CN107126964B - A kind of preparation method and application of regular octahedron cadmium sulfide - Google Patents
A kind of preparation method and application of regular octahedron cadmium sulfide Download PDFInfo
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- CN107126964B CN107126964B CN201710269000.5A CN201710269000A CN107126964B CN 107126964 B CN107126964 B CN 107126964B CN 201710269000 A CN201710269000 A CN 201710269000A CN 107126964 B CN107126964 B CN 107126964B
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- cadmium
- regular octahedron
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- sulfide
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- 229910052980 cadmium sulfide Inorganic materials 0.000 title claims abstract description 59
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 239000001257 hydrogen Substances 0.000 claims abstract description 52
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 230000001699 photocatalysis Effects 0.000 claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 238000007146 photocatalysis Methods 0.000 claims abstract description 13
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 5
- 230000009467 reduction Effects 0.000 claims abstract description 4
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 3
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 3
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 3
- 239000005416 organic matter Substances 0.000 claims abstract description 3
- 230000003647 oxidation Effects 0.000 claims abstract description 3
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 47
- WZRRRFSJFQTGGB-UHFFFAOYSA-N 1,3,5-triazinane-2,4,6-trithione Chemical compound S=C1NC(=S)NC(=S)N1 WZRRRFSJFQTGGB-UHFFFAOYSA-N 0.000 claims description 33
- 238000006303 photolysis reaction Methods 0.000 claims description 23
- 239000008367 deionised water Substances 0.000 claims description 19
- 229910021641 deionized water Inorganic materials 0.000 claims description 19
- HUKFCVYEXPZJJZ-UHFFFAOYSA-N cadmium;hydrate Chemical compound O.[Cd] HUKFCVYEXPZJJZ-UHFFFAOYSA-N 0.000 claims description 18
- 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 14
- 229910052708 sodium Inorganic materials 0.000 claims description 14
- 239000011734 sodium Substances 0.000 claims description 14
- 239000013256 coordination polymer Substances 0.000 claims description 13
- 150000001661 cadmium Chemical class 0.000 claims description 10
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 7
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims description 7
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 6
- 229910052700 potassium Inorganic materials 0.000 claims description 6
- 239000011591 potassium Substances 0.000 claims description 6
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 229920001021 polysulfide Polymers 0.000 claims description 2
- 239000005077 polysulfide Substances 0.000 claims description 2
- 150000008117 polysulfides Polymers 0.000 claims description 2
- GARZCVGWIICURO-UHFFFAOYSA-N [Na].[Na].[Na].N#CO Chemical compound [Na].[Na].[Na].N#CO GARZCVGWIICURO-UHFFFAOYSA-N 0.000 claims 1
- 229910002090 carbon oxide Inorganic materials 0.000 claims 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims 1
- 230000015843 photosynthesis, light reaction Effects 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 55
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 49
- 238000000034 method Methods 0.000 abstract description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 4
- 231100001261 hazardous Toxicity 0.000 abstract description 3
- 231100000614 poison Toxicity 0.000 abstract description 3
- 230000007096 poisonous effect Effects 0.000 abstract description 3
- 239000004094 surface-active agent Substances 0.000 abstract description 3
- 239000001569 carbon dioxide Substances 0.000 abstract description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 2
- 238000006140 methanolysis reaction Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000000843 powder Substances 0.000 description 25
- 239000003643 water by type Substances 0.000 description 21
- 238000005286 illumination Methods 0.000 description 18
- 238000011156 evaluation Methods 0.000 description 17
- 238000007796 conventional method Methods 0.000 description 14
- 238000005406 washing Methods 0.000 description 14
- 238000000634 powder X-ray diffraction Methods 0.000 description 12
- 239000011541 reaction mixture Substances 0.000 description 10
- 229920001795 coordination polymer Polymers 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 238000005119 centrifugation Methods 0.000 description 7
- 229960000935 dehydrated alcohol Drugs 0.000 description 7
- 238000010218 electron microscopic analysis Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 238000005507 spraying Methods 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- SOBHUZYZLFQYFK-UHFFFAOYSA-K trisodium;hydroxy-[[phosphonatomethyl(phosphonomethyl)amino]methyl]phosphinate Chemical compound [Na+].[Na+].[Na+].OP(O)(=O)CN(CP(O)([O-])=O)CP([O-])([O-])=O SOBHUZYZLFQYFK-UHFFFAOYSA-K 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 239000005864 Sulphur Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 description 4
- AJVCUHHHRPBRHU-UHFFFAOYSA-N cadmium nitric acid Chemical compound [Cd].[N+](=O)(O)[O-] AJVCUHHHRPBRHU-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 150000007513 acids Chemical class 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- DPLVEEXVKBWGHE-UHFFFAOYSA-N potassium sulfide Chemical compound [S-2].[K+].[K+] DPLVEEXVKBWGHE-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 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 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 description 1
- GATXPHDUDVSRCV-UHFFFAOYSA-N [Cl].[Cd] Chemical compound [Cl].[Cd] GATXPHDUDVSRCV-UHFFFAOYSA-N 0.000 description 1
- PQLVXDKIJBQVDF-UHFFFAOYSA-N acetic acid;hydrate Chemical compound O.CC(O)=O PQLVXDKIJBQVDF-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- -1 cyanic acid tripotassium Chemical compound 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 238000003466 welding 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
