CN109331843A - Graininess multicomponent sulfide-platinum heterojunction photocatalysis composite material and preparation method thereof and its production hydrogen application - Google Patents
Graininess multicomponent sulfide-platinum heterojunction photocatalysis composite material and preparation method thereof and its production hydrogen application Download PDFInfo
- Publication number
- CN109331843A CN109331843A CN201811245436.1A CN201811245436A CN109331843A CN 109331843 A CN109331843 A CN 109331843A CN 201811245436 A CN201811245436 A CN 201811245436A CN 109331843 A CN109331843 A CN 109331843A
- Authority
- CN
- China
- Prior art keywords
- platinum
- multicomponent
- sulfide
- composite material
- graininess
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 112
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 85
- 239000002131 composite material Substances 0.000 title claims abstract description 79
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 67
- 238000007146 photocatalysis Methods 0.000 title claims abstract description 64
- 239000001257 hydrogen Substances 0.000 title claims abstract description 55
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 55
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims abstract description 48
- 238000000034 method Methods 0.000 claims abstract description 37
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000006303 photolysis reaction Methods 0.000 claims abstract description 20
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 20
- 239000011593 sulfur Substances 0.000 claims abstract description 18
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 16
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 16
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 14
- 239000011733 molybdenum Substances 0.000 claims abstract description 14
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000010937 tungsten Substances 0.000 claims abstract description 14
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 11
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 11
- 239000003960 organic solvent Substances 0.000 claims abstract description 9
- 230000015843 photosynthesis, light reaction Effects 0.000 claims abstract description 9
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 7
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 7
- 239000007791 liquid phase Substances 0.000 claims abstract description 4
- XAOZEFQFJOAXBP-UHFFFAOYSA-N [Mo].CN(C(S)=S)C Chemical compound [Mo].CN(C(S)=S)C XAOZEFQFJOAXBP-UHFFFAOYSA-N 0.000 claims abstract description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 30
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 9
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical compound CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- 230000003197 catalytic effect Effects 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- UDWCKMMKPOGURO-UHFFFAOYSA-N 1,2-dihydropyrazolo[3,4-b]pyridin-4-one Chemical compound O=C1C=CNC2=C1C=NN2 UDWCKMMKPOGURO-UHFFFAOYSA-N 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- 239000004310 lactic acid Substances 0.000 claims description 6
- 235000014655 lactic acid Nutrition 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 4
- 150000002751 molybdenum Chemical class 0.000 claims description 4
- 150000003657 tungsten Chemical class 0.000 claims description 4
- GSFSVEDCYBDIGW-UHFFFAOYSA-N 2-(1,3-benzothiazol-2-yl)-6-chlorophenol Chemical compound OC1=C(Cl)C=CC=C1C1=NC2=CC=CC=C2S1 GSFSVEDCYBDIGW-UHFFFAOYSA-N 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 3
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- -1 dimethyl dithiocarbamic acid tungsten Chemical compound 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 230000003287 optical effect Effects 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- GICWIDZXWJGTCI-UHFFFAOYSA-I molybdenum pentachloride Chemical group Cl[Mo](Cl)(Cl)(Cl)Cl GICWIDZXWJGTCI-UHFFFAOYSA-I 0.000 claims description 2
- KPGXUAIFQMJJFB-UHFFFAOYSA-H tungsten hexachloride Chemical group Cl[W](Cl)(Cl)(Cl)(Cl)Cl KPGXUAIFQMJJFB-UHFFFAOYSA-H 0.000 claims description 2
- 229910052724 xenon Inorganic materials 0.000 claims description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 2
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 claims 1
- 150000003462 sulfoxides Chemical class 0.000 claims 1
- MZGNSEAPZQGJRB-UHFFFAOYSA-N dimethyldithiocarbamic acid Chemical compound CN(C)C(S)=S MZGNSEAPZQGJRB-UHFFFAOYSA-N 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 2
- 230000009467 reduction Effects 0.000 abstract description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract 1
- VMSRVIHUFHQIAL-UHFFFAOYSA-M sodium;n,n-dimethylcarbamodithioate Chemical compound [Na+].CN(C)C([S-])=S VMSRVIHUFHQIAL-UHFFFAOYSA-M 0.000 abstract 1
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 15
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 14
- 239000004065 semiconductor Substances 0.000 description 9
- 239000003054 catalyst Substances 0.000 description 8
- 239000003921 oil Substances 0.000 description 5
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 4
- CJOBVZJTOIVNNF-UHFFFAOYSA-N cadmium sulfide Chemical compound [Cd]=S CJOBVZJTOIVNNF-UHFFFAOYSA-N 0.000 description 4
- 238000012512 characterization method Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000005864 Sulphur Substances 0.000 description 3
- 238000013459 approach Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 238000001782 photodegradation Methods 0.000 description 3
- 238000004073 vulcanization Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 239000003426 co-catalyst Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- WQOXQRCZOLPYPM-UHFFFAOYSA-N dimethyl disulfide Chemical compound CSSC WQOXQRCZOLPYPM-UHFFFAOYSA-N 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000000877 morphologic effect Effects 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- VQNPSCRXHSIJTH-UHFFFAOYSA-N cadmium(2+);carbanide Chemical compound [CH3-].[CH3-].[Cd+2] VQNPSCRXHSIJTH-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- JVEOCWZEOQDIIK-UHFFFAOYSA-N formic acid;molybdenum Chemical compound [Mo].OC=O JVEOCWZEOQDIIK-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- KHYKFSXXGRUKRE-UHFFFAOYSA-J molybdenum(4+) tetracarbamodithioate Chemical compound C(N)([S-])=S.[Mo+4].C(N)([S-])=S.C(N)([S-])=S.C(N)([S-])=S KHYKFSXXGRUKRE-UHFFFAOYSA-J 0.000 description 1
- PDKHNCYLMVRIFV-UHFFFAOYSA-H molybdenum;hexachloride Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Mo] PDKHNCYLMVRIFV-UHFFFAOYSA-H 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000011885 synergistic combination Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002023 wood Substances 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
-
- 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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
-
- 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
- C01B2203/1094—Promotors or activators
-
- 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
Landscapes
- 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 graininess multicomponent sulfide-platinum heterojunction photocatalysis composite material and preparation method thereof and its produce hydrogen application.The preparation method includes the following steps: S1: reacting to obtain sulfur-bearing molybdenum source dimethyl dithiocarbamic acid molybdenum Mo (dedc) using chloride and Sodium Dimethyldithiocarbamate5With tungsten source dimethyl dithiocarbamic acid W (dedc)6；S2: sulfur-bearing molybdenum source, tungsten source and cadmium source presoma being added in organic solvent, are sufficiently stirred, and are uniformly mixed, are obtained forerunner's reaction solution；S3: forerunner's reaction solution is subjected to a step liquid phase microwave assisting method rapid synthesis, obtains multicomponent sulfide composite material；S4: sodium borohydride reduction chloroplatinic acid is utilized, to obtain graininess multicomponent sulfide-platinum heterojunction photocatalysis composite material.The preparation method can be used for photolysis water hydrogen field to obtain graininess multicomponent sulfide-platinum heterojunction photocatalysis composite material with excellent hydrogen manufacturing performance by the selection and combination of specific processing step and technological parameter.
