CN108295903A - A kind of cadmiumsulfide quantum dot-phthalein mountain valley with clumps of trees and bamboo bronzing catalyst and preparation method for hydrogen manufacturing - Google Patents
A kind of cadmiumsulfide quantum dot-phthalein mountain valley with clumps of trees and bamboo bronzing catalyst and preparation method for hydrogen manufacturing Download PDFInfo
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- CN108295903A CN108295903A CN201810076766.6A CN201810076766A CN108295903A CN 108295903 A CN108295903 A CN 108295903A CN 201810076766 A CN201810076766 A CN 201810076766A CN 108295903 A CN108295903 A CN 108295903A
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- cadmium
- quantum dot
- clumps
- trees
- bamboo
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- 229910052980 cadmium sulfide Inorganic materials 0.000 title claims abstract description 94
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 229940116367 cadmium sulfide Drugs 0.000 title claims abstract description 90
- 235000017166 Bambusa arundinacea Nutrition 0.000 title claims abstract description 57
- 235000017491 Bambusa tulda Nutrition 0.000 title claims abstract description 57
- 241001330002 Bambuseae Species 0.000 title claims abstract description 57
- 235000015334 Phyllostachys viridis Nutrition 0.000 title claims abstract description 57
- 239000011425 bamboo Substances 0.000 title claims abstract description 57
- 239000003054 catalyst Substances 0.000 title claims abstract description 44
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 38
- 239000001257 hydrogen Substances 0.000 title claims abstract description 38
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000002096 quantum dot Substances 0.000 claims abstract description 54
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052802 copper Inorganic materials 0.000 claims abstract description 30
- 239000010949 copper Substances 0.000 claims abstract description 30
- 230000003197 catalytic effect Effects 0.000 claims abstract description 25
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 23
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 150000001875 compounds Chemical class 0.000 claims abstract description 18
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 10
- 239000011593 sulfur Substances 0.000 claims abstract description 10
- 150000001661 cadmium Chemical class 0.000 claims abstract description 9
- 239000003960 organic solvent Substances 0.000 claims abstract description 8
- 239000011941 photocatalyst Substances 0.000 claims abstract description 7
- 239000002131 composite material Substances 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 29
- 239000000243 solution Substances 0.000 claims description 28
- 239000007788 liquid Substances 0.000 claims description 23
- 239000006185 dispersion Substances 0.000 claims description 21
- 239000002243 precursor Substances 0.000 claims description 21
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 20
- 239000012086 standard solution Substances 0.000 claims description 17
- 235000019441 ethanol Nutrition 0.000 claims description 15
- 239000012498 ultrapure water Substances 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 9
- 239000011734 sodium Substances 0.000 claims description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- 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 8
- 238000003760 magnetic stirring Methods 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 8
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical group OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 7
- QCUOBSQYDGUHHT-UHFFFAOYSA-L cadmium sulfate Chemical group [Cd+2].[O-]S([O-])(=O)=O QCUOBSQYDGUHHT-UHFFFAOYSA-L 0.000 claims description 7
- 229910000331 cadmium sulfate Inorganic materials 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 239000003995 emulsifying agent Substances 0.000 claims description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 238000000967 suction filtration Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 6
- KPWJBEFBFLRCLH-UHFFFAOYSA-L cadmium bromide Chemical compound Br[Cd]Br KPWJBEFBFLRCLH-UHFFFAOYSA-L 0.000 claims description 6
- OKIIEJOIXGHUKX-UHFFFAOYSA-L cadmium iodide Chemical compound [Cd+2].[I-].[I-] OKIIEJOIXGHUKX-UHFFFAOYSA-L 0.000 claims description 6
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical compound CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- DPLVEEXVKBWGHE-UHFFFAOYSA-N potassium sulfide Chemical compound [S-2].[K+].[K+] DPLVEEXVKBWGHE-UHFFFAOYSA-N 0.000 claims description 6
- ZTSAVNXIUHXYOY-CVBJKYQLSA-L cadmium(2+);(z)-octadec-9-enoate Chemical compound [Cd+2].CCCCCCCC\C=C/CCCCCCCC([O-])=O.CCCCCCCC\C=C/CCCCCCCC([O-])=O ZTSAVNXIUHXYOY-CVBJKYQLSA-L 0.000 claims description 5
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims description 4
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 239000004094 surface-active agent Substances 0.000 claims description 4
- AQMFIGJOWYLUBI-UHFFFAOYSA-N ON=O.[Cd] Chemical compound ON=O.[Cd] AQMFIGJOWYLUBI-UHFFFAOYSA-N 0.000 claims description 3
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 claims description 3
- 229940075417 cadmium iodide Drugs 0.000 claims description 3
- 229960000776 sodium tetradecyl sulfate Drugs 0.000 claims description 3
- UPUIQOIQVMNQAP-UHFFFAOYSA-M sodium;tetradecyl sulfate Chemical compound [Na+].CCCCCCCCCCCCCCOS([O-])(=O)=O UPUIQOIQVMNQAP-UHFFFAOYSA-M 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- BTBJBAZGXNKLQC-UHFFFAOYSA-N ammonium lauryl sulfate Chemical compound [NH4+].CCCCCCCCCCCCOS([O-])(=O)=O BTBJBAZGXNKLQC-UHFFFAOYSA-N 0.000 claims description 2
- 229940063953 ammonium lauryl sulfate Drugs 0.000 claims description 2
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 claims description 2
- PLLZRTNVEXYBNA-UHFFFAOYSA-L cadmium hydroxide Chemical compound [OH-].[OH-].[Cd+2] PLLZRTNVEXYBNA-UHFFFAOYSA-L 0.000 claims description 2
- GWOWVOYJLHSRJJ-UHFFFAOYSA-L cadmium stearate Chemical compound [Cd+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O GWOWVOYJLHSRJJ-UHFFFAOYSA-L 0.000 claims description 2
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims 3
