CN115318319B - MoS (MoS) 2 Preparation method of base heterojunction composite catalyst - Google Patents
MoS (MoS) 2 Preparation method of base heterojunction composite catalyst Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 239000003054 catalyst Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000010941 cobalt Substances 0.000 claims abstract description 49
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 49
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 49
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 48
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims abstract description 45
- 230000005291 magnetic effect Effects 0.000 claims abstract description 35
- 239000002243 precursor Substances 0.000 claims abstract description 26
- 238000001354 calcination Methods 0.000 claims abstract description 25
- 239000002070 nanowire Substances 0.000 claims abstract description 21
- 239000002585 base Substances 0.000 claims abstract description 20
- 239000002904 solvent Substances 0.000 claims abstract description 20
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 16
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 14
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 11
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 150000001868 cobalt Chemical class 0.000 claims abstract description 9
- 150000002751 molybdenum Chemical class 0.000 claims abstract description 9
- 238000004729 solvothermal method Methods 0.000 claims abstract description 9
- 239000004202 carbamide Substances 0.000 claims abstract description 6
- 150000003839 salts Chemical class 0.000 claims abstract description 6
- 239000004094 surface-active agent Substances 0.000 claims abstract description 6
- 238000011065 in-situ storage Methods 0.000 claims abstract description 4
- 239000003513 alkali Substances 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 19
- 239000002135 nanosheet Substances 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 229910003321 CoFe Inorganic materials 0.000 claims description 16
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 9
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 8
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 7
- 239000011609 ammonium molybdate Substances 0.000 claims description 7
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 7
- 229940010552 ammonium molybdate Drugs 0.000 claims description 7
- 150000003463 sulfur Chemical class 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 5
- 239000002096 quantum dot Substances 0.000 claims description 5
- 239000011684 sodium molybdate Substances 0.000 claims description 5
- 235000015393 sodium molybdate Nutrition 0.000 claims description 5
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 5
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 5
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 5
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 4
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 4
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 4
- 150000002505 iron Chemical class 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical group OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 claims description 3
- JDBBTVFYDZWUFI-UHFFFAOYSA-K iron(3+) trinitrite Chemical compound [Fe+3].[O-]N=O.[O-]N=O.[O-]N=O JDBBTVFYDZWUFI-UHFFFAOYSA-K 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 229940011182 cobalt acetate Drugs 0.000 claims description 2
- 229940044175 cobalt sulfate Drugs 0.000 claims description 2
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims description 2
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 2
- 239000013043 chemical agent Substances 0.000 claims 1
- 239000008367 deionised water Substances 0.000 description 16
- 229910021641 deionized water Inorganic materials 0.000 description 16
- 238000010438 heat treatment Methods 0.000 description 15
- 238000003756 stirring Methods 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 12
- 239000011259 mixed solution Substances 0.000 description 12
- 238000005303 weighing Methods 0.000 description 10
- 238000001816 cooling Methods 0.000 description 8
- 239000012535 impurity Substances 0.000 description 8
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 230000020477 pH reduction Effects 0.000 description 4
- -1 polytetrafluoroethylene Polymers 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 230000005389 magnetism Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000001632 sodium acetate Substances 0.000 description 3
- 235000017281 sodium acetate Nutrition 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- 238000001132 ultrasonic dispersion Methods 0.000 description 3
- 239000012855 volatile organic compound Substances 0.000 description 3
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000002894 chemical waste Substances 0.000 description 2
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229960003638 dopamine Drugs 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 159000000014 iron salts Chemical class 0.000 description 2
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 101100069231 Caenorhabditis elegans gkow-1 gene Proteins 0.000 description 1
- 239000001263 FEMA 3042 Substances 0.000 description 1
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003302 ferromagnetic material Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
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- 230000001737 promoting effect Effects 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 description 1
- 229940033123 tannic acid Drugs 0.000 description 1
- 235000015523 tannic acid Nutrition 0.000 description 1
- 229920002258 tannic acid Polymers 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
Classifications
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- 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
- B01J27/24—Nitrogen compounds
-
- B01J35/33—
-
- B01J35/39—
-
- 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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
-
- 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
Abstract
The present disclosure discloses a MoS 2 The preparation method of the base heterojunction composite catalyst comprises the following steps: dissolving soluble cobalt salt, soluble ferric salt, an alkali source and a surfactant in a solvent, and preparing a magnetic cobalt ferrite precursor by a one-step solvothermal method; calcining the magnetic cobalt ferrite precursor to obtain cobalt ferrite balls; calcining melamine or urea, ultrasonically acidifying, washing and drying to obtain graphitized carbon nitride nanowires; placing cobalt ferrite balls, soluble molybdenum salt and soluble ferric salt in a solvent, and performing high-temperature hydrothermal synthesis on the mixture; the mixture and the graphitized carbon nitride nanowire are prepared in situ by a one-step hydrothermal method to obtain MoS 2 A base heterojunction composite catalyst.
