CN107126964A - A kind of preparation method of regular octahedron cadmium sulfide and application - Google Patents
A kind of preparation method of regular octahedron cadmium sulfide and application Download PDFInfo
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- CN107126964A CN107126964A CN201710269000.5A CN201710269000A CN107126964A CN 107126964 A CN107126964 A CN 107126964A CN 201710269000 A CN201710269000 A CN 201710269000A CN 107126964 A CN107126964 A CN 107126964A
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- cadmium
- regular octahedron
- water
- 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 58
- 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
- 230000035484 reaction time Effects 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 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 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
- 238000007796 conventional method Methods 0.000 description 14
- 239000000203 mixture Substances 0.000 description 14
- 238000005406 washing Methods 0.000 description 14
- 238000000634 powder X-ray diffraction Methods 0.000 description 12
- 239000000376 reactant Substances 0.000 description 11
- 238000001035 drying Methods 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
- 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
- 229910052793 cadmium Inorganic materials 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002389 environmental scanning electron microscopy Methods 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
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 230000000694 effects Effects 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
- 230000008569 process Effects 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
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-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
- 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
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004140 cleaning 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
- 238000005191 phase separation Methods 0.000 description 1
- 239000002096 quantum dot 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
- 238000000926 separation method Methods 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
- 238000006467 substitution reaction Methods 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
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- 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
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- 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
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- 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
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- Combustion & Propulsion (AREA)
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Abstract
The invention discloses a kind of preparation method and application of regular octahedron cadmium sulfide.The preparation method that the present invention is provided has raw material cheap, and technique is simple, organic solvent-free and surfactant, is produced without poisonous and hazardous organic intermediate, the features such as the morphology controllable of target product.The invention further relates to 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 ray solution water, photocatalytically degradating organic dye, photocatalysis Decomposition organic matter, photocatalysis carbon dioxide reduction.The catalyst has good stability, and continuous use remains in that higher photocatalytic activity in 100 hours.
Description
【Technical field】
The present invention relates to the preparation and application technical field of catalysis material sulfide, a kind of positive octahedral is related in particular to
The preparation method of body cadmium sulfide and application.
【Background technology】
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,
Hydrogen or a kind of new energy, have the advantages that high combustion heat value, high combustion efficiency and combustion product are cleaned, are generally considered
The clean energy resource of most possible substitution fossil energy.Therefore, the exploitation of hydrogen is that current chemical industry develops with energy field technology
Emphasis.
At present, it is industrial to use the method hydrogen manufacturing such as Coal Gasification hydrogen manufacturing, heavy oil and the conversion of gas water steam catalytic, so
And, these methods not only inefficiency, and need to expend substantial amounts of fossil energy.Utilize inexhaustible cleaning
Solar energy, water decomposition is produced by hydrogen by Photocatalitic Technique of Semiconductor, energy crisis and environment will be effectively solved simultaneously
Two large problems are polluted, therefore photodissociation aquatic products hydrogen technology has obvious superiority, it reacts schematic diagram as shown in Figure 1.
At present, a variety of catalyst have been widely used in the reaction of photodissociation aquatic products hydrogen.In these catalysis materials,
Cadmium sulfide because direct transition type band structure, luminous color it is abundant the features such as, in solar energy conversion, photoelectron chemical cell, non-
All there is extensive and far-reaching application prospect in terms of linear optics and photocatalysis.
During conductor photocatalysis decomposes aquatic products hydrogen, the body phase separation of the absorption of light and electric charge and from body phase to
The speed of surface transfer is the key factor for determining hydrogen generation efficiency, because 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 be effectively increased contact area and tightness degree between CdS semiconduct and water.Use conventional side
The cadmium sulfide that method is prepared 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 the last few years, researchers developed 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 the three-dimensional appearance such as spherical.
