CN109999841A - A kind of SnS2/1T-MoS2QDS composite photo-catalyst, preparation method and application - Google Patents
A kind of SnS2/1T-MoS2QDS composite photo-catalyst, preparation method and application Download PDFInfo
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- CN109999841A CN109999841A CN201910357572.8A CN201910357572A CN109999841A CN 109999841 A CN109999841 A CN 109999841A CN 201910357572 A CN201910357572 A CN 201910357572A CN 109999841 A CN109999841 A CN 109999841A
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- 239000002131 composite material Substances 0.000 title claims abstract description 59
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims description 19
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 80
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 80
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 18
- 230000007547 defect Effects 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims description 33
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 32
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 27
- 239000011593 sulfur Substances 0.000 claims description 23
- 229910052717 sulfur Inorganic materials 0.000 claims description 23
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- 150000001875 compounds Chemical class 0.000 claims description 20
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 18
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 17
- 239000012498 ultrapure water Substances 0.000 claims description 17
- 235000019441 ethanol Nutrition 0.000 claims description 13
- 229940126062 Compound A Drugs 0.000 claims description 8
- NLDMNSXOCDLTTB-UHFFFAOYSA-N Heterophylliin A Natural products O1C2COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC2C(OC(=O)C=2C=C(O)C(O)=C(O)C=2)C(O)C1OC(=O)C1=CC(O)=C(O)C(O)=C1 NLDMNSXOCDLTTB-UHFFFAOYSA-N 0.000 claims description 8
- GVPWHKZIJBODOX-UHFFFAOYSA-N dibenzyl disulfide Chemical group C=1C=CC=CC=1CSSCC1=CC=CC=C1 GVPWHKZIJBODOX-UHFFFAOYSA-N 0.000 claims description 8
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- 239000006228 supernatant Substances 0.000 claims description 7
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 7
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims description 6
- 229910004619 Na2MoO4 Inorganic materials 0.000 claims description 6
- 239000005864 Sulphur Substances 0.000 claims description 6
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 6
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 6
- 239000011684 sodium molybdate Substances 0.000 claims description 6
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 6
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 6
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 5
- 239000011609 ammonium molybdate Substances 0.000 claims description 5
- 229940010552 ammonium molybdate Drugs 0.000 claims description 5
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000002351 wastewater Substances 0.000 claims description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 238000013459 approach Methods 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 4
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 claims description 4
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 claims description 4
- 238000012805 post-processing Methods 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 4
- 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 3
- 235000013878 L-cysteine Nutrition 0.000 claims description 3
- 239000004201 L-cysteine Substances 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 238000000527 sonication Methods 0.000 claims description 2
- -1 sulphur compound Chemical class 0.000 claims description 2
- 150000001408 amides Chemical class 0.000 claims 1
- 239000012295 chemical reaction liquid Substances 0.000 claims 1
- 125000000446 sulfanediyl group Chemical group *S* 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 15
- 238000005215 recombination Methods 0.000 abstract description 5
- 230000006798 recombination Effects 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 35
- 230000001699 photocatalysis Effects 0.000 description 20
- 238000002604 ultrasonography Methods 0.000 description 19
- 239000011651 chromium Substances 0.000 description 17
- 238000010531 catalytic reduction reaction Methods 0.000 description 11
- 238000000034 method Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000725 suspension Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000002835 absorbance Methods 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 230000009467 reduction Effects 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- MOZNLPLOAOJYHH-UHFFFAOYSA-N C(C)O.C(C1=CC=CC=C1)SSCC1=CC=CC=C1 Chemical compound C(C)O.C(C1=CC=CC=C1)SSCC1=CC=CC=C1 MOZNLPLOAOJYHH-UHFFFAOYSA-N 0.000 description 2