Description
Technical field
The invention belongs to inorganic semiconductor material field and field of energy source materials, have specifically supplied semiconductor not of the same race mutual
More specifically a kind of graininess multicomponent sulphur is provided in conjunction with the preparation and purposes for forming heterojunction photocatalysis composite material
Compound-platinum heterojunction photocatalysis composite material preparation and production hydrogen application.
Background technique
Hydrogen Energy is just more and more being paid close attention to by people as a kind of ideal, environmental protection, cleaning, the reproducible energy.Institute
In some chemical energy sources, hydrogen has highest energy density, has reached 142MJ kg-1.Therefore, the following Hydrogen Energy is considered as most
The energy of promising alternative fossil resource, then developing clean, inexpensive technology promotes the release reaction of hydrogen then
It is most important.Currently, concern of the photochemical catalyzing by scientists, the semiconductor with special band structure is needed to be
Catalyst, reaction prepares hydrogen under light illumination.The design of semiconductor catalyst with special band structure prepares and building
Suitable catalystic converter system is the emphasis in photocatalysis hydrogen production field.
In inorganic semiconductor material field, CdS is a kind of typical semiconductor, and the band gap of CdS photochemical catalyst is 2.4eV, conduction band
Current potential (- 0.87eVvs THE) and the position valence band current potential (1.5eV) can satisfy the condition of complete photodegradation water.Therefore, CdS can
Become one of the semiconductor catalyst being concerned in sulfide systems to improve the utilization rate of sunlight.However, simple
There is different problems for catalyst: solar energy utilization ratio is low, photoetch phenomenon, hydrogen generation efficiency is low, stability is poor and excessively electric
The problems such as gesture is high.
The main method of modified CdS has: Morphological control, building hetero-junctions, load cocatalyst, addition sacrifice agent etc..Its
It is middle to improve the problem using load cocatalyst, semiconductor catalyst hydrogen production efficiency can be effectively improved.
CdS/MoS was introduced in CN103566953A and CN201610162861.92Composite material preparation and application,
Material has good photocatalysis efficiency.
MoS is described in CN201710411607.22/WS2The preparation of composite material, prepared MoS2/WS2Nanometer layer
Shape composite material can be applied to the fields such as lube oil additive, photoelectric material, hydrogen storage, photocatalysis.
It synthesizes there are many kinds of multicomponent sulfide-platinum heterojunction photocatalysis composite material methods, including chemical vapor deposition
Area method synthesis, solvent heat, hydro-thermal method etc., wherein chemical vapour deposition technique experiment condition is harsher, needs inert gas and high temperature
Environment, operation are not easy；Solvent heat and hydro-thermal method are reacted in reaction kettle, can not observe material synthesis processes and required time
Up to 10 hours, efficiency was lower.
Based on defect existing for above method, it is heterogeneous to design simple one kind, safety, quick multicomponent sulfide-platinum
Knot optic catalytic composite material preparation method seems particularly significant, especially there is potential application in photocatalytic hydrogen production by water decomposition
Value, this be also the present invention be accomplished basis where and power institute according to.
Summary of the invention
In the presence of overcoming synthesis multicomponent sulfide-platinum heterojunction photocatalysis composite material as indicated above
Many defects, provide it is a kind of simple, quickly, method cost-effective and environmentally friendly to prepare there is rule, the novel multiple groups of morphology controllable
Divide sulfide-platinum heterojunction composite method, and obtains the multicomponent sulfide-platinum with rule, morphology controllable
The composite material of hetero-junctions, and its application in photocatalysis field is studied, present inventor has performed in-depth studies, are paying
After a large amount of creative work, so as to complete the present invention.
Specifically, the present invention provides a kind of graininess multicomponent sulfide-platinum as the first aspect of the invention
Heterojunction photocatalysis composite material and preparation method thereof, the technical scheme comprises the following steps:
S1: it reacts to obtain sulfur-bearing molybdenum source and sulfur-bearing tungsten source using molybdenum salt, tungsten salt and Sodium Dimethyldithiocarbamate and dehydrated alcohol, the sulfur-bearing molybdenum
Source is dimethyl dithiocarbamic acid molybdenum, which is dimethyl dithiocarbamic acid tungsten；
S2: sulfur-bearing molybdenum source, sulfur-bearing tungsten source and cadmium source presoma being added in organic solvent, are sufficiently stirred, and are uniformly mixed,
Obtain forerunner's reaction solution；
S3: forerunner's reaction solution is subjected to a step liquid phase microwave assisting method rapid synthesis, obtains the more of nutty structure
Component sulfide composite material；
S4: by aforementioned three component material, oil bath is reacted in organic solvent with sodium borohydride, platinum acid chloride solution, is restored
Platinum be compound in the multicomponent sulfide composite material surface, obtain graininess multicomponent sulfide-platinum heterojunction photocatalysis
Composite material.
