CN111085209A - Preparation method of carbon nano tube embedded with cobalt nano particles - Google Patents
Preparation method of carbon nano tube embedded with cobalt nano particles Download PDFInfo
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- CN111085209A CN111085209A CN201811239770.6A CN201811239770A CN111085209A CN 111085209 A CN111085209 A CN 111085209A CN 201811239770 A CN201811239770 A CN 201811239770A CN 111085209 A CN111085209 A CN 111085209A
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- carbon nano
- cobalt
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- nano tube
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 38
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 38
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 25
- 239000010941 cobalt Substances 0.000 title claims abstract description 25
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000010453 quartz Substances 0.000 claims abstract description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 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 6
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 239000012535 impurity Substances 0.000 claims abstract description 6
- 229910052751 metal Inorganic materials 0.000 claims abstract description 6
- 239000002184 metal Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000007789 sealing Methods 0.000 claims abstract description 6
- 238000002791 soaking Methods 0.000 claims abstract description 6
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 238000005336 cracking Methods 0.000 abstract description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 229910000510 noble metal Inorganic materials 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 239000011149 active material Substances 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 229910001182 Mo alloy Inorganic materials 0.000 description 1
- 229910015173 MoB2 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- YGHCWPXPAHSSNA-UHFFFAOYSA-N nickel subsulfide Chemical compound [Ni].[Ni]=S.[Ni]=S YGHCWPXPAHSSNA-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Classifications
-
- 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
- B01J23/74—Iron group metals
- B01J23/75—Cobalt
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a preparation method of a carbon nano tube embedded with cobalt nano particles, which comprises the following steps: grinding and uniformly mixing cobalt nitrate and dicyandiamide, placing the mixture in a tube furnace, and calcining the mixture for 4 to 5 hours at 685-; soaking the obtained black powder in 65-75 parts of dilute sulfuric acid for 47-49h to remove impurities such as metal cobalt and the like which do not enter the carbon nano tube, so as to obtain the carbon nano tube embedded with the cobalt nano particles; and (3) putting the obtained carbon nano tube into a quartz tube, removing air in the quartz tube through a vacuum system, sealing the quartz tube, heating the quartz tube in a high-temperature furnace at 780-790 ℃ for 2.5-3.5h, and cooling to obtain the carbon nano tube. The method is simple, convenient, rapid and easy to operate, and the prepared carbon nano tube embedded with the cobalt nano particles has excellent electrocatalytic cracking water performance, can be kept stable for a long time in a catalytic environment, has huge market prospect and can be prepared in a large scale.
Description
Technical Field
The invention relates to a preparation method of a carbon nano tube embedded with cobalt nano particles.
Background
The development of clean hydrogen fuel is one of the important ways for people to get rid of the dependence on fossil fuel, and is also an effective means for solving the environmental problems caused by the current overuse of fossil fuel. Water electrolysis is one of the ideal routes for hydrogen production, which produces no greenhouse gas emissions and can utilize and convert renewable energy sources (e.g., wind, solar, etc.). However, hydrogen production from water electrolysis requires a high activation barrier to be overcome before it can occur. The noble metal platinum-based material is a high-efficiency electrocatalyst, and can remarkably reduce the energy barrier and the overpotential of hydrogen evolution reaction. However, platinum resources are scarce and expensive, which greatly limits the sustainable and large-scale application of this technology. Therefore, the development of a non-noble metal-based electrocatalytic material which is cheap, efficient and abundant in reserves is imperative. In recent years, it has become possible to provide,researchers have made a great deal of effort in the field of developing non-platinum electrocatalytic hydrogen production materials, mainly including Ni — Mo alloy, MoS2，Ni3S2，NiMoNx，MoC2And MoB2And the like. In order to further improve the catalytic activity and stability of these materials, it is an effective strategy to design composite catalysts for synthesizing carbon nanomaterials (graphene, carbon nanotubes, etc.). On one hand, the carbon coating layer can avoid the agglomeration of the nanoscale non-noble metal catalytic active material and can improve the stability of the nano-scale non-noble metal catalytic active material in a strong acid/strong base electrolyte environment; on the other hand, graphitized carbon can increase the electronic conductivity of the composite material and may create more catalytically active sites.