-
- B01J35/39—
-
- 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
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G11/00—Compounds of cadmium
- C01G11/02—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/15—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of oxides of carbon exclusively
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
-
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Abstract
The invention discloses a kind of preparation method and applications of regular octahedron cadmium sulfide.The features such as preparation method provided by the invention has raw material cheap, simple process, organic solvent-free and surfactant, and no poisonous and hazardous organic intermediate generates, the morphology controllable of target product.The invention further relates to the application of the regular octahedron cadmium sulfide as photochemical catalyst, obtained regular octahedron cadmium sulfide can be prepared in the reaction such as the organic matters such as methanol and photocatalysis to selectively oxidation of hydrocarbons as photochemical catalyst used in the hydrogen manufacturing of visible light solution water, photocatalytically degradating organic dye, photocatalysis Decomposition organic matter, photocatalysis carbon dioxide reduction.The catalyst has good stability, and continuous use still maintains higher photocatalytic activity in 100 hours.
Description
[technical field]
The present invention relates to the preparation and application technical fields of catalysis material sulfide, relate in particular to a kind of positive octahedral
The preparation method and application of body cadmium sulfide.
[background technique]
Hydrogen (H2) it is a kind of important basic industries industrial chemicals, in industry synthetic ammonia, industrial salt manufacturing acid, glass mill
The fields such as light, gasoline refinery practice, gold welding, meteorological balloon detection and food industry are all widely used.In addition to this,
Hydrogen or a kind of new energy have many advantages, such as high combustion heat value, high combustion efficiency and combustion product cleaning, are generally considered
The most possible clean energy resource for replacing fossil energy.Therefore, the exploitation of hydrogen is that current chemical industry and energy field technology develop
Emphasis.
Currently, industrially using the methods of Coal Gasification hydrogen manufacturing, heavy oil and the conversion of gas water steam catalytic hydrogen manufacturing, so
And these methods not only inefficiency, and need to expend a large amount of fossil energy.Utilize inexhaustible cleaning
Solar energy, water decomposition is generated by hydrogen by Photocatalitic Technique of Semiconductor, effectively will solve energy crisis and environment simultaneously
Two large problems are polluted, therefore photodissociation aquatic products hydrogen technology has apparent superiority, reaction schematic diagram is as shown in Fig. 1.
Currently, a variety of different catalyst have been widely used in the reaction of photodissociation aquatic products hydrogen.In these catalysis materials,
The features such as cadmium sulfide is abundant because of direct transition type band structure, luminous color, in solar energy conversion, photoelectron chemical cell, non-
Linear optics and photocatalysis etc. all have extensive and far-reaching application prospect.
During conductor photocatalysis decomposes aquatic products hydrogen, the absorption of light and the body of charge are mutually separated and opposite from body
The rate of surface transfer is to determine the key factor of hydrogen generation efficiency, since the light-catalyzed reaction of light induced electron reduction adsorption water is hair
Life is on the surface of catalyst, and therefore, high specific surface area is conducive to the raising of hydrogen generation efficiency.By change cadmium sulfide pattern,
Size, specific surface area etc. can effectively increase contact area and tightness degree between CdS semiconduct and water.With conventional side
The cadmium sulfide that method prepares typically exhibits random graininess, therefore its specific surface area is typically small, so as to cause catalyst
Contact area between reactant is smaller, and reaction active site is less.In recent years, researchers develop the sulphur of different-shape
Cadmium, including quantum dot (zero dimension), the one-dimensional pattern such as nanometer rods, nano wire, nanotube and nanobelt, two-dimensional structure cadmium sulfide are received
Rice piece and spherical grade three-dimensional appearances.
Three-dimensional structure often has the specific surface area bigger than low dimensional structures material and more Adsorptions, this knot
Structure can not only enhance the absorption of light, while also greatly facilitate the separation of surface carrier and the transmission of interface carrier, very
The photocatalytic activity of cadmium sulfide is improved in big degree.However, the research in relation to special three-dimensional appearance cadmium sulfide is less, these are synthesized
The method of special appearance cadmium sulfide usually requires to introduce organic solvent, surfactant, organic structure directing agent etc., due to
The introducing of these organic matters not only increases the difficulty of last handling process and the pollution to environment, while in material synthesis processes
Organic intermediates more poisonous and hazardous than these organic matters can more likely be generated.Therefore, exploitation at room temperature, organic solvent-free
Under the conditions of prepare three-dimensional bigger serface cadmium sulfide new method, for expanding cadmium sulfide in photocatalysis and photoelectric field
Using having a very important significance.