Description
Technical Field
The present disclosure belongs to the technical field of nanomaterial preparation, and in particular relates to a MoS 2 A preparation method of a base heterojunction composite catalyst.
Background
With the rapid development of social economy in China, the unorganized emission of Volatile Organic Compounds (VOCs), nitrogen oxides, sulfur dioxide, ammonia and the like generated by various large chemical projects have seriously affected the surrounding ecological environment and the healthy life of people, and the problem of atmospheric environmental pollution is increasingly serious, so that the efficient prevention and control of the VOCs and the nitrogen oxides is very important.
The current mainstream technology improves the pollution condition of chemical waste gas to a great extent, but has the defects of high treatment cost, short service life of equipment and catalyst, long catalyst regeneration period, possible secondary pollution and the like. The method is different from the traditional chemical waste gas treatment technology, and the photocatalytic oxidation technology is simple and convenient to operate, green, economical, practical and efficient, and has the core of research and development of high-performance catalysts.
Graphitized carbon nitride (g-C) 3 N 4 ) Is a typical polymer semiconductor, has a narrow band gap (2.7 eV) and a suitable redox potential, however, pure g-C 3 N 4 Electrons on (e) - ) And holes (hours) + ) The rapid recombination of (a) results in a short lifetime of the electrons and thus in pure g-C 3 N 4 Is poor in photocatalytic activity. Then, in order to improve the photocatalytic activity, the catalyst is added to the g-C 3 N 4 The materials are improved in a series, and a great deal of research is mainly focused on developing nano-scale g-C 3 N 4 And synthetic heterostructure composites. In one aspect, 0D g-C 3 N 4 The formation of the nanostructure can improve g-C 3 N 4 On the other hand, the formation of the heterojunction promotes the separation of the photogenerated carriers giving them a higher quantum yield. MoS (MoS) 2 As an ideal semiconductor, it has two-dimensional semiconductor characteristics, and g-C 3 N 4 With well-matched band sites, the heterojunction constructed can provide higher charge mobility. Furthermore, coFe 2 O 4 As a narrow bandgap semiconductor, it can be excited under visible light and has unique magnetic anisotropy, electrical properties, physical and chemical stability and low cost.
Disclosure of Invention
In view of the deficiencies in the prior art, an object of the present disclosure is to provide a MoS 2 Preparation method of base heterojunction composite catalyst and MoS prepared by method 2 The base heterojunction composite catalyst has magnetism and is easy to recycle in the practical application process.
In order to achieve the above object, the present disclosure provides the following technical solutions:
MoS (MoS) 2 The preparation method of the base heterojunction composite catalyst comprises the following steps:
s100: dissolving soluble cobalt salt, soluble ferric salt, an alkali source and a surfactant in a solvent, and preparing a magnetic cobalt ferrite precursor by a one-step solvothermal method;
s200: calcining the magnetic cobalt ferrite precursor to obtain cobalt ferrite balls;
s300: calcining melamine, ultrasonically acidifying, washing and drying to obtain graphitized carbon nitride nanowires;
s400: placing cobalt ferrite balls, soluble molybdenum salt and soluble ferric salt in a solvent, and performing high-temperature hydrothermal synthesis on the mixture;
s500: the mixture and the graphitized carbon nitride nanowire are prepared in situ by a one-step hydrothermal method to obtain MoS 2 A base heterojunction composite catalyst.
Preferably, in step S100, the molar ratio of the soluble cobalt salt to the soluble iron salt is 1:2.
Preferably, the soluble cobalt salts include, but are not limited to: cobalt nitrate, cobalt chloride, cobalt sulfate and cobalt acetate.
Preferably, the iron salts include, but are not limited to: ferric chloride, ferric trichloride, and ferric nitrite.
Preferably, the surfactant includes, but is not limited to: polyethylene glycol, polyvinylpyrrolidone and catechol structure-containing compounds.