In multicomponent sulfide-platinum heterojunction photocatalysis composite material preparation side of the nutty structure of the invention
In method, in step sl, the dosage of the dehydrated alcohol is not particularly limited, and be may be, for example, and is easy to react and/or locate afterwards
The amount of reason, those skilled in the art suitably can be selected and be determined, this is no longer going to repeat them.
In multicomponent sulfide-platinum heterojunction photocatalysis composite material preparation side of the nutty structure of the invention
In method, in step sl, reaction temperature is room temperature.
Further setting is in the step S1, and molybdenum salt is molybdenum pentachloride, and the tungsten salt is tungsten hexachloride.
Further setting is in the step S2, and cadmium source presoma is cadmium diethyl dithiocarbamate, acetic acid
Any one in cadmium, dimethyl cadmium or any a variety of mixture.Most preferably cadmium diethyl dithiocarbamate
(CED)。
Further setting is that in step s 2, the organic solvent is C1-6Alcohol, C2-6Glycol, N,N-dimethylformamide,
Any one in dimethyl sulfoxide or N-Methyl pyrrolidone.Preferably C2-6Glycol, most preferably ethylene glycol.
In multicomponent sulfide-platinum heterojunction photocatalysis composite material preparation side of the nutty structure of the invention
In method, in step s 2, the dosage of the organic solvent is not particularly limited, and be may be, for example, and is easy to react and/or locate afterwards
The amount of reason, those skilled in the art suitably can be selected and be determined, this is no longer going to repeat them.
Further setting is that in step s 2, the mass ratio of cadmium source presoma, sulfur-bearing molybdenum source and sulfur-bearing tungsten source is 2:
1:2,5:3:2,2:1:1,5:2:3 or 2:2:1.Most preferably 2:1:1, wherein ethylene glycol is 500mL.
Further setting is that the step S3 is specific as follows:
S3-1: under the microwave power of ultrasonic agitation 200W, being arranged temperature-time program, step S2 is obtained described in
Forerunner's reaction solution is heated to 90 DEG C by room temperature, this process needs 3-5 minutes, and is kept for 10 minutes at such a temperature, obtains first
Reaction solution；
S3-2: first reaction solution being continued to heat, is warming up to 160-170 DEG C, and this process 3-5 minutes, and in the temperature
Degree is lower to be kept for 10 minutes, and the second reaction solution is obtained；
S3-3: being centrifuged 5 minutes by the second reaction solution cooled to room temperature, and with the centrifugal speed of 18000rpm,
Gained precipitating is successively washed 3-4 times with dehydrated alcohol, the multicomponent vulcanization to get the nutty structure is then dried in vacuo
Object composite material, i.e. CdS-MoS2-WS2。
Further setting is that the step S4 is specific as follows:
S4-1: being added above-mentioned multicomponent sulfide composite powder particle in ethylene glycol solvent, and stirring 10-15 divides
Clock obtains dispersion liquid；
S4-2: in above-mentioned dispersion liquid, will be added dropwise the platinum acid chloride solution after being configured, and stir 5-10 minutes；
S4-3: when oil bath heating is to 90 DEG C, shifting in above-mentioned dispersion liquid to oil bath pan, and sodium borohydride solution is added, stirs
It mixes, reacts 2 hours；
S4-4: by above-mentioned reaction solution cooled to room temperature, and with the centrifugal speed of 10000rpm centrifugation 6 minutes, by institute
It must precipitate and successively be washed 3-4 times with dehydrated alcohol, is then dried in vacuo heterogeneous to get the graininess multicomponent sulfide-platinum
Tie optic catalytic composite material, i.e. CdS-MoS2-WS2@Pt。
Further setting is that in step s 4, platiniferous quality and multicomponent sulfide are multiple in the platinum acid chloride solution of the addition
Condensation material powder quality ratio is 1w%-6w%, and most preferably 3w%, the concentration of sodium borohydride is 0.05g/50mL ethylene glycol, and
Holding system final volume is consistent.
Wherein, in step S4-3, platinum containing amount molar ratio is 5- in the platinum acid chloride solution of the sodium borohydride amount and addition
10, most preferably 10, the concentration of the sodium borohydride of configuration is most preferably 0.05g/50mL ethylene glycol, keeps system final volume one
It causes.
The second aspect of the invention, which provides, provides graininess multicomponent sulfide-platinum prepared by a kind of above method
Heterojunction photocatalysis composite material.
MoS2And WS2It is a kind of excellent co-catalyst, present inventor has found under study for action, two kinds of conducts simultaneously
When co-catalyst, synergistic effect can produce, enhance quantity of photogenerated charge separative efficiency.In addition, being loaded in semiconductor catalyst certain
The noble metal platinum of amount, what platinum play a part of is light induced electron receptor, and light induced electron can be by turning on the higher catalyst of fermi level
It moves on the lower noble metal platinum of fermi level, causes efficiently separating for electron-hole pair, enhance photocatalysis hydrolytic hydrogen production
Efficiency.Therefore, the application selection multicomponent sulfide-platinum heterojunction photocatalysis composite material is to improve photocatalysis hydrogen production performance
A kind of good approach.
The inventors discovered that the multiple groups of specific graininess appearance form can be obtained when using preparation method so
Divide sulfide-platinum heterojunction photocatalysis composite material, and when change certain technological parameters such as raw material dosage ratio, microwave function therein
Whens rate, constant temperature time etc., then the optic catalytic composite material of such form is unable to get.
The inventors discovered that the graininess multicomponent sulfide-platinum heterojunction photocatalysis composite material is with excellent
Photocatalysis performance has a good application prospect and industrialization potential so as to be applied to photolysis water hydrogen technical field.