- XTFPYEOBVLWDDP-UHFFFAOYSA-N CCO.CC(N)=S Chemical compound CCO.CC(N)=S XTFPYEOBVLWDDP-UHFFFAOYSA-N 0.000 description 2
- 229910015667 MoO4 Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- QWUWMCYKGHVNAV-UHFFFAOYSA-N 1,2-dihydrostilbene Chemical group C=1C=CC=CC=1CCC1=CC=CC=C1 QWUWMCYKGHVNAV-UHFFFAOYSA-N 0.000 description 1
- 206010007269 Carcinogenicity Diseases 0.000 description 1
- BWGNESOTFCXPMA-UHFFFAOYSA-N Dihydrogen disulfide Chemical compound SS BWGNESOTFCXPMA-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000007670 carcinogenicity Effects 0.000 description 1
- 231100000260 carcinogenicity Toxicity 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
-
- B01J35/39—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Plasma & Fusion (AREA)
- Optics & Photonics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of SnS2/1T‑MoS2QDS composite photo-catalyst, including the SnS containing S vacancy defect2Nanometer sheet and it is supported on SnS21T-MoS in nanometer sheet2QDS, 1T-MoS2QDS and SnS2Nanometer sheet forms hetero-junctions, and 1T-MoS2The weight accounting of QDS in the composite photocatalyst is 1-3%.Catalyst of the invention has efficiently controlled the quantity of generated S vacancy defect, and the vacancy S of generation can effectively adjust SnS2Band structure, 1T-MoS2QDS and SnS2Nanometer sheet forms hetero-junctions, has consolidated the interface of the two by hydro-thermal reaction.Catalyst of the invention can promote the separation of photo-generate electron-hole pair, reduce the recombination rate of photo-generate electron-hole pair, show higher catalytic activity, have broad application prospect.
Description
Technical field
The present invention relates to catalysis material technical fields, and in particular to a kind of SnS2/1T-MoS2QDS composite photo-catalyst,
Preparation method and application.
Background technique
Cr VI is pollutant common in the waste water of industrial process generation such as leather tanning, plating and chromate production.
Since its toxicity is high, mobility is strong and carcinogenicity, serious threat is produced to human health and water resource.Therefore, water
Effectively removing for middle Cr VI is the most important thing in waste water treatment.
Photocatalitic Technique of Semiconductor is as a kind of efficient, environmental protection and has the water treatment technology of broad prospect of application increasingly
It gets more and more people's extensive concerning.In many semiconductor materials, stannic disulfide is because its is low in cost, nontoxic, spectral response is wide etc.
Advantage and extensive concern by researcher, but SnS2As a kind of photochemical catalyst, there are still some disadvantages, such as light for itself
The disadvantages such as raw Carrier recombination rate is high, visible light utilization efficiency is low, cause its photocatalytic activity low, which greatly limits it to urge in light
The practical application in change field.Therefore, to give full play to SnS2Photocatalysis performance, need to reduce electron-hole recombinations probability, mention
High visible utilization rate.And develop that a kind of spectral response is wide, and photo-generate electron-hole recombination probability is low, reliable and stable light is urged
Agent or composite photo-catalyst are most important.
Summary of the invention
The purpose of the invention is to overcome the problems of the prior art, a kind of SnS is provided2/1T-MoS2QDS complex light is urged
Agent and preparation method thereof.
The first purpose of the invention is to provide a kind of SnS2/1T-MoS2QDS composite photo-catalyst, including contain the vacancy S
The SnS of defect2Nanometer sheet and it is supported on the SnS21T-MoS in nanometer sheet2QDS, the 1T-MoS2The QDS and SnS2
Nanometer sheet forms hetero-junctions, and the 1T-MoS2Weight accounting of the QDS in the composite photo-catalyst is 1-3%.
A second object of the present invention is to provide a kind of SnS2/1T-MoS2The preparation method of QDS composite photo-catalyst, including
Following steps:
Step 1, SnCl4·5H2Hydro-thermal reaction occurs for O and sulfur-containing compound A, and the SnS of the vacancy defect containing S is prepared2It receives
Rice piece;
Step 2, hydro-thermal reaction occurs for molybdate and sulfur-containing compound B, and 1T-MoS is prepared2QDS solution;
Step 3, SnS2Nanometer sheet and 1T-MoS2Hydro-thermal reaction occurs for QDS, and the SnS of the vacancy defect containing S is prepared2/1T-
MoS2QDS composite photo-catalyst.
