CN109046409A - A kind of preparation method of phosphatization cobalt-molybdenum disulfide nano sheet@carbon nanotube - Google Patents
A kind of preparation method of phosphatization cobalt-molybdenum disulfide nano sheet@carbon nanotube Download PDFInfo
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- CN109046409A CN109046409A CN201811054986.5A CN201811054986A CN109046409A CN 109046409 A CN109046409 A CN 109046409A CN 201811054986 A CN201811054986 A CN 201811054986A CN 109046409 A CN109046409 A CN 109046409A
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- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 49
- 239000002135 nanosheet Substances 0.000 title claims abstract description 27
- DDUJLRWTYLVGRH-UHFFFAOYSA-N [Co]=S.[Mo]=S Chemical compound [Co]=S.[Mo]=S DDUJLRWTYLVGRH-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- -1 sulfate-molybdenum disulfide carbon Chemical compound 0.000 claims abstract description 13
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 12
- MPMSMUBQXQALQI-UHFFFAOYSA-N cobalt phthalocyanine Chemical compound [Co+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 MPMSMUBQXQALQI-UHFFFAOYSA-N 0.000 claims abstract description 12
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004697 Polyetherimide Substances 0.000 claims abstract description 7
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 7
- 229940011182 cobalt acetate Drugs 0.000 claims abstract description 7
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims abstract description 7
- 229920001601 polyetherimide Polymers 0.000 claims abstract description 7
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims abstract description 6
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 6
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 6
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 8
- 238000002604 ultrasonography Methods 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000000725 suspension Substances 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 13
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 13
- 239000001257 hydrogen Substances 0.000 abstract description 13
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000005406 washing Methods 0.000 abstract description 4
- 239000002131 composite material Substances 0.000 abstract description 3
- 238000004146 energy storage Methods 0.000 abstract description 3
- 230000002195 synergetic effect Effects 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 239000011232 storage material Substances 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 239000006227 byproduct Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 abstract 1
- 239000013049 sediment Substances 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 description 7
- 229910017052 cobalt Inorganic materials 0.000 description 4
- 239000010941 cobalt Substances 0.000 description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 4
- 206010013786 Dry skin Diseases 0.000 description 3
- 241000209094 Oryza Species 0.000 description 3
- 235000007164 Oryza sativa Nutrition 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 235000009566 rice Nutrition 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
-
- B01J35/33—
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/185—Phosphorus; Compounds thereof with iron group metals or platinum group metals
- B01J27/1853—Phosphorus; Compounds thereof with iron group metals or platinum group metals with iron, cobalt or nickel
-
- 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
Abstract
The present invention relates to energy storage material fields, disclose a kind of preparation method of phosphatization cobalt-molybdenum disulfide nano sheet@carbon nanotube, the present invention is with sodium molybdate, polyetherimide, thiocarbamide, carbon nanotube is raw material, it takes water as a solvent, by high-temperature process, is filtered by vacuum after cooling, dry sediment obtains binary complex molybdenum disulfide nano sheet@carbon nanotube.It is dissolved in second alcohol and water using it as raw material again, reacts to form cobaltous sulfate-molybdenum disulfide carbon nanotube with cobalt acetate and ammonium hydroxide.Again by products therefrom and sodium hypophosphite mixed grinding, ternary complex is can be obtained after washing is dry in calcining.This ternary complex with the method synthesis of cheap environmental protection with high catalytic activity, high-efficient, yield is also high.And obtained product large specific surface area, hydrogen evolution activity site is more, has higher electrocatalytic hydrogen evolution activity.Due to the synergistic effect between unique microstructure and more exposed active site, composite material significantly improves catalytic performance.
Description
Technical field
The present invention relates to energy storage material field more particularly to a kind of phosphatization cobalt-molybdenum disulfide nano sheet@carbon nanotube systems
Preparation Method.