Preferably, the solvent includes, but is not limited to: water, ethanol, diethylene glycol and ethylene glycol.
Preferably, the mass ratio of the soluble molybdenum salt to the soluble sulfur salt is 1:2.
Preferably, the soluble molybdenum salts include sodium molybdate and ammonium molybdate.
Preferably, the soluble sulfur salts include thiourea and thioacetamide.
Preferably, in step S200, the calcination temperature of the magnetic cobalt ferrite precursor is 300-600 ℃ and the calcination time is 2-6 hours.
Compared with the prior art, the beneficial effects that this disclosure brought are:
1. zero-dimensional (0D) semiconductor Quantum Dots (QDs) due to their outstanding edge and quantum confinement effects,The unique advantages of large surface area and short effective charge transfer length have made them of great interest in the fields of photoelectrochemistry and photocatalysis. However, in the specific case of photocatalysis, quantum dots suffer from several drawbacks: they are prone to self-aggregation and their high number of surface defects compared to the bulk counterparts make them unstable. In addition, their high photoluminescence results in a high recombination rate of photoexcited electrons and holes. The present disclosure morphologically optimizes graphitized carbon nitride, converts two-dimensional graphitized carbon nitride to zero-dimensional graphitized carbon nitride, and two-dimensional MoS 2 The heterojunction is constructed to make QDs more dispersed and stabilized to significantly improve the photoelectric properties.
2. By introducing cobalt ferrite with unique magnetic anisotropy, the catalyst which is easy to recycle is constructed, so that the catalyst is convenient for practical application.
Drawings
FIG. 1 is a MoS provided in one embodiment of the present disclosure 2 A flow chart of a preparation method of the base heterojunction composite catalyst;
FIG. 2 is a transmission electron microscope image of graphitized carbon nitride quantum dots provided by one embodiment of the present disclosure;
FIG. 3 is a transmission electron microscope image of a molybdenum sulfide nanosheet provided in one embodiment of the present disclosure;
FIG. 4 is a transmission electron microscope image of a cobalt ferrite sphere provided in one embodiment of the present disclosure;
FIG. 5 is a MoS provided in one embodiment of the present disclosure 2 Transmission electron microscopy of the based heterojunction composite catalyst.
Detailed Description
Specific embodiments of the present disclosure will be described in detail below with reference to fig. 1 to 5. While specific embodiments of the disclosure are shown in the drawings, it should be understood that the disclosure may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.
It should be noted that certain terms are used throughout the description and claims to refer to particular components. Those of skill in the art will understand that a person may refer to the same component by different names. The specification and claims do not identify differences in terms of components, but rather differences in terms of the functionality of the components. As used throughout the specification and claims, the terms "include" and "comprise" are used in an open-ended fashion, and thus should be interpreted to mean "include, but not limited to. The description hereinafter sets forth the preferred embodiments for carrying out the present disclosure, but is not intended to limit the scope of the disclosure in general, as the description proceeds. The scope of the present disclosure is defined by the appended claims.
For the purposes of promoting an understanding of the embodiments of the disclosure, reference will now be made to the embodiments illustrated in the drawings and specific examples, without the intention of being limiting the embodiments of the disclosure.
In one embodiment, as shown in FIG. 1, the present disclosure provides a magnetically recoverable MoS 2 The preparation method of the base heterojunction composite catalyst comprises the following steps:
s100: dissolving soluble cobalt salt, soluble ferric salt and a surfactant in a solvent, and preparing a magnetic cobalt ferrite precursor by a one-step solvothermal method;
s200: calcining the magnetic cobalt ferrite precursor to obtain cobalt ferrite balls;
s300: calcining melamine, ultrasonically acidifying, washing and drying to obtain graphitized carbon nitride nanowires;
s400: placing cobalt ferrite balls, soluble molybdenum salt and soluble sulfur salt in a solvent, and performing high-temperature hydrothermal synthesis on the mixture;
s500: the mixture and the graphitized carbon nitride nanowire are prepared in situ by a one-step solvothermal method to obtain MoS 2 A base heterojunction composite catalyst.
In this example, moS prepared by the above method will be 2 The sample of the base heterojunction composite catalyst is dispersed in a container containing aqueous solution, so that the sample is in a suspension state, then the magnet is used for moving on the outer wall of the container, and the attraction of the sample along with the magnet can be clearly observedRapid sedimentation was induced, thereby demonstrating the MoS produced by the present process 2 The base heterojunction composite catalyst has magnetism and is easy to recycle.