Preferably, SnS is prepared in step 12Specific step is as follows for nanometer sheet:
By SnCl4·5H2O and citric acid are dissolved in ultrapure water A, and sulfur-containing compound A is then added, and are stirred 1-5h, have been stirred
Hydro-thermal reaction 12h after completion of the reaction by reaction solution centrifugation, washing, dry obtains yellow solid precipitate at 150-180 DEG C after finishing,
The as described SnS2Nanometer sheet;
Wherein, SnCl4·5H2O, citric acid, sulfur-containing compound A, ultrapure water A amount ratio be 1mmol:1mmol:1-
2mmol:8ml.
Preferably, the sulfur-containing compound A is thioacetamide, thiocarbamide, vulcanized sodium or L-cysteine.
Preferably, the molybdate is ammonium molybdate or Na2MoO4·2H2O;The sulfur-containing compound B is thiocarbamide, dibenzyl
Two sulphur or thioacetamide.
Preferably, 1T-MoS is prepared in step 22Specific step is as follows by QDS:
Molybdate is added in ultrapure water B and is ultrasonically treated, molybdic acid saline solution is obtained;
Sulfur-containing compound B is added in ethyl alcohol and is ultrasonically treated, sulfur-containing compound B ethanol solution is obtained;
Sulfur-containing compound B ethanol solution is added in molybdic acid saline solution and is ultrasonically treated, is then lauched at 180-220 DEG C
Thermal response 12-24h, post-processes after completion of the reaction, obtains 1T-MoS2QDS solution;
And when the sulfur-containing compound B is thiocarbamide or thioacetamide, the post-processing approach are as follows: after completion of the reaction will
Reaction solution centrifugation, takes supernatant, obtains 1T-MoS2QDS solution;
When the sulphur compound B is benzyl disulfide, the post-processing approach are as follows: produce black obtained in reaction solution
Object is dispersed in 30mL ultrapure water, its supernatant of centrifuging and taking obtains 1T-MoS2QDS solution;
Molybdate, sulfur-containing compound B, ultrapure water B, ethyl alcohol amount ratio be 1mmol:1-2mmol:30mL:30mL.
Preferably, SnS is prepared in the step 32/1T-MoS2Specific step is as follows for QDS composite photo-catalyst:
By SnS made from step 121T-MoS made from step 2 is added in nanometer sheet2Ultrasonic disperse 1-3h in QDS solution, so
The hydro-thermal reaction 4-10h at 130-180 DEG C afterwards is centrifuged after completion of the reaction, washs, drying to get the vacancy defect containing S is arrived
SnS2/1T-MoS2QDS composite photo-catalyst;
Wherein, SnS2Nanometer sheet and 1T-MoS2The amount ratio of QDS solution is 0.1g:5-25mL.
Preferably, reaction solution dry 4-12h at 50-100 DEG C obtains the SnS of the vacancy defect containing S in step 32/1T-
MoS2QDS composite photo-catalyst.
Preferably, ultrasonic power is 320-400W in step 2 and step 3, and sonication treatment time is 1-3h.
Third object of the present invention is to provide above-mentioned SnS2/1T-MoS2QDS composite photo-catalyst is containing hexavalent chromium wastewater
Application in processing.
Compared with prior art, the beneficial effects of the present invention are:
The present invention adjusts SnS by changing the dosage of sulphur source in water-heat process2Generated sulphur vacancy in sample
Concentration realizes the controllability preparation of sulphur vacancy concentration;At the same time, 1T-MoS2QDS is as co-catalyst, with sulfur-bearing vacancy
The SnS of concentration2Sample forms close heterogeneous interface by ultrasonic wave auxiliary and hydro-thermal reaction, is more advantageous to photoproduction between interface
The fast transfer of charge, in addition, utilizing 1T-MoS2The upper transfer characteristic of QDS, greatly improves SnS2The light absorpting ability of material.