Background technique
For the energy crisis got worse, people all find one kind can replace coal, the clean and environmental protection energy of petroleum.
Hydrogen is efficiently favored by people with the clean of it.Currently, water electrolysis hydrogen producing is most environmentally friendly hydrogen manufacturing mode.But electro-catalysis
Hydrogen manufacturing causes energy consumption higher there are the higher problem of overpotential of hydrogen evolution.Conventional precious metal catalyst is because of its high cost, low reserves limitation
Its large-scale application.Therefore a kind of low cost is found, the good catalyst of performance is applied on the energy urgently can not be to.
Molybdenum disulfide is a kind of transient metal sulfide semiconductor, because it is with biggish specific surface area, surface-active compared with
Height, low in cost, the features such as excellent chemical stability and thermal stability, is paid close attention to by people.Be considered as by people has prospect very much
Electrocatalytic hydrogen evolution catalyst, it is most likely that instead of precious metals pt as elctro-catalyst.
In recent years, it emerges one after another to the catalytic activity research such as transition metal alloy, nitride, carbide and phosphide,
In more metal phosphides, since the proton/electron transfer rate and hydrogen rate of release of phosphatization cobalt are very fast, have excellent
Catalytic activity can be used as catalyst use.
Summary of the invention
In order to solve the above-mentioned technical problems, the present invention provides a kind of phosphatization cobalt-molybdenum disulfide nano sheet@carbon nanotubes
Preparation method, the ternary complex that the present invention is formed with relatively inexpensive phosphatization cobalt, molybdenum disulfide nano sheet and carbon nanotube, obtains
The product large specific surface area arrived, greatly improves hydrogen evolution activity site, has higher electrocatalytic hydrogen evolution activity.Due to uniqueness
Microstructure and more exposed active site between synergistic effect, composite material significantly improves catalytic performance.It is this new
The ternary complex of type has great potentiality to replace expensive commercial Pt/C catalyst, very widely used.
The specific technical proposal of the invention is: a kind of phosphatization cobalt-molybdenum disulfide nano sheet@carbon nanotube preparation method,
In terms of g and mL, comprising the following steps:
1) 1 ~ 2g sodium molybdate, 0.5 ~ 1.0g polyetherimide are taken, 1 ~ 2g thiocarbamide and 0.5 ~ 1.0g carbon nanotube are dissolved in 50-
In 80mL deionized water, ultrasound, stirring is transferred in polytetrafluoroethyllining lining autoclave, reacts 22 at 200 ~ 240 DEG C
It ~ 26 hours, is cooled to room temperature, is filtered by vacuum, wash drying to get molybdenum disulfide nano sheet@carbon nanotube is arrived.
Ultrasound and stirring are to be wrapped in later period molybdenum disulfide nano sheet equably to be uniformly distributed polyetherimide
Carbon nano tube surface.And desired product is more readily formed at high temperature under high pressure.
2) it takes 0.1 ~ 0.5g molybdenum disulfide nano sheet@carbon nanotube that 50 ~ 80mL ethyl alcohol and 2 ~ 3mL deionized water is added, surpasses
Sound dispersion, is added the cobalt acetate and 20 ~ 30mL ammonium hydroxide of 2 ~ 5mL 0.6M, is stirred at room temperature uniformly, by suspension at 60 ~ 80 DEG C
Lower stirring 20 ~ 25 hours, is transferred in polytetrafluoroethyllining lining autoclave, small in 130 ~ 150 DEG C of at a temperature of reaction 2 ~ 5
When, after cooling, washed with alcohol and deionized water.Obtain cobaltous sulfate-molybdenum disulfide carbon nanotube.
By ultrasound and stirring, the impurity of molybdenum disulfide nano sheet@carbon nano tube surface is removed, and is uniformly dispersed,
A certain proportion of cobalt acetate and ammonium hydroxide and preceding product, at the temperature and high pressure lower compared with front, convenient for forming desired product
Ideal form.
