtained in the step (1) on a quartz boat, placing the quartz boat in the tube, calcining the quartz substrate in a chemical vapor deposition tube furnace in an argon atmosphere of 300 standard cubic centimeters per minute, raising the temperature of the furnace to 800 ℃ at a heating rate of 10 ℃/min, purging the system with argon, introducing a hydrogen flow of 100scc/min and ethylene of 50scc/min, and growing the carbon nano tubes at 800 ℃ for 30 minutes to obtain the carbon nano tubes densely distributed on the surface of the quartz substrate.
2. The method of preparing the thiacalixarene-based 16-nuclear molecular cluster-derived multi-walled carbon nanotubes as claimed in claim 1, wherein the method comprises the steps of: the weight average molecular weight of M16 in step (1) was 1357.
3. The method of claim 1 for preparing thiacalixarene-based 16-core molecular cluster derivatized multi-walled carbon nanotubes, wherein: the diameter of the carbon nanotubes produced was about 20 nm.
4. The method of preparing the thiacalixarene-based 16-nuclear molecular cluster-derived multi-walled carbon nanotubes as claimed in claim 1, wherein the method comprises the steps of: the obtained carbon nano-tubes are bamboo-shaped, and M16 catalyst particles are attached to the tip of each nano-tube.
5. The method of claim 1 for preparing thiacalixarene-based 16-core molecular cluster derivatized multi-walled carbon nanotubes, wherein: the obtained carbon nano tube has the characteristics of micropores and mesopores, and the specific surface area is 66.2m through a BET test2 g-1。
6. The method of preparing the thiacalixarene-based 16-nuclear molecular cluster-derived multi-walled carbon nanotubes as claimed in claim 1, wherein the method comprises the steps of: the lattice fringe spacing of the obtained carbon nanotube was 0.31nm, corresponding to the (002) crystal face of C.
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