- 235000006408 oxalic acid Nutrition 0.000 claims 1
- 150000003871 sulfonates Chemical class 0.000 claims 1
- 239000004065 semiconductor Substances 0.000 abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 15
- 239000005864 Sulphur Substances 0.000 abstract description 6
- 238000005215 recombination Methods 0.000 abstract description 6
- 238000006555 catalytic reaction Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 5
- CJOBVZJTOIVNNF-UHFFFAOYSA-N cadmium sulfide Chemical compound [Cd]=S CJOBVZJTOIVNNF-UHFFFAOYSA-N 0.000 abstract description 4
- 238000001782 photodegradation Methods 0.000 abstract description 4
- 238000000926 separation method Methods 0.000 abstract description 4
- 238000002604 ultrasonography Methods 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 description 14
- 238000007146 photocatalysis Methods 0.000 description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 11
- 229910052697 platinum Inorganic materials 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- 230000003213 activating effect Effects 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- -1 caddy Chemical compound 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 5
- 238000000354 decomposition reaction Methods 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 239000008364 bulk solution Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000004020 conductor Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229910000510 noble metal Inorganic materials 0.000 description 4
- 239000003426 co-catalyst Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 229910052763 palladium Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- CXKCTMHTOKXKQT-UHFFFAOYSA-N cadmium oxide Inorganic materials [Cd]=O CXKCTMHTOKXKQT-UHFFFAOYSA-N 0.000 description 2
- CFEAAQFZALKQPA-UHFFFAOYSA-N cadmium(2+);oxygen(2-) Chemical compound [O-2].[Cd+2] CFEAAQFZALKQPA-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000007540 photo-reduction reaction Methods 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- RMCKOIXJLDOSOT-UHFFFAOYSA-L cadmium(2+);oxalate Chemical compound [Cd+2].[O-]C(=O)C([O-])=O RMCKOIXJLDOSOT-UHFFFAOYSA-L 0.000 description 1
- GPBYMVOIWCIQFK-KVVVOXFISA-N cadmium;(z)-octadec-9-enoic acid Chemical compound [Cd].CCCCCCCC\C=C/CCCCCCCC(O)=O GPBYMVOIWCIQFK-KVVVOXFISA-N 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- VDQVEACBQKUUSU-UHFFFAOYSA-M disodium;sulfanide Chemical compound [Na+].[Na+].[SH-] VDQVEACBQKUUSU-UHFFFAOYSA-M 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- MOTZDAYCYVMXPC-UHFFFAOYSA-N dodecyl hydrogen sulfate Chemical compound CCCCCCCCCCCCOS(O)(=O)=O MOTZDAYCYVMXPC-UHFFFAOYSA-N 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000013007 heat curing Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 230000008961 swelling Effects 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
- 238000005406 washing 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/18—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms
- B01J31/1805—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms the ligands containing nitrogen
- B01J31/181—Cyclic ligands, including e.g. non-condensed polycyclic ligands, comprising at least one complexing nitrogen atom as ring member, e.g. pyridine
- B01J31/1825—Ligands comprising condensed ring systems, e.g. acridine, carbazole
- B01J31/183—Ligands comprising condensed ring systems, e.g. acridine, carbazole with more than one complexing nitrogen atom, e.g. phenanthroline
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
-
- 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
- B01J35/19—Catalysts containing parts with different compositions
-
- 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
-
- 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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/02—Compositional aspects of complexes used, e.g. polynuclearity
- B01J2531/0238—Complexes comprising multidentate ligands, i.e. more than 2 ionic or coordinative bonds from the central metal to the ligand, the latter having at least two donor atoms, e.g. N, O, S, P
- B01J2531/0241—Rigid ligands, e.g. extended sp2-carbon frameworks or geminal di- or trisubstitution
- B01J2531/025—Ligands with a porphyrin ring system or analogues thereof, e.g. phthalocyanines, corroles
-
- 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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/10—Complexes comprising metals of Group I (IA or IB) as the central metal
- B01J2531/16—Copper
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
- C01B2203/1088—Non-supported catalysts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Combustion & Propulsion (AREA)
- Catalysts (AREA)
Abstract
A kind of cadmiumsulfide quantum dot phthalein mountain valley with clumps of trees and bamboo bronzing catalyst and preparation method for hydrogen manufacturing of the invention, cadmium salt and sulfur-containing compound are dissolved in respectively in organic solvent and are used as cadmium source and sulphur source, cadmium source and sulphur source are mixed react under conditions of ultrasound, water-soluble cadmiumsulfide quantum dot is made, then with after phthalein mountain valley with clumps of trees and bamboo copper hybrid reaction, filtering, drying to obtain have cadmiumsulfide quantum dot/phthalein mountain valley with clumps of trees and bamboo copper composite photocatalyst of high catalytic activity.The present invention is mutually compound using cadmiumsulfide quantum dot and the phthalein mountain valley with clumps of trees and bamboo copper with appropriate bandgap structure, it is migrated mutually between the conduction band and valence band of the two using the energy level official post photo-generated carrier of two kinds of semiconductors, promote the separation of light induced electron and hole, and then improve the catalytic performance of its photodegradation water hydrogen manufacturing, bright sulfur cadmium is overcome during photochemical catalyzing there are the defect that light induced electron and hole-recombination rate are fast, has pushed the practical application of cadmium sulfide material light catalysis property.