Disclosure of Invention
The invention aims to provide a preparation method of a carbon nano tube embedded with cobalt nano particles.
The invention is realized by the following technical scheme:
a method for preparing carbon nano-tubes embedded with cobalt nano-particles comprises the following steps: grinding and uniformly mixing 10-20 parts of cobalt nitrate and 20-30 parts of dicyandiamide, placing the mixture in a tubular furnace, and calcining the mixture for 4-5 hours at 685-695 ℃ in a nitrogen atmosphere to obtain black powder; soaking the obtained black powder in 65-75 parts of dilute sulfuric acid for 47-49h to remove impurities such as metal cobalt and the like which do not enter the carbon nano tube, so as to obtain the carbon nano tube embedded with the cobalt nano particles; putting the obtained carbon nano tube into a quartz tube, removing air in the quartz tube through a vacuum system, sealing the quartz tube, heating the quartz tube in a high-temperature furnace at 780-790 ℃ for 2.5-3.5h, and cooling to obtain the carbon nano tube; the raw materials are in parts by weight.
Preferably, in the preparation method, the calcination is carried out for 4.5h at 690 ℃ under a nitrogen atmosphere.
Preferably, in the preparation method, the obtained black powder is soaked in 70 parts of dilute sulfuric acid for 48 hours.
Preferably, in the preparation method, the mixture is placed in a high-temperature furnace and heated for 3 hours at 785 ℃.
The invention has the technical effects that:
the method is simple, convenient, rapid and easy to operate, and the prepared carbon nano tube embedded with the cobalt nano particles has excellent electrocatalytic cracking water performance, can be kept stable for a long time in a catalytic environment, has huge market prospect and can be prepared in a large scale.
Detailed Description
The following describes the substance of the present invention with reference to the examples.
Example 1
A method for preparing carbon nano-tubes embedded with cobalt nano-particles comprises the following steps: grinding and uniformly mixing 15 parts of cobalt nitrate and 25 parts of dicyandiamide, placing the mixture in a tubular furnace, and calcining the mixture for 4.5 hours at 690 ℃ in a nitrogen atmosphere to obtain black powder; soaking the obtained black powder in 70 parts of dilute sulfuric acid for 48 hours to remove impurities such as metal cobalt and the like which do not enter the carbon nano tube, so as to obtain the carbon nano tube embedded with the cobalt nano particles; filling the obtained carbon nano tube into a quartz tube, removing air in the quartz tube through a vacuum system, sealing the quartz tube, heating the quartz tube in a high-temperature furnace at 785 ℃ for 3 hours, and cooling to obtain the carbon nano tube; the raw materials are in parts by weight.
Example 2
A method for preparing carbon nano-tubes embedded with cobalt nano-particles comprises the following steps: grinding and uniformly mixing 10 parts of cobalt nitrate and 20 parts of dicyandiamide, placing the mixture in a tubular furnace, and calcining the mixture for 4 hours at 685 ℃ in a nitrogen atmosphere to obtain black powder; soaking the obtained black powder in 65 parts of dilute sulfuric acid for 47 hours to remove impurities such as metal cobalt and the like which do not enter the carbon nano tube, so as to obtain the carbon nano tube embedded with the cobalt nano particles; filling the obtained carbon nano tube into a quartz tube, removing air in the quartz tube through a vacuum system, sealing the quartz tube, heating the quartz tube in a high-temperature furnace at 780 ℃ for 2.5 hours, and cooling to obtain the carbon nano tube; the raw materials are in parts by weight.
