CN110508295A - A kind of preparation method of molybdenum sulfide doped cadmium sulfide micro Nano material and its application in Photocatalyzed Hydrogen Production - Google Patents
A kind of preparation method of molybdenum sulfide doped cadmium sulfide micro Nano material and its application in Photocatalyzed Hydrogen Production Download PDFInfo
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- CN110508295A CN110508295A CN201910718541.0A CN201910718541A CN110508295A CN 110508295 A CN110508295 A CN 110508295A CN 201910718541 A CN201910718541 A CN 201910718541A CN 110508295 A CN110508295 A CN 110508295A
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- cadmium
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- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910052980 cadmium sulfide Inorganic materials 0.000 title claims abstract description 37
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 30
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 27
- 239000001257 hydrogen Substances 0.000 title claims abstract description 27
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 14
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 7
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 7
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001291 vacuum drying Methods 0.000 claims abstract description 7
- 238000010792 warming Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 150000001661 cadmium Chemical class 0.000 claims abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 5
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims abstract description 4
- 125000003396 thiol group Chemical group [H]S* 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethyl mercaptane Natural products CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 claims description 4
- KOUKXHPPRFNWPP-UHFFFAOYSA-N pyrazine-2,5-dicarboxylic acid;hydrate Chemical compound O.OC(=O)C1=CN=C(C(O)=O)C=N1 KOUKXHPPRFNWPP-UHFFFAOYSA-N 0.000 claims description 4
- -1 sulfhydryl compound Chemical class 0.000 claims description 4
- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 claims description 4
- 229910052793 cadmium Inorganic materials 0.000 claims description 3
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical group [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 claims description 2
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims description 2
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- GATXPHDUDVSRCV-UHFFFAOYSA-N [Cl].[Cd] Chemical compound [Cl].[Cd] GATXPHDUDVSRCV-UHFFFAOYSA-N 0.000 claims 1
- 150000001408 amides Chemical class 0.000 claims 1
- 239000006227 byproduct Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 239000000047 product Substances 0.000 claims 1
- 125000000446 sulfanediyl group Chemical group *S* 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 238000007146 photocatalysis Methods 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000003245 coal Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000003208 petroleum Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- FRLJSGOEGLARCA-UHFFFAOYSA-N cadmium sulfide Chemical class [S-2].[Cd+2] FRLJSGOEGLARCA-UHFFFAOYSA-N 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000001144 powder X-ray diffraction data Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 description 1
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
-
- 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)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Combustion & Propulsion (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of preparation method of molybdenum sulfide doped cadmium sulfide micro Nano material and its applications in Photocatalyzed Hydrogen Production, 0.4mmoL cadmium salt is weighed to be put into 100mL beaker, 100 μ L sulfhydryl compounds stirring 30min is added, the pH value for adding NaOH adjustment mixed system is 6.0-8.0, 4mL is added dropwise, 0.25moL/L sulfide solution is into beaker, solution is in yellow green, then 0.0097g sodium molybdate is added and 0.0122g thiocarbamide stirs 30min, above-mentioned mixed solution is transferred in resolvent hydrothermal reaction kettle, 160-200 DEG C of constant temperature is warming up to for 24 hours with the heating rate of 3 DEG C/min, 30 DEG C are cooled to again with the rate of temperature fall of 3 DEG C/min, vacuum drying after product centrifuge washing is obtained target to produce Object molybdenum sulfide doped cadmium sulfide micro Nano material.The molybdenum sulfide doped cadmium sulfide micro Nano material that the present invention synthesizes has absorption in ultraviolet region and visible region, Photocatalyzed Hydrogen Production field with good application prospect.
Description
Technical field
The invention belongs to the synthesis technical fields of catalysis material, and in particular to a kind of molybdenum sulfide doped cadmium sulfide is micro-nano
The preparation method of material and its application in Photocatalyzed Hydrogen Production.