Three-dimensional structure often has the specific surface area bigger than low dimensional structures material and more Adsorptions, this knot
Structure can not only strengthen the absorption of light, while the separation of surface carrier and the transmission of interface carrier are also greatly facilitated, very
The photocatalytic activity of cadmium sulfide is improved in big degree.However, the research about special three-dimensional appearance cadmium sulfide is less, these are synthesized
The method of special appearance cadmium sulfide is generally required for introducing 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 produced.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
It is of great significance using tool.
【The content of the invention】
It is an object of the invention to provide a kind of preparation method of regular octahedron cadmium sulfide and application, and by the materials application
In the reaction of photodissociation aquatic products hydrogen.The catalyst preparation is simple and easy to do, with higher activity and stability.
The regular octahedron cadmium sulfide catalyst that the present invention is provided, is synthesized using the step of ion exchange two.
To reach above-mentioned purpose, the present invention prepares regular octahedron cadmium sulfide photochemical catalyst, i.e. (S1) using two-step method and prepared
Regular octahedron Cd3(C3N3S3)2Presoma；(S2) regular octahedron cadmium sulfide photochemical catalyst is prepared.
The step of this law invention prepares regular octahedron cadmium sulfide photochemical catalyst is as follows：
S1, take cadmium salt to be dissolved in deionized water, obtain cadmium salt soln；Take trithiocyanuric acid and/or cyclo-trithocyanates
It is dissolved in deionized water, obtains settled solution；Cadmium salt soln is added dropwise at room temperature to settled solution, stirs, centrifuges, wash
Wash, that is, regular octahedron Cd is made3(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, centrifuge, wash, dry, that is, regular octahedron cadmium sulfide is made.
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 mol ratio of the cadmium salt and trithiocyanuric acid and/or cyclo-trithocyanates is 1：
[0.5-2]。
Preferably, in step sl, the stirring reaction time is 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)2Mol ratio with dissolvable sulfide is 1：[3-6].
Preferably, in step s 2, the stirring reaction time is 0.5-48 hours.
The present invention has raw material cheap, and technique is simple, organic solvent-free and surfactant, without it is poisonous and hazardous it is organic in
The features such as mesosome generation, 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, the hydrogen manufacturing of visible ray solution water, photocatalytically degradating organic dye, photocatalysis point can be used in 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 the 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 the regular octahedron cadmium sulfide obtained by the embodiment of the present invention 2；
Fig. 3 show the scanning electron microscope diagram of the regular octahedron cadmium sulfide obtained by the embodiment of the present invention 3；
Fig. 4 show the scanning electron microscope diagram of the graininess cadmium sulfide obtained by comparative example 2 of the present invention.
【Embodiment】
With reference to the embodiment of the present invention, the present invention will be further described：
Embodiment 1
According to caddy in reactant mixture：The mol ratio of trithiocyanuric acid is 1:[0.5], 2.75 grams of caddies are weighed to add
Enter in 200 ml deionized waters, stirring and dissolving；Weigh 1.33 grams of trithiocyanuric acids to add in 200 ml deionized waters, stir molten
Solution.Then trithiocyanuric acid solution is slowly dropped in cadmium chloride solution at room temperature, continues to stir 12 hours after completion of dropping.
Centrifuge, wash according to a conventional method, drying and being calcined to obtain buff powder.Using X-ray powder diffraction instrument, scanning electron microscopy
Mirror etc. is characterized to yellow powder, product be Cd3(C3N3S3)2Coordination polymer, stereoscan photograph shows, gained
Cd3(C3N3S3)2For regular octahedron pattern, diameter is about 1-3 microns, as shown in Figure 1.
By above-mentioned regular octahedron Cd3(C3N3S3)20.7 mM is scattered in 100 ml deionized waters, then adds nine
Water vulcanized sodium, continues to stir at room temperature, controls Cd3(C3N3S3)2Mol ratio with vulcanized sodium is 1:3, stir 24 hours at room temperature.