The composite photo-catalyst that the present invention prepares can promote the separation of photo-generate electron-hole pair, pass through proper proportion
It is compound, the recombination rate of photo-generate electron-hole pair is reduced, to show higher catalytic activity;It is prepared using the present invention
Catalyst out is handled containing hexavalent chromium wastewater, in neutrallty condition and under the conditions of without sacrifice agent, the photo catalytic reduction rate of Cr (VI)
Reach 75% or more, has broad application prospect in water treatment field.
Detailed description of the invention
The SnS that Fig. 1 is embodiment 2, comparative example 1 is prepared2/1T-MoS2QDS composite photo-catalyst and pure SnS2Sample
XRD diagram;
Fig. 2 is the SnS that embodiment 2 is prepared2/1T-MoS2QDS composite photo-catalyst and pure SnS2The UV-vis of sample
Spectrogram;
Fig. 3 is the SnS that embodiment 2 is prepared2/1T-MoS2QDS composite photo-catalyst and pure SnS2The electrochemistry of sample
Impedance (EIS) spectrogram.
Specific embodiment
In order to enable those skilled in the art to more fully understand, technical solution of the present invention is practiced, below with reference to specific
The invention will be further described for embodiment and attached drawing, but illustrated embodiment is not as a limitation of the invention.
Experimental method described in following each embodiments is conventional method unless otherwise specified;The reagent and material, such as
Without specified otherwise, can be commercially available on the market.
Embodiment 1
A kind of SnS2/1T-MoS2QDS composite photo-catalyst, including the SnS containing S vacancy defect2Nanometer sheet and load
In SnS21T-MoS in nanometer sheet2QDS, 1T-MoS2QDS and SnS2Nanometer sheet forms hetero-junctions, and 1T-MoS2QDS is compound
Weight accounting in photochemical catalyst is 1%.
It is specific the preparation method is as follows:
Step 1,5mmol SnCl is weighed4·5H2O and 5mmol citric acid, is dissolved in the ultrapure water of 40mL, magnetic force
Stir 30min;Then the L-cysteine for adding 5mmol continues to stir 1h, and then, by reaction solution, it is transferred to 100mL and has
In the autoclave of polytetrafluoroethyllining lining, it is placed in standing hydro-thermal reaction 12h in 150 DEG C of baking ovens, obtains yellow solid after reaction
Precipitating dries 12h by its centrifuge washing, and at 60 DEG C to get SnS2Nanometer sheet;
Step 2, by 1mmol Na2MoO4·2H2O ultrasound 30min in 30mL ultrapure water, obtains Na2MoO4·2H2O water
Solution;
By 1.5mmol thioacetamide in 30mL ethyl alcohol ultrasound 30min, obtain thioacetamide ethanol solution;
Na is added in thioacetamide ethanol solution2MoO4·2H2Continue ultrasound 30min in O aqueous solution, after ultrasonic,
Above-mentioned suspension is transferred in the autoclave of polytetrafluoroethyllining lining, stands reaction for 24 hours in 200 DEG C of baking ovens, reaction knot
Shu Hou, its supernatant of reaction solution centrifuging and taking, obtains 1T-MoS2QDS solution;
Ultrasound condition is the ultrasound 1h under 320W ultrasonic power;
Step 3, step 1 gained SnS is taken2Nanometer sheet 0.1g, and the resulting 1T-MoS of 5mL step 2 is added2QDS solution,
Suspension, is then transferred in the autoclave of polytetrafluoroethyllining lining by ultrasound 1h under 320W ultrasonic power, in 130 DEG C of baking ovens
Middle hydro-thermal reaction 4h, after reaction, centrifuge washing, dry 4h, can must contain the SnS of S vacancy defect at 100 DEG C2/1T-
MoS2QDS composite photo-catalyst.