The present disclosure will now be described in detail with reference to specific examples.
Example 1:
1. 6m mol of cobalt nitrate, 12m mol of ferric trichloride and 80m mol of sodium acetate are taken as solvents to be added into water, after the cobalt nitrate, the ferric trichloride and the 80m mol of sodium acetate are completely dissolved by magnetic stirring, 5m mol/L of polyethylene glycol is added, and stirring is carried out for 30 minutes again, so that a mixed solution is obtained. Transferring the mixed solution into a reaction kettle with polytetrafluoroethylene as a lining for solvothermal reaction, preserving heat at 200 ℃ for 12 hours, naturally cooling to room temperature to obtain a magnetic cobalt ferrite precursor with solvent impurities on the surface, alternately washing the magnetic cobalt ferrite precursor with ethanol and deionized water for 3-5 times to remove the redundant solvent impurities until the supernatant is transparent, and finally drying in a vacuum oven at 60 ℃ for 12 hours to obtain the magnetic cobalt ferrite precursor.
2. Placing a magnetic cobalt ferrite precursor into a tube furnace, heating to 300 ℃ at a heating rate of 5 ℃/min, and calcining for 2 hours to obtain cobalt ferrite balls; FIG. 4 is a transmission electron microscope image of cobalt ferrite balls, and FIG. 4 shows a spherical morphology with a diameter of about 150nm, and has good crystallinity.
3. Weighing 5g of melamine, placing the melamine into a high-temperature tube furnace, heating to 550 ℃ at a speed of 5 ℃/min under air, and preserving heat for 4 hours; grinding into fine powder, calcining again, heating to 500 ℃ at the speed of 2.5 ℃/min, and preserving heat for 2 hours to obtain the graphitized carbon nitride nano-sheet with two-dimensional dimensions. Then 200mg of two-dimensional graphitized carbon nitride nano-sheets are weighed and placed in a mixed solution composed of 20ml of concentrated sulfuric acid and 20ml of concentrated nitric acid for continuous ultrasonic acidification for 18 hours so as to peel off the graphitized carbon nitride nano-sheets, and then the graphitized carbon nitride nano-wires are obtained through vacuum suction filtration, washing and drying.
4. Weighing 0.2060g of ammonium molybdate and 0.4440g of thiourea, placing into 30ml of deionized water, stirring until the mixture is dissolved, adding 100mg of cobalt ferrite balls, continuously stirring for 30min, placing into a high-pressure reaction kettle, performing hydrothermal reaction at 200 ℃, and keepingNaturally cooling to room temperature after 24 hours, alternately washing with ethanol and deionized water for 3-5 times, and drying in a vacuum oven at 60 ℃ for 12 hours to obtain MoS 2 /CoFe 2 O 4 A composite material.
5. 0.05g MoS was weighed 2 /CoFe 2 O 4 The composite and 0.05g graphitized carbon nitride nanowires were placed in 20ml deionized water, sonicated (for use in dispersing MoS 2 /CoFe 2 O 4 Uniformly dispersing the composite material and the graphitized carbon nitride nanowire) for 1 hour, and then placing the mixture into a reaction kettle at 200 ℃ for hydrothermal reaction for 10 hours to obtain the magnetic recoverable MoS 2 A base heterojunction composite catalyst. FIG. 5 is MoS 2 As can be seen from fig. 5, the cobalt ferrite sphere can be well supported on the molybdenum sulfide nanosheets (graphitized carbon nitride quantum dots on the nanosheets are not clearly seen because graphitized carbon nitride quantum dots are very small in size and are inconsistent with the contrast exhibited by the nanosheets in the electron microscope), due to MoS 2 /CoFe 2 O 4 CoFe in composite material 2 O 4 Is an important ferromagnetic material, also a good semiconductor, and can make the obtained MoS after being compounded 2 The base heterojunction composite catalyst has magnetism.