The third aspect of the invention provides graininess multicomponent sulfide-platinum heterojunction photocatalysis composite material in light
Solve the application method of hydrogen manufacturing.
The method of the photodissociation hydrogen manufacturing includes: by the graininess multicomponent sulfide-platinum heterojunction photocatalysis composite wood
Material is added in the mixture of lactic acid and water composition, with xenon lamp Continuous irradiation, is filtered using 420nm optical filter below, photodissociation
Generate H2。
Further setting is the graininess multicomponent sulfide-platinum heterojunction photocatalysis composite material and lactic acid and water institute
The mass volume ratio of the mixture of composition is 1:1-3mg/ml.Wherein, in the photodissociation hydrogen production process, the volume of lactic acid and water
Than may be, for example, 1:8,1:9,1:10,1:11 or 1:12 for 1:8-12.
There is graininess multicomponent sulfide of the present invention-platinum heterojunction photocatalysis composite material excellent photocatalysis to analyse
Outside hydrogen efficiency, still there is efficient Hydrogen Evolution Performance after continuous reaction for a long time, there is high stability, be effectively improved photoetch bring
Problem.
Inventors have found that present invention graininess multicomponent sulfide-platinum heterojunction photocatalysis composite material obtained exists
Under illumination condition, hydrogen can be prepared by photodissociation in water, there is very excellent H2-producing capacity, and have high stable
Property, effectively improve the problem of photoetch causes.Completely new and efficient photodissociation composite material is provided for photodissociation hydrogen manufacturing, in industry
Field has huge application potential and industrial value.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention, for those of ordinary skill in the art, without any creative labor, according to
These attached drawings obtain other attached drawings and still fall within scope of the invention.
Fig. 1 is graininess multicomponent sulfide obtained by the embodiment of the present invention 1-platinum heterojunction photocatalysis composite material
Low power scanning electron microscope (SEM) photograph (SEM)；
Fig. 2 is graininess multicomponent sulfide obtained by the embodiment of the present invention 1-platinum heterojunction photocatalysis composite material
The high resolution transmission electron microscopy (i.e. Fig. 2 (c) and Fig. 2 (d)) of transmission electron microscope picture (TEM) and part；
Fig. 3 is graininess multicomponent sulfide obtained by the embodiment of the present invention 1-platinum heterojunction photocatalysis composite material
Energy spectrum diagram (EDS)；
Fig. 4 is graininess multicomponent sulfide obtained by the embodiment of the present invention 1-platinum heterojunction photocatalysis composite material
X-ray diffractogram (XRD)；
Fig. 5 be using different raw material dosages than when obtained different samples SEM scheme；
Fig. 6 is graininess multicomponent sulfide obtained by the embodiment of the present invention 1-platinum heterojunction photocatalysis composite material
X-ray photoelectron spectroscopy (XPS)；
Fig. 7 be graininess multicomponent sulfide-platinum heterojunction photocatalysis composite material obtained by the embodiment of the present invention 1 with
Irradiation time-hydrogen output the comparison of bright sulfur cadmium (CdS), two component sulfide, three component sulfide in photolysis water hydrogen is closed
System's figure；
Fig. 8 is graininess multicomponent sulfide obtained by the embodiment of the present invention 1-platinum heterojunction photocatalysis composite material
100 hours production stabilized hydrogen figures.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, the present invention is made into one below in conjunction with attached drawing
Step ground detailed description.
Embodiment 1
S1: the molybdenum chloride MoCl that mass ratio is 1:1.5 is dissolved in 200ml ethyl alcohol5And Sodium Dimethyldithiocarbamate, it is filled with magnetic stirring apparatus
Divide stirring, be uniformly mixed, stands 6h, filtering and washing, vacuum drying 12 hours, obtain sulfur-bearing molybdenum source, i.e., dimethyl disulfide is for ammonia
Base formic acid molybdenum Mo (dedc)5.Same procedure obtains sulfur-bearing tungsten source i.e. dimethyl dithiocarbamic acid W (dedc)6；
S2: cadmium source, molybdenum source, tungsten source are added in organic solvent ethylene glycol according to mass ratio for 2:1:1, stirred using magnetic force
It mixes and stirs ultrasonic cleaning machine to be sufficiently stirred, this process needs 40-50 minutes, is uniformly mixed, obtains forerunner's reaction solution；
S3: forerunner's reaction solution is subjected to a step liquid phase microwave assisting method rapid synthesis, before obtaining multicomponent sulfide
Body material is driven, specific steps are seen below:
S3-1: under the microwave power of ultrasonic agitation 200W, being arranged temperature-time program, step S2 is obtained described in
Forerunner's reaction solution is heated to 90 DEG C by room temperature, this process needs 5 minutes, and is kept for 10 minutes at such a temperature, and it is anti-to obtain first
Answer liquid；
S3-2: first reaction solution being continued to heat, is warming up to 160 DEG C, this process needs 5 minutes, and in the temperature
It is lower to be kept for 10 minutes, obtain the second reaction solution；
S3-3: being centrifuged 5 minutes by the second reaction solution cooled to room temperature, and with the centrifugal speed of 18000rpm,
Gained precipitating is successively washed 3-4 times with dehydrated alcohol, the multicomponent vulcanization to get the nutty structure is then dried in vacuo
Presoma, that is, CdS-MoS of object composite material2-WS2, it is denoted as Cd-Mo-W (2:1:1).