Description
Technical field
The present invention relates to photochemical catalyst fields, and in particular to a kind of cadmiumsulfide quantum dot-phthalein mountain valley with clumps of trees and bamboo bronzing for hydrogen manufacturing is urged
Agent and preparation method.
Background technology
Currently, constantly swelling with society, the mankind utilize the exhaustive exploitation of fossil fuel and cause world wide
Interior energy crisis and environmental problem.Therefore, replace non-renewable energy with the clean renewable sources of energy, reduced as possible to non-renewable
The degree of dependence of fossil fuel resource, it is as much as possible to be using solar energy, water energy, wind energy and this kind of regenerative resource of biological energy source
Solve the important measures of current energy crisis.Wherein, water decomposition is produced using inexhaustible clean solar energy
Raw hydrogen effectively will solve energy crisis and environmental pollution two large problems simultaneously.
Photocatalysis chemistry starts from 20th century the seventies, and light-catalyzed reaction is that the catalysis irradiating and cause using light is anti-
It answers, uses light as the energy, pass through catalysis material（Typically nano semiconductor material）Luminous energy is converted into chemical energy, promotionization
Close synthesis or the degradation process of object.Conductor photocatalysis, which decomposes aquatic products hydrogen, to be converted into high density the solar energy of low-density
, storable Hydrogen Energy, be a kind of environmental-friendly green technology.Semiconductor is the semiconductor between conductor and insulator
It can be divided into intrinsic semiconductor, n types semiconductor and P type semiconductors according to the feature of carrier.N type semiconductors are alms givers to partly
Conductor conduction band conveys electronics, and it is more sub structures to be formed with electronics.P type semiconductors are that acceptor receives semiconductor valence-band electrons, shape
It is more sub structures at hole.The principle that conductor photocatalysis decomposes aquatic products hydrogen is when energy is more than or is equivalent to semiconductor band
The light radiation of gap width Eg on the semiconductor when, the electronics in semiconductor valence band is transitted to from valence band and is led by photon excitation
Band then moves to semiconductor surface, and reduction reaction, which occurs, with the proton or hydrone for being adsorbed on surface generates hydrogen.
Cadmium sulfide has relatively narrow band gap and suitable conduction band positions, meets the necessary condition of visible light production hydrogen, visible
One of most common catalyst in the application of light photocatalysis Decomposition aquatic products hydrogen, in numerous cadmium sulfide nano configurations, cadmiumsulfide quantum dot
Since it the characteristics of controlling band structure, can be considered as having the photochemical catalyst of potentiality by changing size, and vulcanize
Cadmium quantum dot is dispersed fabulous in water, can preferably absorb visible light, causes researchers' in photocatalysis hydrogen production field
Extensive concern.However, the band gap of cadmium sulfide intrinsic semiconductor is relatively narrow, only about 2.4 eV, and cadmium sulfide is that direct band gap is partly led
Body, therefore, after the excitation of electronics light is transitted to from valence band on conduction band, light induced electron and hole-recombination rate are fast, therefore pure
The photochemical catalyzing hydrogen generation efficiency of cadmium sulfide itself is lower, limits the practical application of its photocatalysis performance.
Have at present and be used as co-catalyst by noble metals such as supporting Pt, Pd to improve cadmium sulfide photochemical catalyst catalytic activity,
If Chinese invention patent application number 200510022763.7 discloses a kind of preparation method of photocatalyst of platinum-carried cadmium sulfide, will select
It is raw material to select cadmium acetate, and 1h is thermally decomposed in 300 DEG C~600 DEG C temperature ranges and obtains cadmium oxide presoma；Then 200 DEG C~
To cadmium oxide presoma heat cure 4h at a temperature of 400 DEG C, cadmium sulfide is obtained, and by cadmium sulfide with photoreduction met hod carried noble metal platinum
Up to product.There are special nanometer step type looks for vulcanization cadmium surfaces prepared by the invention so that the catalyst can after carrying platinum
Light-exposed photocatalysis Decomposition aquatic products hydrogen activity is greatly improved.But the invention needs the addition of precious metals platinum catalyst, catalysis
Limited efficacy is unfavorable for cost control.
Also have and improve cadmium sulfide photochemical catalyst catalytic activity, such as China by preparing the cadmium sulfide photochemical catalyst of special construction
Application for a patent for invention number 201210479438.3 discloses cadmium sulfide photochemical catalyst and its preparation of a kind of high light catalytic activity
Method using ethyl alcohol as solvent, is added sulphur source and cadmium source, is transferred in autoclave and is heated controlled at 150 DEG C using the hot method of alcohol
Cooled to room temperature after reaction, by the washing of precipitate of gained to efflux be it is neutral after be dried in vacuo again up to hollow micron ball
The cadmium sulfide photochemical catalyst of structure.Although the cadmium sulfide of the hollow micron spherical structure prepared can increase cadmium sulfide surface area, increase
Added carrier transition number, but preparation condition is harsh, light induced electron and the fast root problem of hole-recombination rate without
To solution, catalytic activity is to be improved.