Centrifugation, deionized water washing, absolute ethyl alcohol washing, dry regular octahedron cadmium sulfide according to a conventional method.Catalyst pattern with
Grain size is characterized using Hitachi S-4800 SEM, and sample is before electron-microscopic analysis test is scanned
Vacuum metal spraying.Using X-ray powder diffraction instrument, the stereoscan photograph such as SEM is shown, gained cadmium sulfide is just
Shape of octahedron, diameter is about 1-3 microns.
The photocatalytic activity of prepared catalyst is investigated by model reaction of photodissociation aquatic products hydrogen：Take prepared by 20 milligrams just
Octahedra cadmium sulfide, is scattered in 50 milliliters of lactic acid solutions (200 ml l), and adding platinum acid chloride solution, (load capacity of platinum is
1wt%), reaction system is extracted into vacuum with vavuum pump, the lower stirring of dark 30 minutes, then open light source (300 watts of xenon lamp,
Add optical filter and filter the light that wavelength is less than 420 nanometers), while it is 5 degrees Celsius to open condensate liquid controlling reaction temperature.With equipped with
The gas Chromatographic Determination hydrogen output of thermal conductivity cell detector and 5A molecular sieve splitters.Illumination 3 hours, hydrogen-producing speed is 11.4 mmoles
Your catalyst per hour per gram.
Embodiment 2
According to two water cadmium acetate in reactant mixture：The mol ratio of trithiocyanuric acid is 1:[0.67], 4.00 gram two is weighed
Water cadmium acetate is added in 200 ml deionized waters, stirring and dissolving；Weigh 1.78 grams of trithiocyanuric acids and add 200 milliliters of deionizations
In water, stirring and dissolving.Then trithiocyanuric acid solution is slowly dropped in cadmium acetate solution at room temperature, continued after completion of dropping
Stirring 48 hours.Centrifuge, wash according to a conventional method, drying and being calcined 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)2For regular octahedron pattern, diameter is about 1-3 microns.
The preparation method of regular octahedron cadmium sulfide is same as Example 1, and the scanning of obtained regular octahedron cadmium sulfide is electric
Sub- microscope figure is as shown in Figure 2.
The photocatalytic activity of prepared catalyst, appreciation condition and embodiment 1 are investigated by model reaction of photodissociation aquatic products hydrogen
Identical, illumination 3 hours, hydrogen-producing speed is 11.1 mMs of catalyst per hour per gram.
Embodiment 3
According to four water cadmium nitrate in reactant mixture：The mol ratio of trithiocyanuric acid trisodium is 1:[0.67], 4.63 are weighed
Gram four water cadmium nitrates are added in 200 ml deionized waters, stirring and dissolving；Weigh 2.43 grams of trithiocyanuric acid trisodiums and add 200 millis
Rise in deionized water, stirring and dissolving.Then the sodium solution of trithiocyanuric acid three is slowly dropped in nitric acid cadmium solution at room temperature, dripped
Add and continue to stir 24 hours after finishing.Centrifuge, wash according to a conventional method, drying and being calcined to obtain buff powder.Using X-ray
Powder diffractometer, SEM etc. is characterized to yellow powder, product be Cd3(C3N3S3)2, ESEM photograph
Piece shows, gained Cd3(C3N3S3)2For regular octahedron pattern, diameter is about 1-3 microns.
The preparation method of regular octahedron cadmium sulfide is same as Example 1, and the scanning of obtained regular octahedron cadmium sulfide is electric
Sub- microscope figure is as shown in Figure 3.
The photocatalytic activity of prepared catalyst, appreciation condition and embodiment 1 are investigated by model reaction of photodissociation aquatic products hydrogen
Identical, illumination 3 hours, hydrogen-producing speed is 12.4 mMs of catalyst per hour per gram.