S4: utilizing sodium borohydride reduction chloroplatinic acid, so that it is multiple to obtain graininess multicomponent sulfide-platinum heterojunction photocatalysis
Condensation material, specific steps are seen below:
S4-1: being added above-mentioned 100 grams of multicomponent sulfide composite powder particle in 40.205mL ethylene glycol solvent,
Stirring 10 minutes, obtains dispersion liquid；
S4-2: in above-mentioned dispersion liquid, will be added dropwise the 3.8616mmol/L platinum acid chloride solution 3.981mL after being configured,
Stirring 5 minutes；
S4-3: when oil bath heating is to 90 DEG C, shifting in above-mentioned dispersion liquid to oil bath pan, and it is 0.05g/ that concentration, which is added dropwise,
The sodium borohydride solution 5.81mL of 50mL ethylene glycol, stirring are reacted 2 hours；
S4-4: by above-mentioned reaction solution cooled to room temperature, and with the centrifugal speed of 10000rpm centrifugation 6 minutes, by institute
It must precipitate and successively be washed 3-4 times with dehydrated alcohol, is then dried in vacuo heterogeneous to get the graininess multicomponent sulfide-platinum
Tie optic catalytic composite material, that is, CdS-MoS2-WS2@Pt is denoted as Cd-Mo-W@Pt (3w%).
The investigation of embodiment 2-8 raw material dosage ratio
Except cadmium diethyl dithiocarbamate (CED), the dimethyl for using different quality ratio shown in the following table 1 in step S3
Molybdenum dithiocarbamate Mo (dedc)5, tungsten source, that is, dimethyl dithiocarbamic acid W (dedc)6, other operations are homogeneously same as
Embodiment 1, to be carried out a 2-8, used raw material dosage ratio and composite material name see the table below 1.
Composite material obtained under 1. different material amount ratio of table
Embodiment 9-13: not same amount Pt load is investigated
Embodiment 9-13: in addition to using Pt load capacity shown in the following table 2 in step S4-1, other operations homogeneously are same as implementing
Example 1, to be carried out a 9-13.
It is specifically shown in the following table 2.
Same amount Pt does not load lower composite material obtained to table 2.Cd-Mo-W (2:1:1)
Microscopic sdIBM-2+2q.p.approach
To the resulting graininess multicomponent sulfide of embodiment 1-platinum heterojunction photocatalysis composite material carried out it is multiple not
It is as a result as follows with the microscopic sdIBM-2+2q.p.approach of means:
1, by the low power scanning electron microscope (SEM) photograph (SEM) of Fig. 1 as it can be seen that multicomponent sulfide-platinum heterojunction photocatalysis is compound
Material morphology is uniform, and for the different knot matter of graininess with raised thorn-like, the particle diameter of the different knot matter of these graininess is 250-
300nm。
2, by the transmission electron microscope picture (b) of Fig. 2 (TEM) as it can be seen that the sample shape observed on the sample topography and SEM observed
Looks profile is consistent, there is graininess hetero-junctions in figure, and graininess topographical surface is relatively rough, observable discovery, and the graininess is compound
Material is accumulated by the little particle of tens nano-scales, and particle surface is with protrusion.
Fig. 2 (c), Fig. 2 (d) are the high resolution transmission electron microscopy picture of circle and Blocked portion in Fig. 2 (b) respectively.
It can be seen that gem-pure lattice fringe, by measurement, the width of lattice fringe is respectively 0.39nm from Fig. 2 (c),
0.22nm, respectively with hexagonal phase CdS (100), Pt (111) crystal face is corresponding.
It can be seen that gem-pure lattice fringe, by measurement, the width of lattice fringe is respectively in Fig. 2 (d)
0.30nm, 0.27nm, respectively with MoS2(006), WS2(101) crystal face is corresponding.
3, shown by Fig. 3 power spectrum (EDS) test: containing five kinds of elements of Cd, Mo, W, S, Pt in sample, illustrating of preparation
Granular multicomponent sulfide-platinum heterojunction photocatalysis composite material contains five kinds of elements of Cd, Mo, W, S, Pt.
4, by the X-ray diffractogram of Fig. 4 (XRD) as it can be seen that there are CdS characteristic main peaks, in different materials, peak-to-peak signal changes
Unobvious, remaining ingredient does not occur apparent peak-to-peak signal in figure, this is because content is too low or exists in the form of indefinite form.
5, by low power scanning electron microscope (SEM) photograph (SEM) comparison diagram of Fig. 5 as it can be seen that the multicomponent sulfide forerunner that different proportion forms
Body is both topographically distinguished less.
6, by the x-ray photoelectron spectroscopy of Fig. 6 (XPS) figure as it can be seen that cadmium exists in the form of cadmium sulfide (CdS), molybdenum is with sulphur
Change molybdenum (MoS2) form presence, tungsten is with tungsten sulfide (WS2) form exists, platinum (Pt) in the form of simple substance platinum exists, and demonstrates multiple groups
Divide sulfide-platinum heterojunction photocatalysis composite material existence form.
Therefore, in summary material characterization, it is known that the present invention has successfully synthesized particle by specific preparation method
Shape multicomponent sulfide-platinum heterojunction photocatalysis composite material, i.e. CdS-MoS2-WS2@Pt。
7, Fig. 7 is graininess multicomponent sulfide obtained by the embodiment of the present invention 1-platinum heterojunction photocatalysis composite material
Three component sulfide under negative from bright sulfur cadmium (CdS), two component sulfide, three component sulfide and different platinum are in photocatalytic water
Irradiation time-hydrogen output relativity figure in hydrogen manufacturing.
As can be seen from the figure the photocatalysis hydrogen production performance of bright sulfur cadmium is most weak, and photodegradation water hydrogen-producing speed is
0.08mmol/g*h, and the graininess multicomponent sulfide of the embodiment of the present invention 1-platinum heterojunction photocatalysis composite material (CdS-
MoS2-WS2@Pt, mass ratio: 2:1:1-3w%) there is best H2-producing capacity: photodegradation water hydrogen-producing speed is 27.89mmol/
G*h, this is higher by about 348 times than pure CdS hydrogen-producing speed, and is much higher than two component sulfide, three component sulfide and difference
Three component sulfide under platinum load.