Example 2:
1. 6m mol of cobalt chloride, 12m mol of ferric chloride and 80m mol of sodium citrate are taken as solvents to be added into ethanol, after being completely dissolved by magnetic stirring, 10m mol/L of polyvinylpyrrolidone (PVP) is added, and stirring is carried out for 30 minutes again, so as to obtain a mixed solution. Transferring the mixed solution into a reaction kettle with polytetrafluoroethylene as a lining for solvothermal reaction, preserving heat at 200 ℃ for 12 hours, naturally cooling to room temperature to obtain a magnetic cobalt ferrite precursor with solvent impurities on the surface, alternately washing the magnetic cobalt ferrite precursor with ethanol and deionized water for 3-5 times to remove the redundant solvent impurities until the supernatant is transparent, and finally drying in a vacuum oven at 60 ℃ for 12 hours to obtain the magnetic cobalt ferrite precursor.
2. And (3) placing the magnetic cobalt ferrite precursor in a tube furnace, heating to 400 ℃ at a heating rate of 5 ℃/min, and calcining for 4 hours to obtain cobalt ferrite balls.
3. Weighing 5g of melamine, placing the melamine into a high-temperature tube furnace, heating to 550 ℃ at a speed of 5 ℃/min under air, and preserving heat for 4 hours; grinding into fine powder, calcining again, heating to 500 ℃ at the speed of 2.5 ℃/min, and preserving heat for 2 hours to obtain the graphitized carbon nitride nano-sheet with two-dimensional dimensions. Then 200mg of two-dimensional graphitized carbon nitride nano-sheets are weighed and placed in a mixed solution composed of 20ml of concentrated sulfuric acid and 20ml of concentrated nitric acid for continuous ultrasonic acidification for 18 hours so as to peel off the graphitized carbon nitride nano-sheets, and then the graphitized carbon nitride nano-wires are obtained through vacuum suction filtration, washing and drying.
4. Weighing 0.2060g of ammonium molybdate and 0.4440g of thiourea, placing into 30ml of deionized water, stirring until the ammonium molybdate and the 0.4440g of thiourea are dissolved, adding 200mg of cobalt ferrite balls, continuously stirring for 30min, placing into a high-pressure reaction kettle, performing hydrothermal reaction at 200 ℃, preserving heat for 24 hours, naturally cooling to room temperature, alternately washing with ethanol and deionized water for 3-5 times, and then drying in a vacuum oven at 60 ℃ for 12 hours to obtain MoS 2 /CoFe 2 O 4 A composite material.
5. Weighing 0.05g to obtain MoS 2 /CoFe 2 O 4 The composite material and 0.1g graphitized carbon nitride nanowire are placed in 20ml deionized water, after ultrasonic dispersion for 1 hour, the composite material and the graphitized carbon nitride nanowire are placed in a reaction kettle at 200 ℃ for hydrothermal reaction for 10 hours, and then the magnetic recyclable MoS 2-based heterojunction composite catalyst is obtained.
Comparative example 1, example 2 was prepared by substituting the soluble cobalt and iron salts of example 1, step 1, with cobalt chloride and iron chloride, adjusting the calcination temperature to 400℃in step 2, adjusting the calcination time to 4 hours, and adjusting the MoS in step 5 2 /CoFe 2 O 4 And the ratio between graphitized carbon nitride nanowires was adjusted to 1:2, and the specific preparation method and operation method were the same as in example 1, and the obtained results were substantially the same as in example 1.
Example 3:
1. 6m mol of cobalt nitrate hexahydrate, 12m mol of ferric nitrite and 80m mol of ammonia water are added into ethylene glycol, after being completely dissolved by magnetic stirring, 15m mol/L of dopamine is added, and stirring is carried out for 30 minutes again, so as to obtain a mixed solution. Transferring the mixed solution into a reaction kettle with polytetrafluoroethylene as a lining for solvothermal reaction, preserving heat at 200 ℃ for 12 hours, naturally cooling to room temperature to obtain a magnetic cobalt ferrite precursor with solvent impurities on the surface, alternately washing the magnetic cobalt ferrite precursor with ethanol and deionized water for 3-5 times to remove the redundant solvent impurities until the supernatant is transparent, and finally drying in a vacuum oven at 60 ℃ for 12 hours to obtain the magnetic cobalt ferrite precursor.
2. And (3) placing the magnetic cobalt ferrite precursor in a tube furnace, heating to 500 ℃ at a heating rate of 5 ℃/min, and calcining for 5 hours to obtain cobalt ferrite balls.