[summary of the invention]
The object of the present invention is to provide the preparation methods and application of a kind of regular octahedron cadmium sulfide, and by the material application
It is reacted in photodissociation aquatic products hydrogen.The catalyst preparation is simple and easy to do, activity and stability with higher.
Regular octahedron cadmium sulfide catalyst provided by the invention is synthesized using two step of ion exchange.
To reach above-mentioned purpose, the present invention prepares regular octahedron cadmium sulfide photochemical catalyst using two-step method, i.e., prepared by (S1)
Regular octahedron Cd3(C3N3S3)2Presoma；(S2) regular octahedron cadmium sulfide photochemical catalyst is prepared.
It is as follows that this law invention prepares the step of regular octahedron cadmium sulfide photochemical catalyst:
S1, it takes cadmium salt to be dissolved in deionized water, obtains cadmium salt soln；Take trithiocyanuric acid and/or cyclo-trithocyanates
It is dissolved in deionized water, obtains clear solution；Cadmium salt soln is added dropwise at room temperature to clear solution, stirs, centrifuge separation is washed
It washs, obtains regular octahedron Cd3(C3N3S3)2Coordination polymer；
S2, by regular octahedron Cd obtained above3(C3N3S3)2Coordination polymer is scattered in deionized water, and stirring is lower to be added
Enter water-soluble sulfide, continue to stir, be centrifugated, washs, it is dry, obtain regular octahedron cadmium sulfide.
Preferably, in step sl, the cadmium salt is at least one in caddy, four water cadmium nitrates or two water cadmium acetates
Kind.
Preferably, in step sl, in step sl, the cyclo-trithocyanates are trithiocyanuric acid trisodium and/or three
Polysulfide cyanic acid tripotassium.
Preferably, in step sl, the molar ratio of the cadmium salt and trithiocyanuric acid and/or cyclo-trithocyanates is 1:
[0.5-2]。
Preferably, in step sl, it is described be stirred to react the time be 12-48 hours.
Preferably, in step s 2, the water-soluble sulfide be in potassium sulfide, vulcanized sodium or ammonium sulfide at least
It is a kind of.
Preferably, in step s 2, the Cd3(C3N3S3)2Mass ratio with deionized water is 1:[40-400]
Preferably, in step s 2, the Cd3(C3N3S3)2Molar ratio with dissolvable sulfide is 1:[3-6].
Preferably, in step s 2, it is described be stirred to react the time be 0.5-48 hours.
The present invention has raw material cheap, simple process, organic solvent-free and surfactant, without it is poisonous and hazardous it is organic in
The features such as mesosome generates, the morphology controllable of target product.Regular octahedron cadmium sulfide obtained by the present invention is a kind of three-dimensional big
The cadmium sulfide of specific surface area can be used in the hydrogen manufacturing of visible light solution water, photocatalytically degradating organic dye, photocatalysis point as photochemical catalyst
Solution organic matter, photocatalysis carbon dioxide reduction prepare the reaction such as the organic matters such as methanol and photocatalysis to selectively oxidation of hydrocarbons
In.
[Brief Description Of Drawings]
Fig. 1 show regular octahedron Cd obtained by the embodiment of the present invention 13(C3N3S3)2Scanning electron microscope diagram；
Fig. 2 show the scanning electron microscope diagram of regular octahedron cadmium sulfide obtained by the embodiment of the present invention 2；
Fig. 3 show the scanning electron microscope diagram of regular octahedron cadmium sulfide obtained by the embodiment of the present invention 3；
Fig. 4 show the scanning electron microscope diagram of graininess cadmium sulfide obtained by comparative example 2 of the present invention.
[specific embodiment]
Below with reference to the embodiment of the present invention, the present invention will be further described:
Embodiment 1
According to caddy in reaction mixture: the molar ratio of trithiocyanuric acid is 1:[0.5], it weighs 2.75 grams of caddies and adds
Enter in 200 ml deionized waters, stirring and dissolving；It weighs 1.33 grams of trithiocyanuric acids to be added in 200 ml deionized waters, stir molten
Solution.Then trithiocyanuric acid solution is slowly dropped in cadmium chloride solution at room temperature, continues stirring 12 hours after being added dropwise.
It is centrifuged according to a conventional method, washs, dries and roast to obtain buff powder.Using X-ray powder diffraction instrument, scanning electron microscopy
Mirror etc. characterizes yellow powder, product be Cd3(C3N3S3)2Coordination polymer, stereoscan photograph show, gained
Cd3(C3N3S3)2Be positive shape of octahedron, and diameter is about 1-3 microns, as shown in Fig. 1.