8, Fig. 8 is graininess multicomponent sulfide obtained by the embodiment of the present invention 1-platinum heterojunction photocatalysis composite material
The continuous performance for stability figure for producing hydrogen 100 hours.
The production stabilized hydrogen of the material is good as can be seen from Figure, and after continuous illumination is reacted 100 hours, H2-producing capacity is still
It is maintained at higher value, and does not occur the trend being decreased obviously.
To demonstrate graininess multicomponent sulfide-platinum heterojunction photocatalysis composite material of the invention with excellent
Photodissociation catalyzing manufacturing of hydrogen performance can be applied to photodissociation hydrogen producing technology field.
The characterization of composite material obtained by other embodiments
1, the material SEM characterization discovery to obtaining under example 2- example 8, the pattern of material is all graininess, but pattern is advised
Then property is less than the material under example 1.
Thus demonstrate in step s3, cadmium source, molybdenum source, tungsten source material quality than be most preferably 2:1:1.
2, the material SEM characterization discovery to obtaining under example 9- example 13, the pattern of material is not much different, but morphological rules
Property is less than the material under example 1.
Thus it demonstrates at step S4, the load capacity of platinum is most preferably the 3w% of presoma gross mass.
Photolysis water hydrogen performance test
1, the resulting graininess multicomponent sulfide of embodiment 1-platinum heterojunction photocatalysis composite material is used for photocatalytic water
Hydrogen manufacturing, specific processing method are as follows:
35mg sample is added in the mixture of 8ml lactic acid and 72ml water composition, is irradiated with solar simulator, used
420nm optical filter below filtering, and with the H of gas chromatographic detection output2。
When sample used is respectively graininess multicomponent sulfide-platinum heterojunction photocatalysis made from the embodiment of the present invention 1
Three components vulcanization under composite material, bright sulfur cadmium (CdS), two component sulfide, three component sulfide and different platinum loads
When object, the relationship between irradiation time and hydrogen output is shown in attached drawing 5.The photocatalysis hydrogen production performance of pure CdS as can be seen from the figure
Most weak, hydrogen-producing speed is only 0.08mmol/g*h, and graininess multicomponent sulfide-platinum hetero-junctions of the embodiment of the present invention 1
Optic catalytic composite material has best H2-producing capacity: hydrogen-producing speed 27.89mmol/g*h, this is than pure CdS hydrogen-producing speed
(0.08mmol/g*h) is higher by about 348 times, even more much higher than under two component sulfide, three component sulfide and different platinum loads
Three component sulfide.
Thus graininess multicomponent sulfide of the present invention-platinum heterojunction photocatalysis composite material is demonstrated with excellent
Photolysis water hydrogen performance, can be used for photolysis water hydrogen field.
2, according to photolysis water hydrogen method same as described above, example 2- example 13 is tested, it is specific to produce hydrogen effect
Rate see the table below, for the ease of comparing, will the hydrogen generation efficiency of Cd-Mo-W (2:1:1)@Pt3w% of embodiment 1 list together.
It can be seen that although the material morphology under example 2- example 8 is still graininess, for the more of different proportion ingredient
Component sulphur compound presoma, Cd-Mo-W (2:1:1) presoma H2-producing capacity under example 1 are better than more under other ratios
Component sulfide presoma；In addition, it is smaller on the influence of the pattern of material for platinum different amounts of under example 9- example 13 load, but
Its photodissociation hydrogen manufacturing performance is but markedly less than the material of example 1.
In conclusion the preparation method of the invention it can be seen from above-mentioned all embodiments passes through specific technique
The synergistic combination and coordinative role of step and technological parameter etc., to obtain multicomponent sulfide-platinum with unique morphology
Heterojunction photocatalysis composite material, and it is with good photolysis water hydrogen performance.
The above disclosure is only the preferred embodiments of the present invention, cannot limit the right model of the present invention with this certainly
It encloses, therefore equivalent changes made in accordance with the claims of the present invention, is still within the scope of the present invention.
Claims (10)
1. a kind of graininess multicomponent sulfide-platinum heterojunction photocatalysis composite material and preparation method thereof, it is characterised in that including with
Lower step:
S1: reacting to obtain sulfur-bearing molybdenum source and sulfur-bearing tungsten source using molybdenum salt, tungsten salt and Sodium Dimethyldithiocarbamate and dehydrated alcohol, which is
Dimethyl dithiocarbamic acid molybdenum, the sulfur-bearing tungsten source are dimethyl dithiocarbamic acid tungsten；
S2: sulfur-bearing molybdenum source, sulfur-bearing tungsten source and cadmium source presoma being added in organic solvent, are sufficiently stirred, and are uniformly mixed, are obtained
Forerunner's reaction solution；
S3: forerunner's reaction solution is subjected to a step liquid phase microwave assisting method rapid synthesis, obtains the multicomponent of nutty structure
Sulfide composite material；
S4: by aforementioned three component material, oil bath is reacted in organic solvent with sodium borohydride, platinum acid chloride solution, the platinum restored
It is compound in the multicomponent sulfide composite material surface, it is compound to obtain graininess multicomponent sulfide-platinum heterojunction photocatalysis
Material.
2. a kind of graininess multicomponent sulfide according to claim 1-platinum heterojunction photocatalysis composite material preparation side
Method, it is characterised in that: in the step S1, molybdenum salt is molybdenum pentachloride, and the tungsten salt is tungsten hexachloride.
3. a kind of graininess multicomponent sulfide according to claim 1-platinum heterojunction photocatalysis composite material preparation side
Method, it is characterised in that: in the step S2, cadmium source presoma is cadmium diethyl dithiocarbamate, cadmium acetate, diformazan
Any one in base cadmium or any a variety of mixture.
4. a kind of graininess multicomponent sulfide according to claim 1-platinum heterojunction photocatalysis composite material preparation side
Method, it is characterised in that: in step s 2, the organic solvent is C1-6Alcohol, C2-6Glycol, N,N-dimethylformamide, dimethyl
Any one in sulfoxide or N-Methyl pyrrolidone.