The SnS for the vacancy defect containing S that measurement the present embodiment obtains by the following method2/1T-MoS2QDS composite photo-catalyst
Photocatalytic activity:
The composite photo-catalyst of 0.05g embodiment 1 is taken to be added to the K that 50mL concentration is 50mg/L2Cr2O7It is dark anti-in solution
30min is answered to reach adsorption-desorption balance, using measuring method-diphenyl carbazide spectrophotometry of Cr VI, with ultraviolet point
Absorbance of the reaction solution at 540nm after the above-mentioned dark reaction of light photometer measurement, while will be surveyed using Cr VI standard curve
The absorbance measured is converted into concentration, is denoted as initial concentration C0, then reaction solution is irradiated under Xe lamp with the optical filter of λ > 420nm
60min surveys its absorbance at 540nm, recycles Cr VI standard curve to convert concentration for the absorbance measured, is denoted as
Ct, then calculate the reduction rate of catalyst, the reduction rate calculation formula of catalyst are as follows: (C0-Ct)/C0× 100%.To this implementation
Example carries out photocatalysis performance test, and the photo catalytic reduction rate for obtaining Cr (VI) is 75.6%.
Embodiment 2
A kind of SnS2/1T-MoS2QDS composite photo-catalyst, including the SnS containing S vacancy defect2Nanometer sheet and load
In SnS21T-MoS in nanometer sheet2QDS, 1T-MoS2QDS and SnS2Nanometer sheet forms hetero-junctions, and 1T-MoS2QDS is compound
Weight accounting in photochemical catalyst is 3%.
It is specific the preparation method is as follows:
Step 1,5mmol SnCl is weighed4·5H2O and 5mmol citric acid is dissolved in 40mL ultrapure water, and magnetic force stirs
30min is mixed, 8.75mmol thioacetamide is then added, continues to stir 4h, then, transferring them to 100mL has polytetrafluoroethyl-ne
In the autoclave of alkene liner, it is placed in standing hydro-thermal reaction 12h in 150 DEG C of baking ovens, yellow solid precipitate is obtained after reaction, by it
Centrifuge washing, and 12h is dried at 60 DEG C to get SnS2Nanometer sheet;
Step 2, by 1mmol Na2MoO4·2H2O ultrasound 30min in 30mL ultrapure water, obtains Na2MoO4·2H2O water
Solution;
By 1mmol benzyl disulfide in 30mL ethyl alcohol ultrasound 30min, obtain benzyl disulfide ethanol solution;
Na is added in benzyl disulfide ethanol solution2MoO4·2H2Continue ultrasound 30min in O aqueous solution, after ultrasonic,
Above-mentioned suspension is transferred in the autoclave of polytetrafluoroethyllining lining, reaction 20h, reaction knot are stood in 180 DEG C of baking ovens
Black product obtained in reaction solution is dispersed in 30mL ultrapure water by Shu Hou, its supernatant of centrifuging and taking obtains 1T-MoS2QDS
Solution;
Ultrasound condition is the ultrasound 2h under 320W ultrasonic power;
Step 3, step 1 gained SnS is taken2Nanometer sheet 0.1g, and the resulting 1T-MoS of 15mL step 2 is added2QDS solution,
Suspension, is then transferred in the autoclave of polytetrafluoroethyllining lining by ultrasound 2h under 320W ultrasonic power, in 150 DEG C of baking ovens
Middle hydro-thermal reaction 5h, after reaction, centrifuge washing, dry 12h, can must contain the SnS of S vacancy defect at 60 DEG C2/1T-
MoS2QDS composite photo-catalyst.
The vacancy defect containing S made from the present embodiment is surveyed according to the method that embodiment 1 measures Cr (VI) photo catalytic reduction rate
SnS2/1T-MoS2The photocatalytic activity of QDS composite photo-catalyst, measuring it is 89.8% to the photo catalytic reduction rate of Cr (VI).