By above-mentioned regular octahedron Cd3(C3N3S3)20.7 mM is scattered in 100 ml deionized waters, is then added nine
Water vulcanized sodium continues to stir at room temperature, controls Cd3(C3N3S3)2Molar ratio with vulcanized sodium is 1:3, is stirred 24 hours at room temperature.
Centrifugation, deionized water washing, dehydrated alcohol washing, dry regular octahedron cadmium sulfide according to a conventional method.Catalyst morphology with
Grain size is characterized using Hitachi S-4800 scanning electron microscope, and sample is before being scanned electron-microscopic analysis test
Vacuum metal spraying.Using X-ray powder diffraction instrument, the stereoscan photographs such as scanning electron microscope show that gained cadmium sulfide is positive
Shape of octahedron, diameter are about 1-3 microns.
The photocatalytic activity of prepared catalyst is investigated using photodissociation aquatic products hydrogen as model reaction: prepared by taking 20 milligrams just
Octahedra cadmium sulfide is scattered in 50 milliliters of lactic acid solutions (200 ml ls), and platinum acid chloride solution is added, and (load capacity of platinum is
1wt%), reaction system is extracted into vacuum with vacuum pump, the lower stirring of dark 30 minutes, then open light source (300 watts of xenon lamp,
Optical filter is added and filters light of the wavelength less than 420 nanometers), opening simultaneously condensate liquid control reaction temperature is 5 degrees Celsius.With being furnished with
The gas Chromatographic Determination hydrogen output of thermal conductivity cell detector and 5A molecular sieve splitter.Illumination 3 hours, hydrogen-producing speed was 11.4 mmoles
Your catalyst per hour per gram.
Embodiment 2
According to two water cadmium acetate in reaction mixture: the molar ratio of trithiocyanuric acid is 1:[0.67], weigh 4.00 gram two
Water cadmium acetate is added in 200 ml deionized waters, stirring and dissolving；It weighs 1.78 grams of trithiocyanuric acids and 200 milliliters of deionizations is added
In water, stirring and dissolving.Then trithiocyanuric acid solution is slowly dropped in cadmium acetate solution at room temperature, is continued after being added dropwise
Stirring 48 hours.It is centrifuged according to a conventional method, washs, dries and roast to obtain buff powder.Using X-ray powder diffraction instrument, sweep
Electron microscope etc. is retouched to characterize yellow powder, product be Cd3(C3N3S3)2, stereoscan photograph shows, gained
Cd3(C3N3S3)2Be positive shape of octahedron, and diameter is about 1-3 microns.
The preparation method of regular octahedron cadmium sulfide is same as Example 1, the scanning electricity of obtained regular octahedron cadmium sulfide
Sub- microscope figure is as shown in Fig. 2.
The photocatalytic activity of prepared catalyst, evaluation condition and embodiment 1 are investigated using photodissociation aquatic products hydrogen as model reaction
Identical, illumination 3 hours, hydrogen-producing speed was 11.1 mMs of catalyst per hour per gram.
Embodiment 3
According to four water cadmium nitrate in reaction mixture: the molar ratio of trithiocyanuric acid trisodium is 1:[0.67], weigh 4.63
Gram four water cadmium nitrates are added in 200 ml deionized waters, stirring and dissolving；It weighs 2.43 grams of trithiocyanuric acid trisodiums and 200 millis is added
It rises in deionized water, stirring and dissolving.Then three sodium solution of trithiocyanuric acid is slowly dropped in nitric acid cadmium solution at room temperature, is dripped
It adds and continues stirring 24 hours after finishing.It is centrifuged according to a conventional method, washs, dries and roast to obtain buff powder.Using X-ray
Powder diffractometer, scanning electron microscope etc. characterize yellow powder, product be Cd3(C3N3S3)2, scanning electron microscope photograph
Piece shows, gained Cd3(C3N3S3)2Be positive shape of octahedron, and diameter is about 1-3 microns.
The preparation method of regular octahedron cadmium sulfide is same as Example 1, the scanning electricity of obtained regular octahedron cadmium sulfide
Sub- microscope figure is as shown in Fig. 3.
The photocatalytic activity of prepared catalyst, evaluation condition and embodiment 1 are investigated using photodissociation aquatic products hydrogen as model reaction
Identical, illumination 3 hours, hydrogen-producing speed was 12.4 mMs of catalyst per hour per gram.
Embodiment 4
According to four water cadmium nitrate in reaction mixture: the molar ratio of trithiocyanuric acid trisodium is 1:1, weighs 4.63 gram of four water
Cadmium nitrate is added in 200 ml deionized waters, stirring and dissolving；Weigh 3.65 grams of trithiocyanuric acid trisodiums be added 200 milliliters go from
In sub- water, stirring and dissolving.Then three sodium solution of trithiocyanuric acid is slowly dropped in nitric acid cadmium solution at room temperature, is added dropwise
After continue stirring 24 hours.It is centrifuged according to a conventional method, washs, dries and roast to obtain buff powder.Spread out using X-ray powder
Penetrate instrument, scanning electron microscope etc. characterizes yellow powder, product be Cd3(C3N3S3)2, stereoscan photograph is aobvious
Show, gained Cd3(C3N3S3)2Be positive shape of octahedron, and diameter is about 1-4 microns.