Current-carrying wavelet moves the notable of change after semi-conducting material is mutually gradually decrease to certain critical dimension from body, and property is with ruler
Very little presentation regularity variation, the high specific surface area of nano particle can dramatically increase the effect of photocatalytic process, and Chinese invention is special
Sharp application number 201410191162.8 discloses a kind of preparation method of cadmiumsulfide quantum dot, uses carboxylic acid cadmium as cadmium source, uses
(TMS)2S synthesizes CdS quantum dot as sulphur source, but the minimum surface energy of CdS quantum dot grain size is larger, extremely unstable, easily
Reunite, influences catalytic effect.
It is mixed in the compound organic photoelectrical material that inorganic-quantum-dot is formed into organic material, carrier is not only with jump
Mode is transmitted, and can also be transmitted between different materials in a manner of electronics transfer, and light induced electron and hole-recombination speed can be reduced
Rate.Therefore, a kind of cadmiumsulfide quantum dot and organic matter composite catalyst are developed, is to improve CdS quantum dot light hydrogen production by water decomposition
Another new way of catalytic.
Invention content
It is limited during photochemical catalyzing there are light induced electron and hole-recombination rate are fast for bright sulfur cadmium
The shortcomings that practical application of its photocatalysis performance.The present invention is using cadmiumsulfide quantum dot and with the phthalein mountain valley with clumps of trees and bamboo copper of appropriate bandgap structure
It is mutually compound, it is migrated mutually, is promoted between the conduction band and valence band of the two using the energy level official post photo-generated carrier of two kinds of semiconductors
The separation of light induced electron and hole, and then improve the catalytic performance of its photodegradation water hydrogen manufacturing.
To solve the above problems, the present invention uses following technical scheme：
A kind of preparation method of cadmiumsulfide quantum dot-phthalein mountain valley with clumps of trees and bamboo bronzing catalyst for hydrogen manufacturing, is characterized in that：It specifically includes following
Step：
（1）Cadmium salt and sulfur-containing compound are added in organic solvent, the quality of the cadmium salt and sulfur-containing compound and organic solvent
Than being 1.35:1.29-3.65:20-30 obtains evenly dispersed mixed solution after ultrasonic agitation, obtains precursor solution；
（2）Precursor solution is mixed with high purity water and surfactant, the precursor solution and high purity water and surface-active
The mass ratio of agent is 21.6-30.6:16.8-23.5:Then 0.22-0.30 carries out hydro-thermal reaction, hydrothermal temperature 160-
220 DEG C, hydro-thermal soaking time is 5-10 hours, then naturally cools to room temperature, obtains water-soluble cadmiumsulfide quantum dot dispersion liquid；
（3）500mg/L phthalein mountain valley with clumps of trees and bamboo copper standard solution is prepared, institute is slowly added into the water-soluble cadmiumsulfide quantum dot dispersion liquid
Standard solution is stated, acetylacetone,2,4-pentanedione and emulsifier, the phthalein mountain valley with clumps of trees and bamboo copper standard solution and the cadmium quantum dot dispersion liquid are added later
Volume ratio is 0.35-0.42:1.38,2-5 hours hybrid reactions are stirred on magnetic stirring apparatus at 35-40 DEG C, are passed through after cooling
Filtering cleaning, low temperature drying obtain cadmiumsulfide quantum dot/phthalein mountain valley with clumps of trees and bamboo copper composite photocatalyst of high catalytic activity.
Preferably, the cadmium salt be cadmium sulfate, caddy, cadmium nitrate, cadmium stearate, cadmium iodide, cadmium bromide, cadmium acetate,
The combination of one or more of cadmium oxalate, cadmium oleate, tetradecylic acid cadmium, nitrous acid cadmium, cadmium hydroxide.
Preferably, the sulfur-containing compound is one or both of thiocarbamide, vulcanized sodium, ammonium sulfide, potassium sulfide, ethyl mercaptan
Above combination.
Preferably, the organic solvent is one kind in ethyl alcohol, methanol, ether, acetone.
Preferably, the ultrasonic power is 3-10kW, mixing speed 200-400r/min, mixing time 1-2h.
Preferably, the surfactant is lauryl sodium sulfate, neopelex, dodecyl sulphate
The combination of one or more of sodium, dodecyl sodium sulfate, ammonium lauryl sulfate and sodium tetradecyl sulfate
Preferably, step（3）Described in filter method to use filtered off with suction, the speed of suction filtration be 16-43mL/h.
Preferably, step（3）Described in low temperature drying condition be under 2-50Pa environment under low pressure, dry 1-5 is small at 50-65 DEG C
When.
In addition a kind of cadmiumsulfide quantum dot-phthalein mountain valley with clumps of trees and bamboo bronzing catalyst is provided, be prepared by the above method, the cadmium sulfide
Quantum dot-phthalein mountain valley with clumps of trees and bamboo bronzing catalyst particle size is 20-150nm, and cadmium sulfide molar content is 52-85%.