Embodiment 4
According to four water cadmium nitrate in reactant mixture：The mol ratio of trithiocyanuric acid trisodium is 1:1, weigh 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 add 200 milliliters go from
In sub- water, stirring and dissolving.Then the sodium solution of trithiocyanuric acid three is slowly dropped in nitric acid cadmium solution at room temperature, completion of dropping
Continue to stir 24 hours afterwards.Centrifuge, wash according to a conventional method, drying and being calcined to obtain buff powder.Spread out using X-ray powder
Penetrate instrument, SEM etc. is characterized to yellow powder, product be Cd3(C3N3S3)2, stereoscan photograph show
Show, gained Cd3(C3N3S3)2For regular octahedron pattern, 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, appreciation condition and embodiment 1 are investigated by model reaction of photodissociation aquatic products hydrogen
Identical, illumination 3 hours, hydrogen-producing speed is 11.8 mMs of catalyst per hour per gram.
Embodiment 5
According to two water cadmium acetate in reactant mixture：The mol ratio of trithiocyanuric acid tripotassium is 1:[1.33], 4.00 are weighed
Gram two water cadmium acetates are added in 200 ml deionized waters, stirring and dissolving；Weigh 5.18 grams of trithiocyanuric acid tripotassiums and add 200 millis
Rise in deionized water, stirring and dissolving.Then the potassium solution of trithiocyanuric acid three is slowly dropped in cadmium acetate solution at room temperature, dripped
Add and continue to stir 36 hours after finishing.Centrifuge, wash according to a conventional method, drying and being calcined to obtain buff powder.Using X-ray
Powder diffractometer, SEM etc. is characterized to yellow powder, product be Cd3(C3N3S3)2, ESEM photograph
Piece shows, gained Cd3(C3N3S3)2For regular octahedron pattern, 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, appreciation condition and embodiment 1 are investigated by model reaction of photodissociation aquatic products hydrogen
Identical, illumination 3 hours, hydrogen-producing speed is 11.6 mMs of catalyst per hour per gram.
Embodiment 6
According to caddy in reactant mixture：The mol ratio of trithiocyanuric acid tripotassium is 1:2, weigh 2.75 grams of caddies and add
Enter in 200 ml deionized waters, stirring and dissolving；Weigh 7.77 grams of trithiocyanuric acid tripotassiums to add in 200 ml deionized waters, stir
Mix dissolving.Then the potassium solution of trithiocyanuric acid three is slowly dropped in cadmium chloride solution at room temperature, continues to stir after completion of dropping
Mix 12 hours.Centrifuge, wash according to a conventional method, drying and being calcined to obtain buff powder.Using X-ray powder diffraction instrument, scanning
Electron microscope etc. is characterized to yellow powder, product be Cd3(C3N3S3)2, stereoscan photograph shows, gained Cd3
(C3N3S3)2For regular octahedron pattern, 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, appreciation condition and embodiment 1 are investigated by model reaction of photodissociation aquatic products hydrogen
Identical, illumination 3 hours, hydrogen-producing speed is 11.5 mMs of catalyst per hour per gram.
Embodiment 7
According to four water cadmium nitrate in reactant mixture：The mol ratio of trithiocyanuric acid trisodium is 1:[1.33], 4.63 are weighed
Gram four water cadmium nitrates are added in 200 ml deionized waters, stirring and dissolving；Weigh 4.85 grams of trithiocyanuric acid trisodiums and add 200 millis
Rise in deionized water, stirring and dissolving.Then the sodium solution of trithiocyanuric acid three is slowly dropped in nitric acid cadmium solution at room temperature, dripped
Add and continue to stir 48 hours after finishing.Centrifuge, wash according to a conventional method, drying and being calcined to obtain buff powder.Using X-ray
Powder diffractometer, SEM etc. is characterized to yellow powder, product be Cd3(C3N3S3)2, ESEM photograph
Piece shows, gained Cd3(C3N3S3)2For regular octahedron pattern, 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, appreciation condition and embodiment 1 are investigated by model reaction of photodissociation aquatic products hydrogen
Identical, illumination 3 hours, hydrogen-producing speed is 11.3 mMs of catalyst per hour per gram.