Background technique
In 21 century, energy and environment problem has become the theme of World Focusing, at present the energy used in human society
If petroleum, coal, oil gas belong to non-renewable resources, storage is limited on the earth, in the exploitation that recent decades have been over
And utilization, since the reserves of coal and petroleum on earth are limited, and they are all the non-renewable energy, thus coal and
Petroleum has been unable to meet the industrial requirement of sustainable development.In addition, the burning of coal and petroleum can generate many poisonous and hazardous objects
Matter seriously pollutes environment.It is understood that combustion of fossil fuel can release a large amount of carbon dioxide, present greenhouse effects is caused to get over
Come more serious, therefore there is an urgent need to develop novel renewable and clean environment type new energy.The appearance of photocatalysis hydrogen production technology
Solution is provided to solve energy shortage and problem of environmental pollution, catalyst can be by the reducing hydrogen ions Cheng Qing in water
Gas, and water is generated again after combustion of hydrogen, there is no any pollution to environment.In addition, tellurian water resource is very rich, institute
To there is enough hydrogen sources, and sunlight can provide light source for photochemical catalyst, therefore photocatalysis hydrogen production technology both solved
Problem of energy crisis in turn avoids the pollution to environment, therefore the research and development of photochemical catalyst also suddenly become current international hot topic and grind
Study carefully one of field.
Cadmium sulfide (CdS) is a kind of extensive photochemical catalyst of research, but some defects existing for CdS itself limit CdS
Application in terms of Photocatalyzed Hydrogen Production.The compound rate of one side CdS photogenerated charge itself is very fast, and photocatalysis generates the work of hydrogen
Property is lower.Therefore in order to improve the activity of CdS Photocatalyzed Hydrogen Production, it is necessary in the area load noble metal of CdS, such as Pt, with
Its Photocatalyzed Hydrogen Production activity is improved, but noble metal is expensive.The MoS of two-dimensional structure2Because its suitable band structure and compared with
Narrow forbidden bandwidth (about 1.9eV) is considered as optimal candidate co-catalyst.And it is reported that MoS2No matter in electricity
There is very high catalytic effect in terms of catalyzing manufacturing of hydrogen or photocatalysis hydrogen production.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of environmentally protective and simple process molybdenum sulfide doped cadmium sulfides
The preparation method of micro Nano material, molybdenum sulfide doped cadmium sulfide micro Nano material made from this method are produced with good photocatalysis
Hydrogen activity, can as photochemical catalyst by the reducing hydrogen ions in water at hydrogen.
The present invention adopts the following technical scheme that solve above-mentioned technical problem, a kind of micro-nano material of molybdenum sulfide doped cadmium sulfide
The preparation method of material, it is characterised in that specific steps are as follows: weigh 0.4mmoL cadmium salt and be put into 100mL beaker, 100 μ L mercaptos are added
Based compound stirs 30min, and the pH value for adding NaOH adjustment mixed system is 6.0-8.0, and 4mL, 0.25moL/L vulcanization is added dropwise
For object solution into beaker, solution is in yellow green, and 0.0097g sodium molybdate is then added and 0.0122g thiocarbamide stirs 30min, will be upper
It states mixed solution and is transferred in resolvent hydrothermal reaction kettle and 160-200 DEG C of constant temperature is warming up to for 24 hours with the heating rate of 3 DEG C/min,
30 DEG C are cooled to the rate of temperature fall of 3 DEG C/min again, vacuum drying after product centrifuge washing is obtained into target product molybdenum sulfide and is mixed
Miscellaneous cadmium sulfide micro Nano material, the cadmium salt are cadmium acetate, caddy or cadmium nitrate, and the sulfhydryl compound is mercaptoethanol
Acid, thioacetic acid or mercaptopropionic acid, the sulfide are thioacetamide, vulcanized sodium or ammonium sulfide.