In order to overcome bright sulfur cadmium during photochemical catalyzing there are light induced electron and hole-recombination rate are fast, limit
The shortcomings that having made the practical application of its photocatalysis performance has be used as co-catalyst by noble metals such as supporting Pt, Pd to carry at present
High-sulfur cadmium photochemical catalyst catalytic activity, needs the addition of precious metals platinum catalyst, and catalytic efficiency is limited, is unfavorable for cost control
System, and improve cadmium sulfide photochemical catalyst catalytic activity, but preparation condition by preparing the cadmium sulfide photochemical catalyst of special construction
Harshness, catalytic activity are to be improved.In consideration of it, a kind of cadmiumsulfide quantum dot-phthalein mountain valley with clumps of trees and bamboo bronzing catalyst for hydrogen manufacturing of the invention
And preparation method, it is used as cadmium source and sulphur source its main feature is that first cadmium salt and sulfur-containing compound are dissolved in respectively in organic solvent, by cadmium
Source and sulphur source, which mix react under conditions of ultrasound, forms presoma；High purity water is added in the presoma of formation, contains table
Water-soluble cadmiumsulfide quantum dot is made in the reactant aqueous solution of face activating agent.Then phthalein mountain valley with clumps of trees and bamboo copper is being added to water-soluble cadmium sulfide amount
After son point hybrid reaction, filtering, drying to obtain have cadmiumsulfide quantum dot/compound photocatalysis of phthalein mountain valley with clumps of trees and bamboo copper of high catalytic activity
Agent.The present invention is mutually compound using cadmiumsulfide quantum dot and the phthalein mountain valley with clumps of trees and bamboo copper with appropriate bandgap structure, utilizes the energy of two kinds of semiconductors
Grade official post photo-generated carrier migrates mutually between the conduction band and valence band of the two, promotes the separation of light induced electron and hole, in turn
The catalytic performance for improving its photodegradation water hydrogen manufacturing has pushed cadmiumsulfide quantum dot photocatalysis performance practical application.
Cadmiumsulfide quantum dot/phthalein mountain valley with clumps of trees and bamboo bronzing catalyst prepared by the present invention carries out test comparison with cadmiumsulfide quantum dot,
The present invention has a clear superiority as shown in table 1 under the conditions of identical contact resistance.
Table 1：
| The present invention | Cadmiumsulfide quantum dot | |
| Degradation efficiency % | ≥96.4 | ≥78.1 |
| Hydrogen generation efficiency（umol/h） | ≥659 | ≥336 |
The present invention provides a kind of cadmiumsulfide quantum dot/phthalein mountain valley with clumps of trees and bamboo bronzing catalyst and preparation method for hydrogen manufacturing, with the prior art
It compares, the feature and excellent effect protruded is：
1, the present invention is mutually compound using cadmiumsulfide quantum dot and the phthalein mountain valley with clumps of trees and bamboo copper with appropriate bandgap structure, prepares cadmium sulfide quantum
Point-phthalein mountain valley with clumps of trees and bamboo bronzing catalyst is mutual between the conduction band and valence band of the two using the energy level official post photo-generated carrier of two kinds of semiconductors
Migration, promotes the separation of light induced electron and hole, and then improves the catalytic performance of its photodegradation water hydrogen manufacturing.
2, cadmiumsulfide quantum dot-phthalein mountain valley with clumps of trees and bamboo bronzing catalyst prepared by the present invention is had excellent performance in practical applications, compared with bright sulfur
Cadmium quantum dot greatly improves in terms of catalytic activity and cyclical stability.
3, the present invention does not need the noble metals such as supporting Pt, Pd can obtain good hydrogen generation efficiency as co-catalyst, system
Preparation Method is simple, of low cost, can synthesize on a large scale.
Specific implementation mode
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
（1）Cadmium sulfate and thiocarbamide are added in ethyl alcohol, the cadmium sulfate and the mass ratio of thiocarbamide and ethyl alcohol are 1.35: 3.65:
20, ultrasonic power 10kW, mixing speed 200r/min, mixing time 1h are obtained after ultrasonic agitation evenly dispersed mixed
Solution is closed, precursor solution is obtained；
（2）Precursor solution is mixed with high purity water and lauryl sodium sulfate, the precursor solution and high purity water and surface
The mass ratio of activating agent is 21.6: 23.5 :0.22, hydro-thermal reaction is then carried out, hydrothermal temperature is 160 DEG C, hydro-thermal
Soaking time is 10 hours, then naturally cools to room temperature, obtains water-soluble cadmiumsulfide quantum dot dispersion liquid；
（3）500mg/L phthalein mountain valley with clumps of trees and bamboo copper standard solution is prepared, institute is slowly added into the water-soluble cadmiumsulfide quantum dot dispersion liquid
State standard solution, it is backward per 0.3ml acetylacetone,2,4-pentanediones being added in bulk solution and 0.2gOP emulsifiers, the phthalein mountain valley with clumps of trees and bamboo copper standard are molten
The volume ratio of liquid and the cadmium quantum dot dispersion liquid is 0.35:1.38, it stirs 2 hours and mixes on magnetic stirring apparatus at 35 DEG C
Reaction, by filtered off with suction after cooling, the speed of suction filtration is 43mL/h, after ethyl alcohol and deionized water cleaning, 2Pa environment under low pressure
Under, cadmiumsulfide quantum dot/phthalein mountain valley with clumps of trees and bamboo copper composite photocatalyst that low temperature drying drying obtains high catalytic activity in 5 hours at 50- DEG C,
The cadmiumsulfide quantum dot-phthalein mountain valley with clumps of trees and bamboo bronzing catalyst particle size is 20nm, and cadmium sulfide molar content is 52%.