5. a kind of graininess multicomponent sulfide according to claim 1-platinum heterojunction photocatalysis composite material preparation side
Method, it is characterised in that: in step s 2, the mass ratio of cadmium source presoma, sulfur-bearing molybdenum source and sulfur-bearing tungsten source is 2:1:2,5:
3:2,2:1:1,5:2:3 or 2:2:1.
6. a kind of graininess multicomponent sulfide according to claim 1-platinum heterojunction photocatalysis composite material preparation side
Method, it is characterised in that: the step S3 is specific as follows:
S3-1: under the microwave power of ultrasonic agitation 200W, temperature-time program is set, by step
Forerunner's reaction solution that S2 is obtained is heated to 90 DEG C by room temperature, this process needs 3-5 minutes, and keeps at such a temperature
10 minutes, obtain the first reaction solution；
S3-2: first reaction solution being continued to heat, is warming up to 160-170 DEG C, and this process 3-5 minutes, and at such a temperature
It is kept for 10 minutes, obtains the second reaction solution；
S3-3: by the second reaction solution cooled to room temperature, and with the centrifugal speed of 18000rpm centrifugation 5 minutes, by institute
It must precipitate and successively be washed 3-4 times with dehydrated alcohol, is then dried in vacuo multiple to get the multicomponent sulfide of the nutty structure
Condensation material, i.e. CdS-MoS2-WS2。
7. a kind of graininess multicomponent sulfide according to claim 1-platinum heterojunction photocatalysis composite material preparation side
Method, it is characterised in that the step S4 is specific as follows:
S4-1: being added above-mentioned multicomponent sulfide composite powder particle in ethylene glycol solvent, stirs 10-15 minutes, obtains
To dispersion liquid；
S4-2: in above-mentioned dispersion liquid, will be added dropwise the platinum acid chloride solution after being configured, and stir 5-10 minutes；
S4-3: when oil bath heating is to 90 DEG C, shifting in above-mentioned dispersion liquid to oil bath pan, is added sodium borohydride solution, stirring, instead
It answers 2 hours；
S4-4: by above-mentioned reaction solution cooled to room temperature, and with the centrifugal speed of 10000rpm centrifugation 6 minutes, gained is sunk
Shallow lake is successively washed 3-4 times with dehydrated alcohol, is then dried in vacuo to get the graininess multicomponent sulfide-platinum hetero-junctions light
Catalytic composite materials, i.e. CdS-MoS2-WS2@Pt。
8. a kind of graininess multicomponent sulfide according to claim 1-platinum heterojunction photocatalysis composite material preparation side
Method, it is characterised in that in step s 4, platiniferous quality and multicomponent sulfide composite material in the platinum acid chloride solution of the addition
Powder quality ratio is 1w%-6w%, and the concentration of sodium borohydride is 0.05g/50mL ethylene glycol, and keeps system final volume consistent.
9. graininess prepared by a kind of preparation method as described in one of claim 1-8 and the multiple groups for having photolysis water hydrogen purposes
Divide sulfide-platinum heterojunction photocatalysis composite material.
10. a kind of method of photodissociation hydrogen manufacturing, it is characterised in that: graininess multicomponent sulfide-platinum as claimed in claim 9 is different
Matter knot optic catalytic composite material is added in the mixture of lactic acid and water composition, with mixture composed by lactic acid and water
Mass volume ratio is 1:1-3mg/ml, with xenon lamp Continuous irradiation, is filtered using 420nm optical filter below, photodissociation generates H2。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811245436.1A CN109331843A (en) | 2018-10-24 | 2018-10-24 | Graininess multicomponent sulfide-platinum heterojunction photocatalysis composite material and preparation method thereof and its production hydrogen application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811245436.1A CN109331843A (en) | 2018-10-24 | 2018-10-24 | Graininess multicomponent sulfide-platinum heterojunction photocatalysis composite material and preparation method thereof and its production hydrogen application |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109331843A true CN109331843A (en) | 2019-02-15 |
Family
ID=65311610
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811245436.1A Pending CN109331843A (en) | 2018-10-24 | 2018-10-24 | Graininess multicomponent sulfide-platinum heterojunction photocatalysis composite material and preparation method thereof and its production hydrogen application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109331843A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113019413A (en) * | 2021-03-11 | 2021-06-25 | 王岩 | M/GaN/FTO catalyst and preparation method thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103055900A (en) * | 2013-01-28 | 2013-04-24 | 上海电力学院 | Pt/CdS composite visible-light-induced photocatalyst and preparation method thereof |
| CN103990472A (en) * | 2014-06-09 | 2014-08-20 | 中国科学技术大学 | Stable and efficient hydrogen production co-catalyst and preparation method thereof |
| CN104923264A (en) * | 2015-05-28 | 2015-09-23 | 淮北师范大学 | Preparation method and application of precious metal-modified CdS nanorod photocatalyst |
| CN105618098A (en) * | 2016-01-13 | 2016-06-01 | 西安交通大学 | Platinum supported nitrogen-doped molybdenum disulfide photocatalyst and preparation method thereof |
| CN106964369A (en) * | 2017-03-21 | 2017-07-21 | 温州大学 | A kind of preparation method and application of heterojunction photocatalyst |
| CN107670676A (en) * | 2017-10-13 | 2018-02-09 | 温州大学新材料与产业技术研究院 | The preparation method and applications of the cadmium sulfide molybdenum sulfide tungsten sulfide heterojunction photocatalysis composite of one species sea urchin shape structure |