3) 0.1 ~ 0.3g cobaltous sulfate-molybdenum disulfide@carbon nanotube and 0.5 ~ 1.0g sodium hypophosphite, mixed grinding, in horse are taken
300 ~ 350 DEG C not are warming up to 2 ~ 3 DEG C of heating rate per minute in furnace, and keeps 300 ~ 350 DEG C of temperature calcination 2 ~ 3 small
When, the product of acquisition is washed with deionized, it is dry to get phosphatization cobalt-molybdenum disulfide nano sheet@carbon nanotube.
Particle becomes smaller after grinding, increases reactant contact area, improves the efficiency for generating compound.
By cobaltous sulfate-molybdenum disulfide@carbon nanotube and sodium hypophosphite high-temperature calcination, complicated chemical reaction can produce,
So that phosphatization cobalt is attached to the surface of molybdenum disulfide nano sheet@carbon nanotube, ternary complex is formed.
Preferably, in step 1), ultrasonic time 20-30min, mixing time 5-8h.
Preferably, in step 2,5 ~ 8min of ultrasonic disperse.
Preferably, drying temperature is 60-80 DEG C in step 3).
It is compared with the prior art, the beneficial effects of the present invention are:
Step of the present invention is simple, high-efficient, and yield is also high, and required solvent is water, can make in environmental-friendly and cheap method
The ternary complex for producing phosphatization cobalt, molybdenum disulfide and carbon nanotube improves energy storage capacity, and obtained product specific surface
Product is big, greatly improves hydrogen evolution activity site, has higher electrocatalytic hydrogen evolution activity.Due to unique microstructure and more
Synergistic effect between exposed active site, composite material significantly improve catalytic performance.This novel ternary complex
There are great potentiality to replace expensive commercial Pt/C catalyst, it is very widely used.
Specific embodiment
The present invention will be further described with reference to the examples below.
Embodiment 1
(1) 1.45 grams of sodium molybdate, 0.5 gram of polyetherimide, 1.37 grams of thiocarbamide and the dissolution of 0.5 gram of carbon nanotube are taken
In the deionized water of 60mL, ultrasound 30 minutes, and after stirring 6 hours, it is transferred to the autoclave of polytetrafluoroethyllining lining
In, 220 DEG C at a temperature of react 24 hours, be cooled to room temperature, be filtered by vacuum, wash drying, molybdenum disulfide can be obtained and receive
Rice piece@carbon nanotube.
(2) take 0.1 gram of molybdenum disulfide nano sheet@carbon nanotube that 60mL ethyl alcohol and 2.5mL deionized water, ultrasonic disperse is added
5 minutes, the cobalt acetate of 3mL0.6M and the ammonium hydroxide of 25mL is added, is stirred at room temperature uniformly, suspension is stirred 20 at 80 DEG C
Hour, be transferred in the autoclave of polytetrafluoroethyllining lining, 150 DEG C at a temperature of react 3 hours, after cooling, use wine
Essence and deionized water washing.Cobaltous sulfate-molybdenum disulfide@carbon nanotube can be obtained.
(3) 0.1 gram of cobaltous sulfate-molybdenum disulfide@carbon nanotube and 0.5 gram of (in terms of weight g) sodium hypophosphite are taken, mixing is ground
Mill is warming up to 300 DEG C in Muffle furnace with 2 DEG C of heating rate per minute, and is kept for temperature calcination 2 hours of 300 DEG C, will obtain
The product obtained is washed with deionized, and in 80 DEG C of dryings, can obtain phosphatization cobalt-molybdenum disulfide nano sheet@carbon nanotube.