The preparation method of regular octahedron cadmium sulfide is same as Example 1.
The photocatalytic activity of prepared catalyst, evaluation condition and embodiment 1 are investigated using photodissociation aquatic products hydrogen as model reaction
Identical, illumination 3 hours, hydrogen-producing speed was 11.8 mMs of catalyst per hour per gram.
Embodiment 5
According to two water cadmium acetate in reaction mixture: the molar ratio of trithiocyanuric acid tripotassium is 1:[1.33], weigh 4.00
Gram two water cadmium acetates are added in 200 ml deionized waters, stirring and dissolving；It weighs 5.18 grams of trithiocyanuric acid tripotassiums and 200 millis is added
It rises in deionized water, stirring and dissolving.Then three potassium solution of trithiocyanuric acid is slowly dropped in cadmium acetate solution at room temperature, is dripped
It adds and continues stirring 36 hours after finishing.It is centrifuged according to a conventional method, washs, dries and roast to obtain buff powder.Using X-ray
Powder diffractometer, scanning electron microscope etc. characterize yellow powder, product be Cd3(C3N3S3)2, scanning electron microscope photograph
Piece shows, gained Cd3(C3N3S3)2Be positive shape of octahedron, and diameter is about 2-5 microns.
The preparation method of regular octahedron cadmium sulfide is same as Example 1.
The photocatalytic activity of prepared catalyst, evaluation condition and embodiment 1 are investigated using photodissociation aquatic products hydrogen as model reaction
Identical, illumination 3 hours, hydrogen-producing speed was 11.6 mMs of catalyst per hour per gram.
Embodiment 6
According to caddy in reaction mixture: the molar ratio of trithiocyanuric acid tripotassium is 1:2, weighs 2.75 grams of caddies and adds
Enter in 200 ml deionized waters, stirring and dissolving；It weighs 7.77 grams of trithiocyanuric acid tripotassiums to be added in 200 ml deionized waters, stir
Mix dissolution.Then three potassium solution of trithiocyanuric acid is slowly dropped in cadmium chloride solution at room temperature, continues to stir after being added dropwise
It mixes 12 hours.It is centrifuged according to a conventional method, washs, dries and roast to obtain buff powder.Using X-ray powder diffraction instrument, scanning
Electron microscope etc. characterizes yellow powder, product be Cd3(C3N3S3)2, stereoscan photograph shows, gained Cd3
(C3N3S3)2Be positive shape of octahedron, and diameter is about 2-5 microns.
The preparation method of regular octahedron cadmium sulfide is same as Example 1.
The photocatalytic activity of prepared catalyst, evaluation condition and embodiment 1 are investigated using photodissociation aquatic products hydrogen as model reaction
Identical, illumination 3 hours, hydrogen-producing speed was 11.5 mMs of catalyst per hour per gram.
Embodiment 7
According to four water cadmium nitrate in reaction mixture: the molar ratio of trithiocyanuric acid trisodium is 1:[1.33], weigh 4.63
Gram four water cadmium nitrates are added in 200 ml deionized waters, stirring and dissolving；It weighs 4.85 grams of trithiocyanuric acid trisodiums and 200 millis is added
It rises in deionized water, stirring and dissolving.Then three sodium solution of trithiocyanuric acid is slowly dropped in nitric acid cadmium solution at room temperature, is dripped
It adds and continues stirring 48 hours after finishing.It is centrifuged according to a conventional method, washs, dries and roast to obtain buff powder.Using X-ray
Powder diffractometer, scanning electron microscope etc. characterize yellow powder, product be Cd3(C3N3S3)2, scanning electron microscope photograph
Piece shows, gained Cd3(C3N3S3)2Be positive shape of octahedron, and diameter is about 2-5 microns.
The preparation method of regular octahedron cadmium sulfide is same as Example 1.
The photocatalytic activity of prepared catalyst, evaluation condition and embodiment 1 are investigated using photodissociation aquatic products hydrogen as model reaction
Identical, illumination 3 hours, hydrogen-producing speed was 11.3 mMs of catalyst per hour per gram.