Embodiment 8
According to two water cadmium acetate in reactant mixture：The mol ratio of trithiocyanuric acid is 1:1, weigh 4.00 gram of two water acetic acid
Cadmium is added in 200 ml deionized waters, stirring and dissolving；Weigh 2.66 grams of trithiocyanuric acids to add in 200 ml deionized waters, stir
Mix dissolving.Then trithiocyanuric acid solution is slowly dropped in cadmium acetate solution at room temperature, continues to stir 24 after completion of dropping
Hour.Centrifuge, wash according to a conventional method, drying and being calcined to obtain buff powder.Using X-ray powder diffraction instrument, scanning electron
Microscope etc. is characterized to yellow powder, product be Cd3(C3N3S3)2, stereoscan photograph shows, gained Cd3
(C3N3S3)2For regular octahedron pattern, 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, appreciation condition and embodiment 1 are investigated by model reaction of photodissociation aquatic products hydrogen
Identical, illumination 3 hours, hydrogen-producing speed is 11.0 mMs of catalyst per hour per gram.
Embodiment 9
According to caddy in reactant mixture：The mol ratio of trithiocyanuric acid tripotassium is 1:[1.67], 2.75 grams of chlorine are weighed
Cadmium is added in 200 ml deionized waters, stirring and dissolving；Weigh 6.49 grams of trithiocyanuric acid tripotassiums and add 200 milliliters of deionizations
In water, stirring and dissolving.Then the potassium solution of trithiocyanuric acid three is slowly dropped in cadmium chloride solution at room temperature, after completion of dropping
Continue to stir 36 hours.Centrifuge, wash according to a conventional method, drying and being calcined to obtain buff powder.Using X-ray powder diffraction
Instrument, SEM etc. is characterized to yellow powder, product be Cd3(C3N3S3)2, stereoscan photograph shows,
Gained Cd3(C3N3S3)2For regular octahedron pattern, 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, appreciation condition and embodiment 1 are investigated by model reaction of photodissociation aquatic products hydrogen
Identical, illumination 3 hours, hydrogen-producing speed is 10.5 mMs of catalyst per hour per gram.
Embodiment 10
According to two water cadmium acetate in reactant mixture：The mol ratio of trithiocyanuric acid trisodium is 1:[0.5], 4.00 grams are weighed
Two water cadmium acetates are added in 200 ml deionized waters, stirring and dissolving；Weigh 1.82 grams of trithiocyanuric acid trisodiums and add 200 milliliters
In deionized water, stirring and dissolving.Then the sodium solution of trithiocyanuric acid three is slowly dropped in cadmium acetate solution at room temperature, be added dropwise
Continue to stir 36 hours after finishing.Centrifuge, wash according to a conventional method, drying and being calcined to obtain buff powder.Using X-ray powder
Last diffractometer, SEM etc. is characterized to yellow powder, product be Cd3(C3N3S3)2, stereoscan photograph
It has been shown that, gained Cd3(C3N3S3)2For regular octahedron pattern, 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, appreciation condition and embodiment 1 are investigated by model reaction of photodissociation aquatic products hydrogen
Identical, illumination 3 hours, hydrogen-producing speed is 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, then adds nine water
Vulcanized sodium, continues to stir at room temperature, controls Cd3(C3N3S3)2Mol ratio with vulcanized sodium is 1:3, stir 12 hours at room temperature.Press
Conventional method centrifugation, deionized water washing, absolute ethyl alcohol washing, dry regular octahedron cadmium sulfide.Catalyst pattern and particle
Size is characterized using Hitachi S-4800 SEM, and sample is true before electron-microscopic analysis test is scanned
Empty metal spraying.Using X-ray powder diffraction instrument, the stereoscan photograph such as SEM is shown, gained cadmium sulfide is positive eight
Face bodily form looks, diameter is about 1-3 microns.