Embodiment 2
(1) 1.05 grams of sodium molybdate, 0.5 gram of polyetherimide, 1.07 grams of thiocarbamide and the dissolution of 0.5 gram of carbon nanotube are taken
In the deionized water of 50mL, ultrasound 20 minutes, and after stirring 5 hours, it is transferred to the autoclave of polytetrafluoroethyllining lining
In, 200 DEG C at a temperature of react 22 hours, be cooled to room temperature, be filtered by vacuum, wash drying, molybdenum disulfide can be obtained and receive
Rice piece@carbon nanotube.
(2) take 0.1 gram of molybdenum disulfide nano sheet@carbon nanotube that 50mL ethyl alcohol and 2.0mL deionized water, ultrasonic disperse is added
5 minutes, the cobalt acetate of 2mL0.6M and the ammonium hydroxide of 20mL is added, is stirred at room temperature uniformly, suspension is stirred 20 at 60 DEG C
Hour, be transferred in the autoclave of polytetrafluoroethyllining lining, 130 DEG C at a temperature of react 2 hours, after cooling, use wine
Essence and deionized water washing.Cobaltous sulfate-molybdenum disulfide@carbon nanotube can be obtained.
(3) 0.1 gram of cobaltous sulfate-molybdenum disulfide@carbon nanotube and 0.5 gram of (in terms of weight g) sodium hypophosphite are taken, mixing is ground
Mill is warming up to 300 DEG C in Muffle furnace with 2 DEG C of heating rate per minute, and is kept for temperature calcination 2 hours of 300 DEG C, will obtain
The product obtained is washed with deionized, and in 60 DEG C of dryings, can obtain phosphatization cobalt-molybdenum disulfide nano sheet@carbon nanotube.
Embodiment 3
(1) 2.00 grams of sodium molybdate, 1.0 grams of polyetherimide, 2.00 grams of thiocarbamide and the dissolution of 1.0 grams of carbon nanotube are taken
In the deionized water of 80mL, ultrasound 40 minutes, and after stirring 8 hours, it is transferred to the autoclave of polytetrafluoroethyllining lining
In, 240 DEG C at a temperature of react 26 hours, be cooled to room temperature, be filtered by vacuum, wash drying, molybdenum disulfide can be obtained and receive
Rice piece@carbon nanotube.
(2) take 0.5 gram of molybdenum disulfide nano sheet@carbon nanotube that 80mL ethyl alcohol and 3mL deionized water, ultrasonic disperse 8 is added
Minute, the cobalt acetate of 5mL0.6M and the ammonium hydroxide of 30mL is added, is stirred at room temperature uniformly, suspension is stirred 25 at 80 DEG C
Hour, be transferred in the autoclave of polytetrafluoroethyllining lining, 150 DEG C at a temperature of react 5 hours, after cooling, use wine
Essence and deionized water washing.Cobaltous sulfate-molybdenum disulfide@carbon nanotube can be obtained.
(3) 0.3 gram of cobaltous sulfate-molybdenum disulfide@carbon nanotube and 1.0 grams of (in terms of weight g) sodium hypophosphites are taken, mixing is ground
Mill is warming up to 350 DEG C in Muffle furnace with 3 DEG C of heating rate per minute, and is kept for temperature calcination 3 hours of 300 DEG C, will obtain
The product obtained is washed with deionized, and in 80 DEG C of dryings, can obtain phosphatization cobalt-molybdenum disulfide nano sheet@carbon nanotube.
Raw materials used in the present invention, equipment is unless otherwise noted the common raw material, equipment of this field；It is used in the present invention
Method is unless otherwise noted the conventional method of this field.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way, it is all according to the present invention
Technical spirit any simple modification, change and equivalent transformation to the above embodiments, still fall within the technology of the present invention side
The protection scope of case.