| CN107983272A (en) * | 2016-10-26 | 2018-05-04 | 中国科学院化学研究所 | Sulfide encapsulated particles and preparation method and application |
| CN108246316A (en) * | 2018-03-16 | 2018-07-06 | 中国科学技术大学先进技术研究院 | A kind of Pt/MoS2Nanocatalyst and its preparation method and application |
-
2018
- 2018-10-24 CN CN201811245436.1A patent/CN109331843A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103055900A (en) * | 2013-01-28 | 2013-04-24 | 上海电力学院 | Pt/CdS composite visible-light-induced photocatalyst and preparation method thereof |
| CN103990472A (en) * | 2014-06-09 | 2014-08-20 | 中国科学技术大学 | Stable and efficient hydrogen production co-catalyst and preparation method thereof |
| CN104923264A (en) * | 2015-05-28 | 2015-09-23 | 淮北师范大学 | Preparation method and application of precious metal-modified CdS nanorod photocatalyst |
| CN105618098A (en) * | 2016-01-13 | 2016-06-01 | 西安交通大学 | Platinum supported nitrogen-doped molybdenum disulfide photocatalyst and preparation method thereof |
| CN107983272A (en) * | 2016-10-26 | 2018-05-04 | 中国科学院化学研究所 | Sulfide encapsulated particles and preparation method and application |
| CN106964369A (en) * | 2017-03-21 | 2017-07-21 | 温州大学 | A kind of preparation method and application of heterojunction photocatalyst |
| CN107670676A (en) * | 2017-10-13 | 2018-02-09 | 温州大学新材料与产业技术研究院 | The preparation method and applications of the cadmium sulfide molybdenum sulfide tungsten sulfide heterojunction photocatalysis composite of one species sea urchin shape structure |
| CN108246316A (en) * | 2018-03-16 | 2018-07-06 | 中国科学技术大学先进技术研究院 | A kind of Pt/MoS2Nanocatalyst and its preparation method and application |
Non-Patent Citations (1)
| Title |
|---|
| JIAN JIN ET AL.: "Single crystal CdS nanowires with high visible-light", 《JOURNAL OF MATERIALS CHEMISTRY A》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113019413A (en) * | 2021-03-11 | 2021-06-25 | 王岩 | M/GaN/FTO catalyst and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Meng et al. | Metal-organic framework as nanoreactors to co-incorporate carbon nanodots and CdS quantum dots into the pores for improved H2 evolution without noble-metal cocatalyst | |
| Shi et al. | Onion-ring-like g-C3N4 modified with Bi3TaO7 quantum dots: A novel 0D/3D S-scheme heterojunction for enhanced photocatalytic hydrogen production under visible light irradiation | |
| Wang et al. | Sb2WO6/BiOBr 2D nanocomposite S-scheme photocatalyst for NO removal | |
| Xing et al. | Mo‐doped ZnIn2S4 flower‐like hollow microspheres for improved visible light‐driven hydrogen evolution | |
| Shi et al. | Implantation of Iron (III) in porphyrinic metal organic frameworks for highly improved photocatalytic performance | |
| CN110918126B (en) | Preparation method of flower-shaped molybdenum disulfide combined UiO-66 photocatalyst | |
| Lu et al. | In situ fabrication of BiVO4-CeVO4 heterojunction for excellent visible light photocatalytic degradation of levofloxacin | |
| Wang et al. | Quasi-Polymeric Metal-Organic Framework UiO-66/gC 3 N 4 Heterojunctions for Enhanced Photocatalytic Hydrogen Evolution under Visible Light Irradiation. | |
| Zhang et al. | Construction of Pt-decorated g-C3N4/Bi2WO6 Z-scheme composite with superior solar photocatalytic activity toward rhodamine B degradation | |
| Bai et al. | CQDs decorated oxygen vacancy-rich CeO2/BiOCl heterojunctions for promoted visible light photoactivity towards chromium (Ⅵ) reduction and rhodamine B degradation | |
| CN105722592B (en) | Combination transition metal for efficient liberation of hydrogen promotes light-catalysed system | |
| CN110882705B (en) | Microwave synthesis oxygen vacancy BiOCl/Bi 2 S 3 Catalyst and preparation method and application thereof | |
| Wu et al. | Controllable synthesis of Ag/AgCl@ MIL-88A via in situ growth method for morphology-dependent photocatalytic performance | |
| Gao et al. | Construction of heterostructured g-C3N4@ TiATA/Pt composites for efficacious photocatalytic hydrogen evolution | |
| Sun et al. | Dye degradation activity and stability of perovskite-type LaCoO3− x (x= 0∼ 0.075) | |
| CN113751029B (en) | Co (cobalt) 9 S 8 /ZnIn 2 S 4 Photocatalytic hydrogen production material and preparation method and application thereof | |
| CN109622035A (en) | The preparation method and application of RGO-MIL-68 (Fe) nano-complex | |
| CN107670676A (en) | The preparation method and applications of the cadmium sulfide molybdenum sulfide tungsten sulfide heterojunction photocatalysis composite of one species sea urchin shape structure | |
| Ma et al. | New UiO-66/CuxS heterostructures: surface functionalization synthesis and their application in photocatalytic degradation of RhB | |
| Gao et al. | Synthesis of a reticular porous MoS 2/gC 3 N 4 heterojunction with enhanced visible light efficiency in photocatalytic degradation of RhB | |
| Sun et al. | Nitrogen-doped carbon supported ZnO as highly stable heterogeneous catalysts for transesterification synthesis of ethyl methyl carbonate | |
| CN108816254A (en) | A kind of BiOI catalysis material and its preparation method and application | |
| Ding et al. | Nano‐SH‐MOF@ Self‐Assembling Hollow Spherical g‐C3N4 Heterojunction for Visible‐Light Photocatalytic Nitrogen Fixation | |
| Ding et al. | Ultrathin defective nanosheet subunit ZnIn2S4 hollow nanoflowers for efficient photocatalytic hydrogen evolution | |
| Wu et al. | Synthesis of a novel ternary BiOBr/g-C3N4/Ti3C2Tx hybrid for effectively removing tetracycline hydrochloride and rhodamine B |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190215 |
|
| RJ01 | Rejection of invention patent application after publication |