Embodiment 8
According to two water cadmium acetate in reaction mixture: the molar ratio of trithiocyanuric acid is 1:1, weighs 4.00 gram of two water acetic acid
Cadmium is added in 200 ml deionized waters, stirring and dissolving；It weighs 2.66 grams of trithiocyanuric acids to be added in 200 ml deionized waters, stir
Mix dissolution.Then trithiocyanuric acid solution is slowly dropped in cadmium acetate solution at room temperature, continues stirring 24 after being added dropwise
Hour.It is centrifuged according to a conventional method, washs, dries and roast to obtain buff powder.Using X-ray powder diffraction instrument, scanning electron
Microscope etc. characterizes yellow powder, product be Cd3(C3N3S3)2, stereoscan photograph shows, gained Cd3
(C3N3S3)2Be positive shape of octahedron, and diameter is about 1-4 microns.
The preparation method of regular octahedron cadmium sulfide is same as Example 1.
The photocatalytic activity of prepared catalyst, evaluation condition and embodiment 1 are investigated using photodissociation aquatic products hydrogen as model reaction
Identical, illumination 3 hours, hydrogen-producing speed was 11.0 mMs of catalyst per hour per gram.
Embodiment 9
According to caddy in reaction mixture: the molar ratio of trithiocyanuric acid tripotassium is 1:[1.67], weigh 2.75 grams of chlorine
Cadmium is added in 200 ml deionized waters, stirring and dissolving；It weighs 6.49 grams of trithiocyanuric acid tripotassiums and 200 milliliters of deionizations is added
In water, stirring and dissolving.Then three potassium solution of trithiocyanuric acid is slowly dropped in cadmium chloride solution at room temperature, after being added dropwise
Continue stirring 36 hours.It is centrifuged according to a conventional method, washs, dries and roast to obtain buff powder.Using X-ray powder diffraction
Instrument, scanning electron microscope etc. characterize yellow powder, product be Cd3(C3N3S3)2, stereoscan photograph shows,
Gained Cd3(C3N3S3)2Be positive shape of octahedron, and diameter is about 2-5 microns.
The preparation method of regular octahedron cadmium sulfide is same as Example 1.
The photocatalytic activity of prepared catalyst, evaluation condition and embodiment 1 are investigated using photodissociation aquatic products hydrogen as model reaction
Identical, illumination 3 hours, hydrogen-producing speed was 10.5 mMs of catalyst per hour per gram.
Embodiment 10
According to two water cadmium acetate in reaction mixture: the molar ratio of trithiocyanuric acid trisodium is 1:[0.5], weigh 4.00 grams
Two water cadmium acetates are added in 200 ml deionized waters, stirring and dissolving；It weighs 1.82 grams of trithiocyanuric acid trisodiums and is added 200 milliliters
In deionized water, stirring and dissolving.Then three sodium solution of trithiocyanuric acid is slowly dropped in cadmium acetate solution at room temperature, is added dropwise
After continue stirring 36 hours.It is centrifuged according to a conventional method, washs, dries and roast to obtain buff powder.Using X-ray powder
Last diffractometer, scanning electron microscope etc. characterize yellow powder, product be Cd3(C3N3S3)2, stereoscan photograph
It has been shown that, gained Cd3(C3N3S3)2Be positive shape of octahedron, and diameter is about 1-3 microns.
The preparation method of regular octahedron cadmium sulfide is same as Example 1.
The photocatalytic activity of prepared catalyst, evaluation condition and embodiment 1 are investigated using photodissociation aquatic products hydrogen as model reaction
Identical, illumination 3 hours, hydrogen-producing speed was 11.5 mMs of catalyst per hour per gram.
Embodiment 11
Regular octahedron Cd3(C3N3S3)2The preparation method of coordination polymer is same as Example 3.
By above-mentioned regular octahedron Cd3(C3N3S3)20.7 mM is scattered in 50 ml deionized waters, and nine water are then added
Vulcanized sodium continues to stir at room temperature, controls Cd3(C3N3S3)2Molar ratio with vulcanized sodium is 1:3, is stirred 12 hours at room temperature.It presses
Conventional method centrifugation, deionized water washing, dehydrated alcohol washing, dry regular octahedron cadmium sulfide.Catalyst morphology and particle
Size is characterized using Hitachi S-4800 scanning electron microscope, and sample is true before being scanned electron-microscopic analysis test
Empty metal spraying.Using X-ray powder diffraction instrument, the stereoscan photographs such as scanning electron microscope are shown, gained cadmium sulfide is positive eight
Face bodily form looks, diameter are about 1-3 microns.
The photocatalytic activity of prepared catalyst, evaluation condition and embodiment 1 are investigated using photodissociation aquatic products hydrogen as model reaction
Identical, illumination 3 hours, hydrogen-producing speed was 12.5 mMs of catalyst per hour per gram.
Embodiment 12
Regular octahedron Cd3(C3N3S3)2The preparation method of coordination polymer is same as Example 3.
By above-mentioned regular octahedron Cd3(C3N3S3)20.7 mM is scattered in 100 ml deionized waters, is then added nine
Water vulcanized sodium continues to stir at room temperature, controls Cd3(C3N3S3)2Molar ratio with vulcanized sodium is 1:5, is stirred 24 hours at room temperature.