Claims (4)
1. a kind of phosphatization cobalt-molybdenum disulfide nano sheet@carbon nanotube preparation method, which is characterized in that in terms of g and mL, including
Following steps:
1) 1 ~ 2g sodium molybdate, 0.5 ~ 1.0g polyetherimide are taken, 1 ~ 2g thiocarbamide and 0.5 ~ 1.0g carbon nanotube are dissolved in 50-
In 80mL deionized water, ultrasound, stirring is transferred in polytetrafluoroethyllining lining autoclave, reacts 22 at 200 ~ 240 DEG C
It ~ 26 hours, is cooled to room temperature, is filtered by vacuum, wash drying to get molybdenum disulfide nano sheet@carbon nanotube is arrived；
2) take 0.1 ~ 0.5g molybdenum disulfide nano sheet@carbon nanotube that 50 ~ 80mL ethyl alcohol and 2 ~ 3mL deionized water, ultrasound point is added
It dissipates, the cobalt acetate and 20 ~ 30mL ammonium hydroxide of 2 ~ 5mL 0.6M is added, be stirred at room temperature uniformly, suspension is stirred at 60 ~ 80 DEG C
Mix 20 ~ 25 hours, be transferred in polytetrafluoroethyllining lining autoclave, 130 ~ 150 DEG C at a temperature of react 2 ~ 5 hours,
After cooling, washed with alcohol and deionized water；
Obtain cobaltous sulfate-molybdenum disulfide carbon nanotube；
3) 0.1 ~ 0.3g cobaltous sulfate-molybdenum disulfide@carbon nanotube and 0.5 ~ 1.0g sodium hypophosphite, mixed grinding, in Muffle furnace are taken
In with 2 ~ 3 DEG C of heating rate per minute be warming up to 300 ~ 350 DEG C, and kept for temperature calcination 2 ~ 3 hours of 300 ~ 350 DEG C, will
The product of acquisition is washed with deionized, dry to get phosphatization cobalt-molybdenum disulfide nano sheet@carbon nanotube.
2. a kind of preparation method of phosphatization cobalt-molybdenum disulfide nano sheet@carbon nanotube as described in claim 1, feature exist
In, in step 1), ultrasonic time 20-30min, mixing time 5-8h.
3. a kind of preparation method of phosphatization cobalt-molybdenum disulfide nano sheet@carbon nanotube as described in claim 1, feature exist
In, in step 2,5 ~ 8min of ultrasonic disperse.
4. a kind of preparation method of phosphatization cobalt-molybdenum disulfide nano sheet@carbon nanotube as described in claim 1, feature exist
In in step 3), drying temperature is 60-80 DEG C.
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| CN111068694A (en) * | 2019-12-03 | 2020-04-28 | 上海工程技术大学 | Cobalt-molybdenum composite/carbon fiber composite material of nano array and preparation method thereof |
| CN113040169A (en) * | 2021-03-09 | 2021-06-29 | 泉州师范学院 | Carbon doped MoS2/CoP/C composite antibacterial material and preparation method and application thereof |
| WO2023174768A1 (en) | 2022-03-18 | 2023-09-21 | IFP Energies Nouvelles | Catalytic material based on a group vib element and a group ivb element for the production of hydrogen by electrolysis of water |
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| CN111068694A (en) * | 2019-12-03 | 2020-04-28 | 上海工程技术大学 | Cobalt-molybdenum composite/carbon fiber composite material of nano array and preparation method thereof |
| CN113040169A (en) * | 2021-03-09 | 2021-06-29 | 泉州师范学院 | Carbon doped MoS2/CoP/C composite antibacterial material and preparation method and application thereof |
| CN113040169B (en) * | 2021-03-09 | 2021-11-23 | 泉州师范学院 | Carbon doped MoS2/CoP/C composite antibacterial material and preparation method and application thereof |
| WO2023174768A1 (en) | 2022-03-18 | 2023-09-21 | IFP Energies Nouvelles | Catalytic material based on a group vib element and a group ivb element for the production of hydrogen by electrolysis of water |
| FR3133544A1 (en) | 2022-03-18 | 2023-09-22 | IFP Energies Nouvelles | Catalytic material based on a group VIB element and a group IVB element for the production of hydrogen by water electrolysis |
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