Example 3
A method for preparing carbon nano-tubes embedded with cobalt nano-particles comprises the following steps: grinding and uniformly mixing 20 parts of cobalt nitrate and 30 parts of dicyandiamide, placing the mixture in a tubular furnace, and calcining the mixture for 5 hours at 695 ℃ in a nitrogen atmosphere to obtain black powder; soaking the obtained black powder in 75 parts of dilute sulfuric acid for 49 hours to remove impurities such as metal cobalt and the like which do not enter the carbon nano tube, so as to obtain the carbon nano tube embedded with the cobalt nano particles; filling the obtained carbon nano tube into a quartz tube, removing air in the quartz tube through a vacuum system, sealing the quartz tube, heating the quartz tube in a high-temperature furnace at 790 ℃ for 3.5 hours, and cooling to obtain the carbon nano tube; the raw materials are in parts by weight.
The method is simple, convenient, rapid and easy to operate, and the prepared carbon nano tube embedded with the cobalt nano particles has excellent electrocatalytic cracking water performance, can be kept stable for a long time in a catalytic environment, has huge market prospect and can be prepared in a large scale.
Claims (4)
1. A preparation method of a carbon nano tube embedded with cobalt nano particles is characterized by comprising the following steps: grinding and uniformly mixing 10-20 parts of cobalt nitrate and 20-30 parts of dicyandiamide, placing the mixture in a tubular furnace, and calcining the mixture for 4-5 hours at 685-695 ℃ in a nitrogen atmosphere to obtain black powder; soaking the obtained black powder in 65-75 parts of dilute sulfuric acid for 47-49h to remove impurities such as metal cobalt and the like which do not enter the carbon nano tube, so as to obtain the carbon nano tube embedded with the cobalt nano particles; putting the obtained carbon nano tube into a quartz tube, removing air in the quartz tube through a vacuum system, sealing the quartz tube, heating the quartz tube in a high-temperature furnace at 780-790 ℃ for 2.5-3.5h, and cooling to obtain the carbon nano tube; the raw materials are in parts by weight.
2. The method of claim 1, wherein: calcining at 690 ℃ for 4.5h under nitrogen atmosphere.
3. The method of claim 1, wherein: the resulting black powder was soaked with 70 parts of dilute sulfuric acid for 48 h.
4. The method of claim 1, wherein: heating at 785 deg.C for 3h in a high temperature furnace.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811239770.6A CN111085209A (en) | 2018-10-23 | 2018-10-23 | Preparation method of carbon nano tube embedded with cobalt nano particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811239770.6A CN111085209A (en) | 2018-10-23 | 2018-10-23 | Preparation method of carbon nano tube embedded with cobalt nano particles |
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| Publication Number | Publication Date |
|---|---|
| CN111085209A true CN111085209A (en) | 2020-05-01 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811239770.6A Pending CN111085209A (en) | 2018-10-23 | 2018-10-23 | Preparation method of carbon nano tube embedded with cobalt nano particles |
Country Status (1)
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| CN (1) | CN111085209A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113381030A (en) * | 2021-05-13 | 2021-09-10 | 三峡大学 | Co9S8Preparation method of-Co @ NCNTs composite electrode |
| CN113668008A (en) * | 2021-08-25 | 2021-11-19 | 常州大学 | Molybdenum disulfide/cobalt carbon nanotube electrocatalyst and preparation method and application thereof |
-
2018
- 2018-10-23 CN CN201811239770.6A patent/CN111085209A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113381030A (en) * | 2021-05-13 | 2021-09-10 | 三峡大学 | Co9S8Preparation method of-Co @ NCNTs composite electrode |
| CN113381030B (en) * | 2021-05-13 | 2022-08-05 | 三峡大学 | Co 9 S 8 Preparation method of-Co @ NCNTs composite electrode |
| CN113668008A (en) * | 2021-08-25 | 2021-11-19 | 常州大学 | Molybdenum disulfide/cobalt carbon nanotube electrocatalyst and preparation method and application thereof |
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