Centrifugation, deionized water washing, dehydrated alcohol washing, dry regular octahedron cadmium sulfide according to a conventional method.Catalyst morphology with
Grain size is characterized using Hitachi S-4800 scanning electron microscope, and sample is before being scanned electron-microscopic analysis test
Vacuum metal spraying.Using X-ray powder diffraction instrument, the stereoscan photographs such as scanning electron microscope show that gained cadmium sulfide is positive
Shape of octahedron, diameter are about 1-3 microns.
The photocatalytic activity of prepared catalyst, evaluation condition and embodiment 1 are investigated using photodissociation aquatic products hydrogen as model reaction
Identical, illumination 3 hours, hydrogen-producing speed was 12.2 mMs of catalyst per hour per gram.
Embodiment 13
Regular octahedron Cd3(C3N3S3)2The preparation method of coordination polymer is same as Example 3.
By above-mentioned regular octahedron Cd3(C3N3S3)20.7 mM is scattered in 200 ml deionized waters, and sulphur is then added
Change potassium, continue to stir at room temperature, controls Cd3(C3N3S3)2Molar ratio with potassium sulfide is 1:4, is stirred 36 hours at room temperature.By normal
The centrifugation of rule method, deionized water washing, dehydrated alcohol washing, dry regular octahedron cadmium sulfide.Catalyst morphology is big with particle
Small to be characterized using Hitachi S-4800 scanning electron microscope, sample is being scanned electron-microscopic analysis test initial vacuum
Metal spraying.Using X-ray powder diffraction instrument, the stereoscan photographs such as scanning electron microscope are shown, gained cadmium sulfide is positive octahedral
Bodily form looks, diameter are about 1-3 microns.
The photocatalytic activity of prepared catalyst, evaluation condition and embodiment 1 are investigated using photodissociation aquatic products hydrogen as model reaction
Identical, illumination 3 hours, hydrogen-producing speed was 12.3 mMs of catalyst per hour per gram.
Embodiment 14
Regular octahedron Cd3(C3N3S3)2The preparation method of coordination polymer is same as Example 3.
By above-mentioned regular octahedron Cd3(C3N3S3)20.7 mM is scattered in 50 ml deionized waters, and vulcanization is then added
Potassium continues to stir at room temperature, controls Cd3(C3N3S3)2Molar ratio with potassium sulfide is 1:6, is stirred 12 hours at room temperature.Routinely
Method centrifugation, deionized water washing, dehydrated alcohol washing, dry regular octahedron cadmium sulfide.Catalyst morphology and granular size
It is characterized using Hitachi S-4800 scanning electron microscope, sample is being scanned electron-microscopic analysis test initial vacuum spray
Gold.Using X-ray powder diffraction instrument, the stereoscan photographs such as scanning electron microscope are shown, gained cadmium sulfide is regular octahedron
Pattern, diameter are about 1-3 microns.
The photocatalytic activity of prepared catalyst, evaluation condition and embodiment 1 are investigated using photodissociation aquatic products hydrogen as model reaction
Identical, illumination 3 hours, hydrogen-producing speed was 12.8 mMs of catalyst per hour per gram.
Embodiment 15
Regular octahedron Cd3(C3N3S3)2The preparation method of coordination polymer is same as Example 3.
By above-mentioned regular octahedron Cd3(C3N3S3)20.7 mM is scattered in 100 ml deionized waters, and sulphur is then added
Change ammonium, continue to stir at room temperature, controls Cd3(C3N3S3)2Molar ratio with ammonium sulfide is 1:4, is stirred 48 hours at room temperature.By normal
The centrifugation of rule method, deionized water washing, dehydrated alcohol washing, dry regular octahedron cadmium sulfide.Catalyst morphology is big with particle
Small to be characterized using Hitachi S-4800 scanning electron microscope, sample is being scanned electron-microscopic analysis test initial vacuum
Metal spraying.Using X-ray powder diffraction instrument, the stereoscan photographs such as scanning electron microscope are shown, gained cadmium sulfide is positive octahedral
Bodily form looks, diameter are about 1-3 microns.
The photocatalytic activity of prepared catalyst, evaluation condition and embodiment 1 are investigated using photodissociation aquatic products hydrogen as model reaction
Identical, illumination 3 hours, hydrogen-producing speed was 12.5 mMs of catalyst per hour per gram.
Embodiment 16
Regular octahedron Cd3(C3N3S3)2The preparation method of coordination polymer is same as Example 3.