3. Weighing 5g of melamine, placing the melamine into a high-temperature tube furnace, heating to 550 ℃ at a speed of 5 ℃/min under air, and preserving heat for 4 hours; grinding into fine powder, calcining again, heating to 500 ℃ at the speed of 2.5 ℃/min, and preserving heat for 2 hours to obtain the graphitized carbon nitride nano-sheet with two-dimensional dimensions. Then 200mg of two-dimensional graphitized carbon nitride nano-sheets are weighed and placed in a mixed solution composed of 20ml of concentrated sulfuric acid and 20ml of concentrated nitric acid for continuous ultrasonic acidification for 18 hours so as to peel off the graphitized carbon nitride nano-sheets, and then the graphitized carbon nitride nano-wires are obtained through vacuum suction filtration, washing and drying.
4. Weighing 0.2060g of sodium molybdate and 0.4440g of thioacetamide, placing into 30ml of deionized water, stirring until the sodium molybdate and the thioacetamide are dissolved, adding 300mg of cobalt ferrite balls, continuously stirring for 30min, placing into a high-pressure reaction kettle, performing hydrothermal reaction at 200 ℃, preserving heat for 24 hours, naturally cooling to room temperature, alternately washing with ethanol and deionized water for 3-5 times, and then drying in a vacuum oven at 60 ℃ for 12 hours to obtain MoS 2 /CoFe 2 O 4 A composite material.
5. 0.05g MoS was weighed 2 -CoFe 2 O 4 Placing the composite material and 0.2g of graphitized carbon nitride nanowire into 20ml of deionized water, performing ultrasonic dispersion for 1 hour, and then placing into a reaction kettle with the temperature of 200 ℃ for hydrothermal reaction for 10 hours to obtain the magnetic recoverable MoS 2 A base heterojunction composite catalyst.
Comparative example 1, example 3 was performed as in example 1, step 4The soluble molybdenum salt and sulfur salt of (2) are replaced by sodium molybdate and thioacetamide, the calcination temperature in the step (2) is adjusted to 500 ℃, the calcination time is adjusted to 5 hours, and the MoS in the step (5) is adjusted 2 /CoFe 2 O 4 And the ratio between graphitized carbon nitride nanowires was adjusted to 1:4, and the specific preparation method and operation method were the same as in example 1, and the obtained results were substantially the same as in example 1.
Example 4:
1. adding 6m mol of cobalt nitrate hexahydrate, 12m mol of ferric trichloride and 80m mol of sodium acetate into diethylene glycol, stirring by magnetic force to dissolve completely, adding 20m mol/L tannic acid or 3- (4-hydroxyphenyl) propionic acid (the two substances and dopamine belong to compounds containing catechol structures, the compounds can be firmly bonded with metal oxide molecules to modify the surfaces of the compounds, and simultaneously a plurality of hydroxyl groups in the structures can also effectively inhibit the growth of nanocrystals and play a role of surface activation), and stirring again for 30 minutes to obtain a mixed solution. Transferring the mixed solution into a reaction kettle with polytetrafluoroethylene as a lining for solvothermal reaction, preserving heat at 200 ℃ for 12 hours, naturally cooling to room temperature to obtain a magnetic cobalt ferrite precursor with solvent impurities on the surface, alternately washing the magnetic cobalt ferrite precursor with ethanol and deionized water for 3-5 times to remove the redundant solvent impurities until the supernatant is transparent, and finally drying in a vacuum oven at 60 ℃ for 12 hours to obtain the magnetic cobalt ferrite precursor.
2. And (3) placing the magnetic cobalt ferrite precursor in a tube furnace, heating to 300 ℃ at a heating rate of 5 ℃/min, and calcining for 2 hours to obtain cobalt ferrite balls.
3. Weighing 20g of urea, placing the urea into a high-temperature tube furnace, heating to 550 ℃ at a speed of 5 ℃/min under air, and preserving heat for 4 hours to obtain two-dimensional graphitized carbon nitride nano-sheets (urea is a porous agent, ammonia gas is released in a high-temperature calcination process, and loose porous graphitized carbon nitride thin nano-sheets can be obtained through one-time calcination). Then weighing 200mg of graphitized carbon nitride nano-sheets with two-dimensional dimensions, placing the graphitized carbon nitride nano-sheets in a mixed solution consisting of 20ml of concentrated sulfuric acid and 20ml of concentrated nitric acid for 18 hours for continuous ultrasonic acidification, and obtaining graphitized carbon nitride nano-wires through vacuum filtration, washing and drying;
4. weighing 0.2060g of ammonium molybdate and 0.4440g of thiourea, placing into 30ml of deionized water, stirring until the ammonium molybdate and the 0.4440g of thiourea are dissolved, adding 400mg of cobalt ferrite balls, continuously stirring for 30min, placing into a high-pressure reaction kettle, performing hydrothermal reaction at 200 ℃, keeping the temperature for 24 hours, naturally cooling to room temperature, alternately washing with ethanol and deionized water for 3-5 times, and then drying in a vacuum oven at 60 ℃ for 12 hours to obtain a product MoS 2 /CoFe 2 O 4 A composite material.