Application of the molybdenum sulfide doped cadmium sulfide micro Nano material of the present invention in Photocatalyzed Hydrogen Production, the molybdenum sulfide are mixed
When the optimum mole ratio of Cd and Mo is 10:1 in miscellaneous cadmium sulfide micro Nano material, Photocatalyzed Hydrogen Production efficiency can reach 235.41 μ
mol g-1 h-1。
Compared with the prior art, the invention has the following beneficial effects: the micro-nano material of molybdenum sulfide doped cadmium sulfide in the present invention
The synthesis process of material is simple and low in cost, and the molybdenum sulfide doped cadmium sulfide micro Nano material of synthesis is not soluble in water, urges conducive to light
The recycling and recycling of agent；The molybdenum sulfide doped cadmium sulfide micro Nano material of synthesis has in ultraviolet region and visible region
Absorb, Photocatalyzed Hydrogen Production field with good application prospect.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of molybdenum sulfide doped cadmium sulfide micro Nano material made from embodiment 1；
Fig. 2 is the scanning electron microscope (SEM) photograph of molybdenum sulfide doped cadmium sulfide micro Nano material made from embodiment 1；
Fig. 3 is the Powder XRD pattern of molybdenum sulfide doped cadmium sulfide micro Nano material made from embodiment 1；
Fig. 4 is that the uv-vis spectra of molybdenum sulfide doped cadmium sulfide micro Nano material made from embodiment 1 absorbs map.
Specific embodiment
Above content of the invention is described in further details by the following examples, but this should not be interpreted as to this
The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on above content of the present invention belong to this hair
Bright range.
Embodiment 1
Electronic balance precise 0.4mmoL cadmium acetate is put into 100mL beaker, and 100 μ L thioacetic acid are added and stir 30min,
The pH value for adding NaOH adjustment mixed system is 6.2,4mL, 0.25moL/L TAA solution is added dropwise into beaker, solution is in Huang
Green, is then added 0.0097g sodium molybdate and 0.0122g thiocarbamide stirs 30min, and above-mentioned mixed solution is transferred to resolvent water
200 DEG C of constant temperature are warming up to the heating rate of 3 DEG C/min in thermal response kettle and for 24 hours, then with the rate of temperature fall of 3 DEG C/min are cooled to 30
DEG C, vacuum drying after product centrifuge washing is obtained into target product molybdenum sulfide doped cadmium sulfide micro Nano material.
Embodiment 2
Electronic balance precise 0.4mmoL caddy is put into 100mL beaker, and 100 μ L thioacetic acid are added and stir 30min,
The pH value for adding NaOH adjustment mixed system is 6.2,4mL, 0.25moL/L TAA solution is added dropwise into beaker, solution is in Huang
Green, is then added 0.0097g sodium molybdate and 0.0122g thiocarbamide stirs 30min, and above-mentioned mixed solution is transferred to resolvent water
200 DEG C of constant temperature are warming up to the heating rate of 3 DEG C/min in thermal response kettle and for 24 hours, then with the rate of temperature fall of 3 DEG C/min are cooled to 30
DEG C, vacuum drying after product centrifuge washing is obtained into target product molybdenum sulfide doped cadmium sulfide micro Nano material.
Embodiment 3
Electronic balance precise 0.4mmoL caddy is put into 100mL beaker, and the stirring of 100 μ L mercaptoethanol acid is added
30min, the pH value for adding NaOH adjustment mixed system is 6.2, and 4mL, 0.25moL/L TAA solution is added dropwise into beaker, molten
Liquid is in yellow green, and 0.0097g sodium molybdate is then added and 0.0122g thiocarbamide stirs 30min, above-mentioned mixed solution is transferred to and is disappeared
200 DEG C of constant temperature are warming up to for 24 hours with the heating rate of 3 DEG C/min in solution formula hydrothermal reaction kettle, then are dropped with the rate of temperature fall of 3 DEG C/min
Temperature obtains target product molybdenum sulfide doped cadmium sulfide micro Nano material to 30 DEG C, by vacuum drying after product centrifuge washing.