Embodiment 2
（1）Cadmium sulfate, caddy, cadmium nitrate, vulcanized sodium mixture are added in ethyl alcohol, cadmium sulfate, caddy, cadmium nitrate mixing
The mass ratio of object and vulcanized sodium and ethyl alcohol is 1.5: 3.65:30, ultrasonic power 5kW, mixing speed 300r/min, stirring
Time is 1h, and evenly dispersed mixed solution is obtained after ultrasonic agitation, obtains precursor solution；
（2）Precursor solution is mixed with high purity water and lauryl sodium sulfate, the precursor solution and high purity water and surface
The mass ratio of activating agent is 25: 16.8:0.25, hydro-thermal reaction is then carried out, hydrothermal temperature is 180 DEG C, hydro-thermal heat preservation
Time is 7 hours, then naturally cools to room temperature, obtains water-soluble cadmiumsulfide quantum dot dispersion liquid；
（3）500mg/L phthalein mountain valley with clumps of trees and bamboo copper standard solution is prepared, institute is slowly added into the water-soluble cadmiumsulfide quantum dot dispersion liquid
State standard solution, it is backward per 0.35ml acetylacetone,2,4-pentanediones and 0.3gOP emulsifiers, the phthalein mountain valley with clumps of trees and bamboo copper standard are added in bulk solution
The volume ratio of solution and the cadmium quantum dot dispersion liquid is 0.39:1.38, it is stirred 2.5 hours on magnetic stirring apparatus at 38 DEG C
Hybrid reaction, by filtered off with suction after cooling, the speed of suction filtration is 18mL/h, and after ethyl alcohol and deionized water cleaning, 10Pa is low
Under pressure ring border, at 55 DEG C low temperature drying dry obtain high catalytic activity within 1.5 hours cadmiumsulfide quantum dot/compound light of phthalein mountain valley with clumps of trees and bamboo copper
Catalyst, the cadmiumsulfide quantum dot-phthalein mountain valley with clumps of trees and bamboo bronzing catalyst particle size are 50nm, and cadmium sulfide molar content is 65%.
Embodiment 3
（1）Cadmium oleate and potassium sulfide are added in ether, the cadmium oleate and the mass ratio of potassium sulfide and ether are 1.35:
1.35:24, ultrasonic power 7kW, mixing speed 300r/min, mixing time 1h are obtained after ultrasonic agitation evenly dispersed
Mixed solution, obtain precursor solution；
（2）Precursor solution is mixed with high purity water and lauryl sodium sulfate, the precursor solution and high purity water and surface
The mass ratio of activating agent is 21.6: 23.5 :0.22, hydro-thermal reaction is then carried out, hydrothermal temperature is 160 DEG C, hydro-thermal
Soaking time is 10 hours, then naturally cools to room temperature, obtains water-soluble cadmiumsulfide quantum dot dispersion liquid；
（3）500mg/L phthalein mountain valley with clumps of trees and bamboo copper standard solution is prepared, institute is slowly added into the water-soluble cadmiumsulfide quantum dot dispersion liquid
State standard solution, it is backward per 0.3ml acetylacetone,2,4-pentanediones being added in bulk solution and 0.2gOP emulsifiers, the phthalein mountain valley with clumps of trees and bamboo copper standard are molten
The volume ratio of liquid and the cadmium quantum dot dispersion liquid is 0.35:1.38, it stirs 2 hours and mixes on magnetic stirring apparatus at 35 DEG C
Reaction, by filtered off with suction after cooling, the speed of suction filtration is 16mL/h, after ethyl alcohol and deionized water cleaning, 20Pa low-voltage rings
Under border, at 55 DEG C low temperature drying dry obtain high catalytic activity within 3 hours cadmiumsulfide quantum dot/compound photocatalysis of phthalein mountain valley with clumps of trees and bamboo copper
Agent, the cadmiumsulfide quantum dot-phthalein mountain valley with clumps of trees and bamboo bronzing catalyst particle size are 100nm, and cadmium sulfide molar content is 75%.
Embodiment 4
（1）Cadmium oleate and vulcanized sodium, potassium sulfide mixture are added in ethyl alcohol, nitrous acid cadmium and vulcanized sodium, potassium sulfide mixture
It is 1.5 with the mass ratio of vulcanized sodium and ethyl alcohol: 3.65:28, ultrasonic power 6kW, mixing speed 280r/min, when stirring
Between be 1h, evenly dispersed mixed solution is obtained after ultrasonic agitation, obtains precursor solution；
（2）Precursor solution is mixed with high purity water and lauryl sodium sulfate, the precursor solution and high purity water and surface
The mass ratio of activating agent is 30.3: 26.8:0.28, hydro-thermal reaction is then carried out, hydrothermal temperature is 200 DEG C, and hydro-thermal is protected
The warm time is 9 hours, then naturally cools to room temperature, obtains water-soluble cadmiumsulfide quantum dot dispersion liquid；
（3）500mg/L phthalein mountain valley with clumps of trees and bamboo copper standard solution is prepared, institute is slowly added into the water-soluble cadmiumsulfide quantum dot dispersion liquid
State standard solution, it is backward per 0.35ml acetylacetone,2,4-pentanediones and 0.3gOP emulsifiers, the phthalein mountain valley with clumps of trees and bamboo copper standard are added in bulk solution
The volume ratio of solution and the cadmium quantum dot dispersion liquid is 0.42:1.38, it stirs 4 hours and mixes on magnetic stirring apparatus at 32 DEG C
Reaction is closed, by filtered off with suction after cooling, the speed of suction filtration is 35mL/h, after ethyl alcohol and deionized water cleaning, 45Pa low pressure
Under environment, cadmiumsulfide quantum dot/compound light of phthalein mountain valley with clumps of trees and bamboo copper that low temperature drying drying obtains high catalytic activity in 4.5 hours at 58 DEG C is urged
Agent, the cadmiumsulfide quantum dot-phthalein mountain valley with clumps of trees and bamboo bronzing catalyst particle size are 150nm, and cadmium sulfide molar content is 85%.