5. 0.05g MoS was weighed 2 -CoFe 2 O 4 Placing the composite material and 0.3g graphitized carbon nitride nanowire into 20ml deionized water, performing ultrasonic dispersion for 1 hour, and then placing into a reaction kettle at 200 ℃ to react for 10 hours to obtain the magnetic recoverable MoS 2 A base heterojunction composite catalyst.
Comparative example 1, example 3 is a melamine replacement with urea in step 3 of example 1, without a second calcination. MoS in step 5 2 /CoFe 2 O 4 And the ratio between graphitized carbon nitride nanowires was adjusted to 1:6, and the specific preparation method and operation method were the same as in example 1, and the obtained results were substantially the same as in example 1.
In the above examples, the molar ratio of the soluble cobalt salt to the soluble iron salt is fixed to 1:2, and this ratio is determined according to the crystal structure of the magnetic cobalt ferrite to be formed, and experiments prove that when the ratio is larger or smaller, the crystal structure of the magnetic cobalt ferrite cannot be formed.
The foregoing has outlined rather broadly the principles and embodiments of the present disclosure using specific examples that are presented herein to aid in the understanding of the methods of the present disclosure and the core concepts thereof; meanwhile, as those skilled in the art will have variations in the specific embodiments and application scope in light of the ideas of the present disclosure, the present disclosure should not be construed as being limited to the above description.
Claims (10)
1. MoS (MoS) 2 Base heterojunction composite catalysisThe preparation method of the chemical agent comprises the following steps:
s100: dissolving soluble cobalt salt, soluble ferric salt, an alkali source and a surfactant in a solvent, and preparing a magnetic cobalt ferrite precursor by a one-step solvothermal method;
s200: calcining the magnetic cobalt ferrite precursor to obtain cobalt ferrite balls;
s300: calcining melamine or urea to obtain a two-dimensional graphitized carbon nitride nano sheet, ultrasonically acidifying the graphitized carbon nitride nano sheet, and washing and drying to obtain graphitized carbon nitride nano wires;
s400: placing cobalt ferrite balls, soluble molybdenum salt and soluble sulfur salt in a solvent, and performing high-temperature hydrothermal synthesis on MoS 2 /CoFe 2 O 4 A mixture;
s500: the mixture and the graphitized carbon nitride nanowire are prepared in situ by a one-step hydrothermal method to obtain MoS 2 Base heterojunction composite catalyst, the MoS 2 In the base heterojunction composite catalyst, graphitized carbon nitride is loaded on MoS in the shape of quantum dots 2 /CoFe 2 O 4 On the mixture.
2. The process according to claim 1, wherein preferably, in step S100, the molar ratio of the soluble cobalt salt and the soluble iron salt is 1:2.
3. The method of claim 1, wherein the soluble cobalt salt includes, and is not limited to: cobalt nitrate, cobalt chloride, cobalt sulfate and cobalt acetate.
4. The method of claim 1, wherein the iron salt includes, and is not limited to: ferric chloride, ferric trichloride, and ferric nitrite.
5. The method of claim 1, wherein the surfactant includes, and is not limited to: polyethylene glycol, polyvinylpyrrolidone and catechol structure-containing compounds.
6. The method of claim 1, wherein the solvent includes, and is not limited to:
water, ethanol, diethylene glycol and ethylene glycol.
7. The method of claim 1, wherein the mass ratio of the soluble molybdenum salt to the soluble sulfur salt is 1:2.
8. The method of claim 1, wherein the soluble molybdenum salts comprise sodium molybdate and ammonium molybdate.
9. The method of claim 1, wherein the soluble sulfur salts comprise thiourea and thioacetamide.
10. The method of claim 1, wherein in step S200, the calcination temperature of the magnetic cobalt ferrite precursor is 300-600 ℃ and the calcination time is 2-6 hours.
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