Embodiment 3
A kind of SnS2/1T-MoS2QDS composite photo-catalyst, including the SnS containing S vacancy defect2Nanometer sheet and load
In SnS21T-MoS in nanometer sheet2QDS, 1T-MoS2QDS and SnS2Nanometer sheet forms hetero-junctions, and 1T-MoS2QDS is compound
Weight accounting in photochemical catalyst is 3%.
It is specific the preparation method is as follows:
Step 1,5mmol SnCl is weighed4·5H2O and 5mmol citric acid is dissolved in 40mL ultrapure water, and magnetic force stirs
30min is mixed, 10mmol vulcanized sodium is then added, continues to stir 5h, then, transferring them to 100mL has polytetrafluoroethyllining lining
Autoclave in, be placed in 180 DEG C of baking ovens standing hydro-thermal reaction 12h, after reaction yellow solid precipitate, be centrifuged and washed
It washs, and dries 12h at 60 DEG C to get SnS2Nanometer sheet;
Step 2, by 1mmol ammonium molybdate in 30mL ultrapure water ultrasound 30min, obtain ammonium molybdate aqueous solution;
By 2mmol thiocarbamide in 30mL ethyl alcohol ultrasound 30min, obtain thiocarbamide ethanol solution;
Thiocarbamide ethanol solution is added in ammonium molybdate aqueous solution and continues ultrasound 30min, after ultrasound, by above-mentioned suspension
Be transferred in the autoclave of polytetrafluoroethyllining lining, in 220 DEG C of baking ovens stand reaction 12h, after reaction, centrifuging and taking its
Supernatant obtains 1T-MoS2QDS solution;
Ultrasound condition is the ultrasound 3h under 400W ultrasonic power;
Step 3, step 1 gained SnS is taken2Nanometer sheet 0.1g, and the resulting 1T-MoS of 25mL step 2 is added2QDS solution,
Suspension, is then transferred in the autoclave of polytetrafluoroethyllining lining by ultrasound 3h under 400W ultrasonic power, in 180 DEG C of baking ovens
Middle hydro-thermal reaction 10h, after reaction, centrifuge washing, dry 12h, can must contain the SnS of S vacancy defect at 50 DEG C2/1T-
MoS2QDS composite photo-catalyst.
According to the method that embodiment 1 measures Cr (VI) photo catalytic reduction rate, the vacancy defect containing S made from the present embodiment is surveyed
SnS2/1T-MoS2The photocatalytic activity of QDS composite photo-catalyst, measuring it is 78.9% to the photo catalytic reduction rate of Cr (VI).
Effect in order to further illustrate the present invention, the present invention is also provided with comparative example, specific as follows.
Comparative example 1
A kind of SnS2/1T-MoS2QDS composite photo-catalyst, including the SnS containing S vacancy defect2Nanometer sheet and load
In SnS21T-MoS in nanometer sheet2QDS, 1T-MoS2QDS and SnS2Nanometer sheet forms hetero-junctions, and 1T-MoS2QDS is compound
Weight accounting in photochemical catalyst is 0.4%.Specific preparation method with embodiment 2, the difference is that, the step 3 of comparative example 1
Middle 1T-MoS2The additional amount of QDS solution is 2ml.
According to the method that embodiment 1 measures Cr (VI) photo catalytic reduction rate, the vacancy defect containing S made from the present embodiment is surveyed
SnS2/1T-MoS2The photocatalytic activity of QDS composite photo-catalyst, measuring it is 53.8% to the photo catalytic reduction rate of Cr (VI).
Comparative example 2
A kind of SnS2/1T-MoS2QDS composite photo-catalyst, including the SnS containing S vacancy defect2Nanometer sheet and load
In SnS21T-MoS in nanometer sheet2QDS, 1T-MoS2QDS and SnS2Nanometer sheet forms hetero-junctions, and 1T-MoS2QDS is compound
Weight accounting in photochemical catalyst is 7%.Specific preparation method with embodiment 2, the difference is that, in the step 3 of comparative example 1
1T-MoS2The additional amount of QDS solution is 35ml.