Embodiment 5
（1）Cadmium sulfate, cadmium iodide, cadmium bromide and ethyl mercaptan are added in acetone, the cadmium salt and sulfur-containing compound with it is organic molten
The mass ratio of agent is 1.35: 2.65:21, ultrasonic power 8kW, mixing speed 380r/min, mixing time 1.7h surpass
Evenly dispersed mixed solution is obtained after sound stirring, obtains precursor solution；
（2）Precursor solution is mixed with high purity water and sodium tetradecyl sulfate, the precursor solution and high purity water and surface
The mass ratio of activating agent is 23: 18.5:0.27, hydro-thermal reaction is then carried out, hydrothermal temperature is 180 DEG C, hydro-thermal heat preservation
Time is 9 hours, then naturally cools to room temperature, obtains water-soluble cadmiumsulfide quantum dot dispersion liquid；
（3）500mg/L phthalein mountain valley with clumps of trees and bamboo copper standard solution is prepared, institute is slowly added into the water-soluble cadmiumsulfide quantum dot dispersion liquid
Standard solution is stated, acetylacetone,2,4-pentanedione and emulsifier, the phthalein mountain valley with clumps of trees and bamboo copper standard solution and the cadmium quantum dot dispersion liquid are added later
Volume ratio is 0.40:1.38, stir 4 hours hybrid reactions on magnetic stirring apparatus at 39 DEG C, it is cooling after by filtered off with suction,
The speed of suction filtration is 36mL/h, after ethyl alcohol and deionized water cleaning, under 35Pa environment under low pressure, and low temperature drying drying 3 at 52 DEG C
Hour obtains cadmiumsulfide quantum dot/phthalein mountain valley with clumps of trees and bamboo copper composite photocatalyst of high catalytic activity, the cadmiumsulfide quantum dot-phthalein mountain valley with clumps of trees and bamboo copper
Photochemical catalyst grain size is 60nm, and cadmium sulfide molar content is 68%.
Comparative example 1
Take the oxidation cadmium dust of 0.4mmol, the oleic acid of 0.65mmol and the octadecylene of 3.787mL, nitrogen protection condition
Under be heated to 250 DEG C to oxidation cadmium dusts dissolving, be cooled to 80 DEG C, be configured to oleic acid cadmium solution, be in light yellow transparent solution,
Then the octadecylene solution for taking (TMS) 2 S of a concentration of 0.1 mol/Ls of 0.5mL, is injected into above-mentioned 80 DEG C of oil
Sour cadmium solution reacts 5 minutes, the CdS quantum dots of a diameter of 4.1nm is prepared.
By the photocatalyst applications of the preparation in embodiment 1-5 and comparative example 1 in Photocatalyzed Hydrogen Production reaction, 10- is weighed
50 mg embodiments 1-5 and the photochemical catalyst in comparative example, are dispersed in 40-80 mL distilled water, are then respectively adding
Na2SO 3And Na2S is as photocatalysis sacrifice agent, under magnetic stirring, uses 300 W xenon lamps as visible light source, carries out photo-reduction
Hydrogen experiment is produced in water decomposition, and reacting space same time carries out a test sample, each sample is carried out continuously 3 production hydrogen analyses, uses gas
Phase chromatography carries out qualitative analysis, determines the content of product, as shown in table 2.As can be seen from the table, the cadmium sulfide that prepared by the present invention
Quantum dot-phthalein mountain valley with clumps of trees and bamboo bronzing catalyst has the catalytic activity excellent compared with cadmiumsulfide quantum dot, and hydrogen-producing speed is cadmiumsulfide quantum dot
About 2 times, by light degradation three times recycle after, degradation efficiency still maintains higher level.