The photocatalytic activity of prepared catalyst, appreciation condition and embodiment 1 are investigated by model reaction of photodissociation aquatic products hydrogen
Identical, illumination 3 hours, hydrogen-producing speed is 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, then adds nine
Water vulcanized sodium, continues to stir at room temperature, controls Cd3(C3N3S3)2Mol ratio with vulcanized sodium is 1:5, stir 24 hours at room temperature.
Centrifugation, deionized water washing, absolute ethyl alcohol washing, dry regular octahedron cadmium sulfide according to a conventional method.Catalyst pattern with
Grain size is characterized using Hitachi S-4800 SEM, and sample is before electron-microscopic analysis test is scanned
Vacuum metal spraying.Using X-ray powder diffraction instrument, the stereoscan photograph such as SEM is shown, gained cadmium sulfide is just
Shape of octahedron, diameter is about 1-3 microns.
The photocatalytic activity of prepared catalyst, appreciation condition and embodiment 1 are investigated by model reaction of photodissociation aquatic products hydrogen
Identical, illumination 3 hours, hydrogen-producing speed is 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, then adds sulphur
Change potassium, continue to stir at room temperature, control Cd3(C3N3S3)2Mol ratio with potassium sulfide is 1:4, stir 36 hours at room temperature.By normal
The centrifugation of rule method, deionized water washing, absolute ethyl alcohol washing, dry regular octahedron cadmium sulfide.Catalyst pattern and particle are big
Small use Hitachi S-4800 SEM is characterized, and sample is being scanned electron-microscopic analysis test initial vacuum
Metal spraying.Using X-ray powder diffraction instrument, the stereoscan photograph such as SEM is shown, gained cadmium sulfide is positive octahedral
Bodily form looks, diameter is about 1-3 microns.
The photocatalytic activity of prepared catalyst, appreciation condition and embodiment 1 are investigated by model reaction of photodissociation aquatic products hydrogen
Identical, illumination 3 hours, hydrogen-producing speed is 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, then adds vulcanization
Potassium, continues to stir at room temperature, controls Cd3(C3N3S3)2Mol ratio with potassium sulfide is 1:6, stir 12 hours at room temperature.Routinely
Method centrifugation, deionized water washing, absolute ethyl alcohol washing, dry regular octahedron cadmium sulfide.Catalyst pattern and granular size
Characterized using Hitachi S-4800 SEM, sample is being scanned electron-microscopic analysis test initial vacuum spray
Gold.Using X-ray powder diffraction instrument, the stereoscan photograph such as SEM is shown, gained cadmium sulfide is regular octahedron
Pattern, diameter is about 1-3 microns.
The photocatalytic activity of prepared catalyst, appreciation condition and embodiment 1 are investigated by model reaction of photodissociation aquatic products hydrogen
Identical, illumination 3 hours, hydrogen-producing speed is 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, then adds sulphur
Change ammonium, continue to stir at room temperature, control Cd3(C3N3S3)2Mol ratio with ammonium sulfide is 1:4, stir 48 hours at room temperature.By normal
The centrifugation of rule method, deionized water washing, absolute ethyl alcohol washing, dry regular octahedron cadmium sulfide.Catalyst pattern and particle are big
Small use Hitachi S-4800 SEM is characterized, and sample is being scanned electron-microscopic analysis test initial vacuum
Metal spraying.Using X-ray powder diffraction instrument, the stereoscan photograph such as SEM is shown, gained cadmium sulfide is positive octahedral
Bodily form looks, diameter is about 1-3 microns.
The photocatalytic activity of prepared catalyst, appreciation condition and embodiment 1 are investigated by model reaction of photodissociation aquatic products hydrogen
Identical, illumination 3 hours, hydrogen-producing speed is 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, then adds sulphur
Change ammonium, continue to stir at room temperature, control Cd3(C3N3S3)2Mol ratio with ammonium sulfide is 1:5, stir 24 hours at room temperature.By normal
The centrifugation of rule method, deionized water washing, absolute ethyl alcohol washing, dry regular octahedron cadmium sulfide.Catalyst pattern and particle are big
Small use Hitachi S-4800 SEM is characterized, and sample is being scanned electron-microscopic analysis test initial vacuum
Metal spraying.Using X-ray powder diffraction instrument, the stereoscan photograph such as SEM is shown, gained cadmium sulfide is positive octahedral
Bodily form looks, diameter is about 1-3 microns.