According to the method that embodiment 1 measures Cr (VI) photo catalytic reduction rate, the vacancy defect containing S made from the present embodiment is surveyed
SnS2/1T-MoS2The photocatalytic activity of QDS composite photo-catalyst, measuring it is 62.3% to the photo catalytic reduction rate of Cr (VI).
From the composite photo-catalyst that embodiment 1-4 and comparative example 1-2 are prepared to from the point of view for the treatment of effect containing hexavalent chromium wastewater,
The composite photo-catalyst of embodiment 1-4 is more preferable to the photo catalytic reduction effect of Cr (VI), this is because suitable load can be one
Determine to improve 1T-MoS in degree2QDS agglomeration increases the interface face between two monomers while improving active catalyst sites
Product, is conducive to the raising of photocatalytic activity.But excessive load and load capacity deficiency will cause the reduction of active site in catalyst
So as to cause photocatalytic activity to reduce.
The SnS that embodiment 1-3 is prepared2/1T-MoS2The performance of QDS composite photo-catalyst is essentially identical, therefore only to reality
Apply the SnS that example 1 is prepared2/1T-MoS2The performance of QDS composite photo-catalyst is detected, to illustrate effect of the invention, tool
Body is shown in Fig. 1-3, wherein Fig. 1 is the SnS that embodiment 2 is prepared2/1T-MoS2QDS composite photo-catalyst and pure SnS2Sample
The XRD diagram of composite photo-catalyst, it will be seen from figure 1 that all diffraction maximums in the XRD spectrum of composite material with hexagonal phase two
The standard diffraction peak of artificial gold is corresponding, and no other miscellaneous peaks occur, and shows that sample purity is higher, and composite material is with fabulous
Crystallinity.
Fig. 2 is the SnS that embodiment 2 is prepared2/1T-MoS2QDS composite photo-catalyst and pure SnS2The complex light of sample
The UV-vis spectrogram of catalyst, figure it is seen that with pure SnS2Sample is compared, SnS2/1T-MoS2QDS complex light is urged
Agent sample shows broader light abstraction width, and is greater than at 450nm in wavelength, and the ability of light absorption is higher than pure SnS2
Sample.
Fig. 3 is the SnS that embodiment 2 is prepared2/1T-MoS2QDS composite photo-catalyst and pure SnS2The complex light of sample
Electrochemical impedance (EIS) spectrogram of catalyst, from figure 3, it can be seen that SnS2/1T-MoS2The Buddhist nun of QDS composite photocatalyst sample
Qwest's arc radius is far smaller than pure SnS2Sample, the separative efficiency for showing the photo-generate electron-hole pair of composite material are high.
The present invention describes preferred embodiment and its effect.It is created once a person skilled in the art knows basic
Property concept, then additional changes and modifications may be made to these embodiments.So it includes excellent that the following claims are intended to be interpreted as
It selects embodiment and falls into all change and modification of the scope of the invention.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (10)
1. a kind of SnS2/1T-MoS2QDS composite photo-catalyst, which is characterized in that including the SnS containing S vacancy defect2Nanometer sheet
And it is supported on the SnS21T-MoS in nanometer sheet2QDS, the 1T-MoS2The QDS and SnS2Nanometer sheet forms heterogeneous
Knot, and the 1T-MoS2Weight accounting of the QDS in the composite photo-catalyst is 1-3%.
2. SnS according to claim 12/1T-MoS2The preparation method of QDS composite photo-catalyst, which is characterized in that including
Following steps:
Step 1, SnCl4·5H2Hydro-thermal reaction occurs for O and sulfur-containing compound A, and the SnS of the vacancy defect containing S is prepared2Nanometer
Piece;
Step 2, hydro-thermal reaction occurs for molybdate and sulfur-containing compound B, and 1T-MoS is prepared2QDS solution;
Step 3, SnS2Nanometer sheet and 1T-MoS2Hydro-thermal reaction occurs for QDS solution, and the SnS of the vacancy defect containing S is prepared2/1T-
MoS2QDS composite photo-catalyst.