Embodiment 4
Electronic balance precise 0.4mmoL caddy is put into 100mL beaker, and the stirring of 100 μ L mercaptoethanol acid is added
30min, the pH value for adding NaOH adjustment mixed system is 6.2, and 4mL, 0.25moL/L Na is added dropwise2S solution is molten into beaker
Liquid is in yellow green, and 0.0097g sodium molybdate is then added and 0.0122g thiocarbamide stirs 30min, above-mentioned mixed solution is transferred to and is disappeared
200 DEG C of constant temperature are warming up to for 24 hours with the heating rate of 3 DEG C/min in solution formula hydrothermal reaction kettle, then are dropped with the rate of temperature fall of 3 DEG C/min
Temperature obtains target product molybdenum sulfide doped cadmium sulfide micro Nano material to 30 DEG C, by vacuum drying after product centrifuge washing.
Embodiment 5
The application of molybdenum sulfide doped cadmium sulfide micro Nano material Photocatalyzed Hydrogen Production
The molybdenum sulfide doped cadmium sulfide micro Nano material 25mg prepared is weighed, molybdenum sulfide doped cadmium sulfide micro Nano material is fallen
Containing Na2SO3And Na2It is uniform with magnetic stirrer in the quartz reactor of the 50mL aqueous solution of S, in the xenon lamp of 300W
Light source irradiation is lower to be tested with photocatalytic water H2-producing capacity of Labsolar-III (AG) system to sample.And pass through photocatalysis system
Hydrogen experiment show that the optimum mole ratio of Cd and Mo in molybdenum sulfide doped cadmium sulfide micro Nano material is 10:1, Photocatalyzed Hydrogen Production efficiency
235.41 μm of ol g can be reached-1 h-1。
Embodiment above describes basic principles and main features of the invention and advantage, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe originals of the invention
Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (2)
1. a kind of preparation method of molybdenum sulfide doped cadmium sulfide micro Nano material, it is characterised in that specific steps are as follows: weigh
0.4mmoL cadmium salt is put into 100mL beaker, and 100 μ L sulfhydryl compounds are added and stir 30min, adds NaOH adjustment mixture
The pH value of system is 6.0-8.0, and 4mL, 0.25moL/L sulfide solution is added dropwise into beaker, and solution is in yellow green, is then added
0.0097g sodium molybdate and 0.0122g thiocarbamide stir 30min, and above-mentioned mixed solution is transferred in resolvent hydrothermal reaction kettle with 3
DEG C/heating rate of min is warming up to 160-200 DEG C of constant temperature for 24 hours, then is cooled to 30 DEG C with the rate of temperature fall of 3 DEG C/min, by product
Vacuum drying obtains target product molybdenum sulfide doped cadmium sulfide micro Nano material after centrifuge washing, and the cadmium salt is cadmium acetate, chlorine
Cadmium or cadmium nitrate, the sulfhydryl compound are mercaptoethanol acid, thioacetic acid or mercaptopropionic acid, and the sulfide is thio second
Amide, vulcanized sodium or ammonium sulfide.
2. molybdenum sulfide doped cadmium sulfide micro Nano material is in Photocatalyzed Hydrogen Production made from the method according to claim 11
Using, when the optimum mole ratio of Cd and Mo is 10:1 in the molybdenum sulfide doped cadmium sulfide micro Nano material, Photocatalyzed Hydrogen Production efficiency
235.41 μm of ol g can be reached-1 h-1。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112237839A (en) * | 2020-09-30 | 2021-01-19 | 福建农林大学 | Construction method and application of transition metal mediated semi-artificial photosynthesis system |
| CN114308079A (en) * | 2021-12-31 | 2022-04-12 | 武汉工程大学 | Cadmium sulfide-double-cocatalyst composite photocatalytic material and preparation method and application thereof |
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| CN114950492B (en) * | 2022-05-31 | 2023-09-08 | 安徽大学 | 1, 2-diaminoanthraquinone-molybdenum disulfide composite antibacterial material for photoelectrocatalysis to kill bacteria |
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