By above-mentioned regular octahedron Cd3(C3N3S3)20.7 mM is scattered in 200 ml deionized waters, and sulphur is then added
Change ammonium, continue to stir at room temperature, controls Cd3(C3N3S3)2Molar ratio with ammonium sulfide is 1:5, is stirred 24 hours at room temperature.By normal
The centrifugation of rule method, deionized water washing, dehydrated alcohol washing, dry regular octahedron cadmium sulfide.Catalyst morphology is big with particle
Small to be characterized using Hitachi S-4800 scanning electron microscope, sample is being scanned electron-microscopic analysis test initial vacuum
Metal spraying.Using X-ray powder diffraction instrument, the stereoscan photographs such as scanning electron microscope are shown, gained cadmium sulfide is positive octahedral
Bodily form looks, diameter are about 1-3 microns.
The photocatalytic activity of prepared catalyst, evaluation condition and embodiment 1 are investigated using photodissociation aquatic products hydrogen as model reaction
Identical, illumination 3 hours, hydrogen-producing speed was 11.9 mMs of catalyst per hour per gram.
Comparative example 1
Regular octahedron Cd3(C3N3S3)2The preparation method of coordination polymer is same as Example 1.
Prepared regular octahedron Cd is investigated by model reaction of photodissociation aquatic products hydrogen3(C3N3S3)2The photocatalysis of coordination polymer
Activity, evaluation condition is same as Example 1, and illumination 3 hours, hydrogen-producing speed was 0.01 mM of catalyst per hour per gram.
Comparative example 2
Graininess cadmium sulfide is prepared at room temperature.According to four water cadmium nitrate in mixture: the molar ratio of nine water vulcanized sodium is 1:
1, it weighs 4.63 gram of four water cadmium nitrate and is added in 200 ml deionized waters, stirring and dissolving；It weighs nine water vulcanized sodium and 200 millis is added
It rises in deionized water, stirring and dissolving.Then sodium sulfide solution is slowly dropped in nitric acid cadmium solution at room temperature, after being added dropwise
Continue stirring 24 hours.It is centrifuged, washs according to a conventional method, dry graininess cadmium sulfide.Its pattern and granular size use
Hitachi S-4800 scanning electron microscope characterization, as shown in Figure 4.
The photocatalytic activity of prepared catalyst, evaluation condition and embodiment 1 are investigated using photodissociation aquatic products hydrogen as model reaction
Identical, illumination 3 hours, hydrogen-producing speed was 4.6 mMs of catalyst per hour per gram.
Above-described embodiment and comparative example can be seen that regular octahedron cadmium sulfide made from the method for the present invention with unique object
Change structure feature, it under visible light can efficient photodissociation aquatic products hydrogen as photochemical catalyst.
Claims (10)
1. a kind of preparation method of regular octahedron cadmium sulfide comprising the steps of:
S1, it takes cadmium salt to be dissolved in deionized water, obtains cadmium salt soln；Trithiocyanuric acid and/or cyclo-trithocyanates is taken to dissolve
In deionized water, clear solution is obtained；Cadmium salt soln is added dropwise at room temperature to clear solution, stirs, is centrifugated, wash, make
Obtain regular octahedron Cd3(C3N3S3)2Coordination polymer；
S2, by regular octahedron Cd obtained above3(C3N3S3)2Coordination polymer is scattered in deionized water, is added with stirring water
Dissolubility sulfide continues to stir, and is centrifugated, and washs, dry, obtains regular octahedron cadmium sulfide.
2. preparation method according to claim 1, which is characterized in that in step sl, the cadmium salt is caddy, four water
At least one of cadmium nitrate or two water cadmium acetates.
3. preparation method according to claim 1, which is characterized in that in step sl, the cyclo-trithocyanates are three
Polysulfide cyanic acid trisodium and/or trithiocyanuric acid tripotassium.
4. preparation method according to claim 1, which is characterized in that in step sl, the cadmium salt and trithiocyanuric acid
And/or the molar ratio of cyclo-trithocyanates is 1:[0.5-2].
5. preparation method according to claim 1, which is characterized in that in step sl, described to be stirred to react the time as 12-
48 hours.
6. preparation method according to claim 1, which is characterized in that in step s 2, the water-soluble sulfide is choosing
At least one of autovulcanization potassium, vulcanized sodium or ammonium sulfide.
7. preparation method according to claim 1, which is characterized in that in step s 2, the Cd3(C3N3S3)2With go from
The mass ratio of sub- water is 1:[40-400].
8. preparation method according to claim 1, which is characterized in that in step s 2, the Cd3(C3N3S3)2With it is water-soluble
Property sulfide molar ratio be 1:[3-6].
9. preparation method according to claim 1, which is characterized in that in step s 2, described to be stirred to react the time and be
0.5-48 hours.
10. a kind of regular octahedron cadmium sulfide prepared by preparation method described in any one of claim 1-9, as photocatalysis
Agent visible light photolysis water hydrogen, photocatalytically degradating organic dye, photocatalysis Decomposition organic matter, photocatalytic reduction of carbon oxide and
Application in the reaction of photocatalysis to selectively oxidation of hydrocarbons.
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