The photocatalytic activity of prepared catalyst, appreciation condition and embodiment 1 are investigated by model reaction of photodissociation aquatic products hydrogen
Identical, illumination 3 hours, hydrogen-producing speed is 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, appreciation condition is same as Example 1, illumination 3 hours, and hydrogen-producing speed is 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 mol ratio of nine water vulcanized sodium is 1:
1, weigh 4.63 gram of four water cadmium nitrate and add in 200 ml deionized waters, stirring and dissolving；Weigh nine water vulcanized sodium and add 200 millis
Rise in deionized water, stirring and dissolving.Then sodium sulfide solution is slowly dropped in nitric acid cadmium solution at room temperature, after completion of dropping
Continue to stir 24 hours.Centrifuge, wash according to a conventional method, dry graininess cadmium sulfide.Its pattern is used with granular size
Hitachi S-4800 SEM is characterized, as shown in Figure 4.
The photocatalytic activity of prepared catalyst, appreciation condition and embodiment 1 are investigated by model reaction of photodissociation aquatic products hydrogen
Identical, illumination 3 hours, hydrogen-producing speed is 4.6 mMs of catalyst per hour per gram.
Above-described embodiment and comparative example, which can be seen that regular octahedron cadmium sulfide made from the inventive method, has unique thing
Change architectural 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, is comprised the steps of：
S1, take cadmium salt to be dissolved in deionized water, obtain cadmium salt soln；Trithiocyanuric acid and/or cyclo-trithocyanates are taken to dissolve
In deionized water, settled solution is obtained；Cadmium salt soln is added dropwise at room temperature to settled solution, stirs, centrifuges, wash, system
Obtain 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 add water
Dissolubility sulfide, continues to stir, centrifuges, wash, dry, that is, regular octahedron cadmium sulfide is made.
2. preparation method according to claim 1, it is characterised 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, it is characterised 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, it is characterised in that in step sl, the cadmium salt and trithiocyanuric acid
And/or the mol ratio of cyclo-trithocyanates is 1：[0.5-2].
5. preparation method according to claim 1, it is characterised in that in step sl, the stirring reaction time is 12-
48 hours.
6. preparation method according to claim 1, it is characterised 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, it is characterised 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, it is characterised in that in step s 2, the Cd3(C3N3S3)2With it is water-soluble
Property sulfide mol ratio be 1：[3-6].
9. preparation method according to claim 1, it is characterised in that in step s 2, the stirring reaction time is
0.5-48 hours.
10. regular octahedron cadmium sulfide prepared by a kind of preparation method as described in claim 1-9 any one, is used as photocatalysis
Agent visible ray 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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| CN109289925B (en) * | 2018-09-20 | 2021-03-26 | 西北师范大学 | Preparation and application of graphite-like phase carbon nitride/cadmium organic coordination polymer nanocomposite |
| CN109663599A (en) * | 2018-12-29 | 2019-04-23 | 西安交通大学 | A kind of preparation and its application of the octahedra Cd-Co binary sulfide of pattern size tunable |
| CN111362321A (en) * | 2020-04-10 | 2020-07-03 | 浙江大学 | Preparation method of metal sulfide |
| CN113289664A (en) * | 2021-06-23 | 2021-08-24 | 淮北师范大学 | Schottky junction Sn/Cd3(C3N3S3)2Photocatalyst and preparation method and application thereof |
| CN113289664B (en) * | 2021-06-23 | 2022-03-11 | 淮北师范大学 | Schottky junction Sn/Cd3(C3N3S3)2Photocatalyst and preparation method and application thereof |
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