Table 2
| Sample | Load capacity % | Hydrogen generation efficiency（umol/h） | Degradation efficiency（umol/h） | Recycle 3 degradation efficiencies（%） |
| Embodiment 1 | 0.1 | 642 | 96.5 | 95.7 |
| Embodiment 2 | 0.5 | 651 | 96.8 | 95.9 |
| Embodiment 3 | 1.0 | 659 | 97.3 | 96.8 |
| Embodiment 4 | 1.5 | 640 | 96.4 | 95.5 |
| Embodiment 5 | 3.0 | 632 | 96.7 | 95.0 |
| Comparative example 1 | 1.0 | 336 | 78.1 | 65.2 |
Claims (9)
1. a kind of preparation method of cadmiumsulfide quantum dot-phthalein mountain valley with clumps of trees and bamboo bronzing catalyst for hydrogen manufacturing, which is characterized in that specifically include
Following steps：
（1）Cadmium salt and sulfur-containing compound are added in organic solvent, the quality of the cadmium salt and sulfur-containing compound and organic solvent
Than being 1.35:1.29-3.65:20-30 obtains evenly dispersed mixed solution after ultrasonic agitation, obtains precursor solution；
（2）Precursor solution is mixed with high purity water and surfactant, the precursor solution and high purity water and surface-active
The mass ratio of agent is 21.6-30.6:16.8-23.5:Then 0.22-0.30 carries out hydro-thermal reaction, hydrothermal temperature 160-
220 DEG C, hydro-thermal soaking time is 5-10 hours, then naturally cools to room temperature, obtains water-soluble cadmiumsulfide quantum dot dispersion liquid；
（3）500mg/L phthalein mountain valley with clumps of trees and bamboo copper standard solution is prepared, institute is slowly added into the water-soluble cadmiumsulfide quantum dot dispersion liquid
Standard solution is stated, acetylacetone,2,4-pentanedione and emulsifier, the phthalein mountain valley with clumps of trees and bamboo copper standard solution and the cadmium quantum dot dispersion liquid are added later
Volume ratio is 0.35-0.42:1.38,2-5 hours hybrid reactions are stirred on magnetic stirring apparatus at 35-40 DEG C, are passed through after cooling
Filtering cleaning, low temperature drying obtain cadmiumsulfide quantum dot/phthalein mountain valley with clumps of trees and bamboo copper composite photocatalyst of high catalytic activity.
2. a kind of preparation method of cadmiumsulfide quantum dot-phthalein mountain valley with clumps of trees and bamboo bronzing catalyst for hydrogen manufacturing according to claim 1,
It is characterized in that, the cadmium salt is cadmium sulfate, caddy, cadmium nitrate, cadmium stearate, cadmium iodide, cadmium bromide, cadmium acetate, oxalic acid
The combination of one or more of cadmium, cadmium oleate, tetradecylic acid cadmium, nitrous acid cadmium, cadmium hydroxide.
3. a kind of preparation method of cadmiumsulfide quantum dot-phthalein mountain valley with clumps of trees and bamboo bronzing catalyst for hydrogen manufacturing according to claim 1,
It is characterized in that, the sulfur-containing compound is one or more of thiocarbamide, vulcanized sodium, ammonium sulfide, potassium sulfide, ethyl mercaptan
Combination.
4. a kind of preparation method of cadmiumsulfide quantum dot-phthalein mountain valley with clumps of trees and bamboo bronzing catalyst for hydrogen manufacturing according to claim 1,
It is characterized in that, the organic solvent is one kind in ethyl alcohol, methanol, ether, acetone.
5. a kind of preparation method of cadmiumsulfide quantum dot-phthalein mountain valley with clumps of trees and bamboo bronzing catalyst for hydrogen manufacturing according to claim 1,
It is characterized in that, the ultrasonic power is 3-10kW, mixing speed 200-400r/min, mixing time 1-2h.
6. a kind of preparation method of cadmiumsulfide quantum dot-phthalein mountain valley with clumps of trees and bamboo bronzing catalyst for hydrogen manufacturing according to claim 1,
It is characterized in that, the surfactant is lauryl sodium sulfate, neopelex, lauryl sodium sulfate, ten
The combination of one or more of dialkyl sulfonates, ammonium lauryl sulfate and sodium tetradecyl sulfate.
7. a kind of preparation method of cadmiumsulfide quantum dot-phthalein mountain valley with clumps of trees and bamboo bronzing catalyst for hydrogen manufacturing according to claim 1,
It is characterized in that, step（3）Described in filter method to use filtered off with suction, the speed of suction filtration be 16-43mL/h.
8. a kind of preparation method of cadmiumsulfide quantum dot-phthalein mountain valley with clumps of trees and bamboo bronzing catalyst for hydrogen manufacturing according to claim 1,
It is characterized in that, step（3）Described in low temperature drying condition be under 2-50Pa environment under low pressure, dry 1-5 hours at 50-65 DEG C.
9. a kind of cadmiumsulfide quantum dot-phthalein mountain valley with clumps of trees and bamboo bronzing for hydrogen manufacturing prepared by the method described in any claims of claim 1-8
Catalyst, which is characterized in that the cadmiumsulfide quantum dot-phthalein mountain valley with clumps of trees and bamboo bronzing catalyst particle size is 20-150nm.
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| CN113563077A (en) * | 2021-07-21 | 2021-10-29 | 广州市尤特新材料有限公司 | Sulfide target material applied to solar cell and preparation method thereof |
| CN113755164A (en) * | 2021-10-14 | 2021-12-07 | 汕头职业技术学院 | Green and environment-friendly cadmium sulfide quantum dot preparation and manufacturing process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113563077A (en) * | 2021-07-21 | 2021-10-29 | 广州市尤特新材料有限公司 | Sulfide target material applied to solar cell and preparation method thereof |
| CN113755164A (en) * | 2021-10-14 | 2021-12-07 | 汕头职业技术学院 | Green and environment-friendly cadmium sulfide quantum dot preparation and manufacturing process |
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