3. SnS according to claim 22/1T-MoS2The preparation method of QDS composite photo-catalyst, which is characterized in that step
SnS is prepared in 12Specific step is as follows for nanometer sheet:
By SnCl4·5H2O and citric acid are dissolved in ultrapure water A, and sulfur-containing compound A is then added, and 1-5h are stirred, after stirring
The hydro-thermal reaction 12h at 150-180 DEG C obtains yellow solid precipitate, as after completion of the reaction by reaction solution centrifugation, washing, drying
The SnS2Nanometer sheet;
Wherein, SnCl4·5H2O, citric acid, sulfur-containing compound A, ultrapure water A amount ratio be 1mmol:1mmol:1-2mmol:
8ml。
4. SnS according to claim 2 or 32/1T-MoS2The preparation method of QDS composite photo-catalyst, which is characterized in that
The sulfur-containing compound A is thioacetamide, thiocarbamide, vulcanized sodium or L-cysteine.
5. SnS according to claim 22/1T-MoS2The preparation method of QDS composite photo-catalyst, which is characterized in that step
Molybdate described in 2 is ammonium molybdate or Na2MoO4·2H2O;The sulfur-containing compound B is thiocarbamide, benzyl disulfide or thio second
Amide.
6. SnS according to claim 2 or 52/1T-MoS2The preparation method of QDS composite photo-catalyst, which is characterized in that
1T-MoS is prepared in step 22Specific step is as follows by QDS:
Molybdate is added in ultrapure water B and is ultrasonically treated, molybdic acid saline solution is obtained;
Sulfur-containing compound B is added in ethyl alcohol and is ultrasonically treated, sulfur-containing compound B ethanol solution is obtained;
Sulfur-containing compound B ethanol solution is added in molybdic acid saline solution and is ultrasonically treated, then hydro-thermal is anti-at 180-220 DEG C
12-24h is answered, is post-processed after completion of the reaction, 1T-MoS is obtained2QDS solution;
And when the sulfur-containing compound B is thiocarbamide or thioacetamide, the post-processing approach are as follows: after completion of the reaction will reaction
Liquid centrifugation, takes supernatant, obtains 1T-MoS2QDS solution;
When the sulphur compound B is benzyl disulfide, the post-processing approach are as follows: by black product obtained in reaction solution point
It is dispersed in 30mL ultrapure water, its supernatant of centrifuging and taking obtains 1T-MoS2QDS solution;
Molybdate, sulfur-containing compound B, ultrapure water B, ethyl alcohol amount ratio be 1mmol:1-2mmol:30mL:30mL.
7. SnS according to claim 22/1T-MoS2The preparation method of QDS composite photo-catalyst, which is characterized in that step
SnS is prepared in 32/1T-MoS2Specific step is as follows for QDS composite photo-catalyst:
By SnS made from step 121T-MoS made from step 2 is added in nanometer sheet2Ultrasonic disperse 1-3h, then exists in QDS solution
Hydro-thermal reaction 4-10h at 130-180 DEG C is centrifuged after completion of the reaction, washs, is dry to get the SnS for arriving the vacancy defect containing S2/1T-
MoS2QDS composite photo-catalyst;
Wherein, SnS2Nanometer sheet and 1T-MoS2The amount ratio of QDS solution is 0.1g:5-25mL.
8. SnS according to claim 72/1T-MoS2The preparation method of QDS composite photo-catalyst, which is characterized in that step
Reaction solution dry 4-12h at 50-100 DEG C obtains the SnS of the vacancy defect containing S in 32/1T-MoS2QDS composite photo-catalyst.
9. the SnS according to claim 5 or 72/1T-MoS2The preparation method of QDS composite photo-catalyst, which is characterized in that
Ultrasonic power is 320-400W in step 2 and step 3, and sonication treatment time is 1-3h.
10. a kind of SnS described in claim 12/1T-MoS2QDS composite photo-catalyst answering in being handled containing hexavalent chromium wastewater
With.
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