CN107899599A - A kind of V N codopes TiO2/MoS2The preparation method of composite photocatalyst material - Google Patents
A kind of V N codopes TiO2/MoS2The preparation method of composite photocatalyst material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 34
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 239000002131 composite material Substances 0.000 title claims abstract description 23
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 44
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 8
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 7
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 25
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 14
- 239000011159 matrix material Substances 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 9
- 229960000583 acetic acid Drugs 0.000 claims description 8
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 8
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 8
- 229940043237 diethanolamine Drugs 0.000 claims description 8
- 239000012362 glacial acetic acid Substances 0.000 claims description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 8
- JAJWGJBVLPIOOH-IZYKLYLVSA-M sodium taurocholate Chemical compound [Na+].C([C@H]1C[C@H]2O)[C@H](O)CC[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@H]([C@@H](CCC(=O)NCCS([O-])(=O)=O)C)[C@@]2(C)[C@@H](O)C1 JAJWGJBVLPIOOH-IZYKLYLVSA-M 0.000 claims description 7
- 239000006228 supernatant Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 14
- 238000006555 catalytic reaction Methods 0.000 abstract description 10
- 238000007146 photocatalysis Methods 0.000 abstract description 10
- 230000002708 enhancing effect Effects 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 230000005540 biological transmission Effects 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 239000002800 charge carrier Substances 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 238000010276 construction Methods 0.000 abstract description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 2
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- 229940086056 activeoxy Drugs 0.000 abstract 1
- 125000001820 oxy group Chemical group [*:1]O[*:2] 0.000 abstract 1
- 239000003643 water by type Substances 0.000 description 7
- 239000004065 semiconductor Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 4
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 125000005909 ethyl alcohol group Chemical group 0.000 description 4
- 238000002835 absorbance Methods 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- YCIHPQHVWDULOY-FMZCEJRJSA-N (4s,4as,5as,6s,12ar)-4-(dimethylamino)-1,6,10,11,12a-pentahydroxy-6-methyl-3,12-dioxo-4,4a,5,5a-tetrahydrotetracene-2-carboxamide;hydrochloride Chemical compound Cl.C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H](N(C)C)C(=O)C(C(N)=O)=C(O)[C@@]4(O)C(=O)C3=C(O)C2=C1O YCIHPQHVWDULOY-FMZCEJRJSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- 150000001336 alkenes Chemical group 0.000 description 1
- 230000003466 anti-cipated effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000004577 artificial photosynthesis Methods 0.000 description 1
- 230000003542 behavioural effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 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
-
- 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
- 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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Chemical & Material Sciences (AREA)
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Materials Engineering (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a kind of V N codopes TiO2/MoS2The preparation method of composite photocatalyst material, belongs to catalysis material preparing technical field.The present invention with slotted mode by V N by entering TiO2Lattice, and and MoS2Special construction is compounded to form, more avtive spots are provided in light-catalyzed reaction, is more conducive to the absorption and transmission of material in catalytic process, i.e. absorbing synergic effect enhancing photocatalysis, the present invention reduces TiO by codope2Band gap, TiO2 is to ultraviolet-visible absorption ability for enhancing, and and MoS2It is compound, cause the very poor change of energy between the two, and sufficiently narrow band gap enable absorb visible ray after valence electron be excited to conduction band, strengthen photoresponse scope, strengthen photocatalysis performance, composite material prepared by the present invention produces high electronics, hole separation rate through photoinduction, and light induced electron can easily migrate to surface from the interior zone of catalysis material and participate in reacting, the enhancing of charge carrier separation will cause the increase of more active oxy groups, strengthen photocatalytic degradation capability.
Description
Technical field
The present invention relates to a kind of V-N codopes TiO2/MoS2The preparation method of composite photocatalyst material, belongs to photocatalysis material
Expect preparing technical field.
Background technology
Solar energy has been to be concerned by more and more people as a kind of cleaning, safe, abundant regenerative resource.The earth it is big
The solar energy that gas, ocean and land absorb every year is about 3.85 × 106EJ, all earth for obtaining and exploiting equivalent to the mankind
Upper non-renewable energy resources coal, oil, 2 times of natural gas and uranium summation.Therefore, solar energy is made full use of not only to solve energy danger
Machine, it may also reduce environmental pollution and ecological disruption.Although the solar energy total amount for reaching earth surface is very big, energy-flux density is very
It is low, and be subject to round the clock, season, the natural conditions such as geographic latitude and height above sea level limited, Yi Jiyin, fine, cloud, rain etc. are random
The influence of factor, makes solar energy have unstability.It would therefore be desirable to a kind of effective means convert solar energy into electricity
Energy, chemical energy etc., and concentrated and store and then overcome the limitation of natural conditions and enchancement factor.Semiconductor light sulfate ferroelectric functional material
Due to photoconduction and photovoltaic effect, being the main media for converting solar energy into chemical energy and electric energy, being the profit of solar energy
With providing possibility.The photoelectric activity of photoelectric functional material is inherently subject to the light of enough energy to excite by semi-conducting material
The behavioral trait of generation photogenerated charge is determined afterwards.
Among various green technologies, researchers focus more on Photocatalitic Technique of Semiconductor, because photocatalytic process energy
Amount consumption it is low, reaction condition is gentle, and device is simple, can outdoor using sunlight resource or indoors using it is low into
This artificial light sources, and oxidation reaction and reduction reaction can occur in reaction process at the same time, photocatalytic water prepare hydrogen and
Oxygen, photodegradation pollutant, artificial photosynthesis, opto-electronic conversion etc. all have potential using value.
Photocatalitic Technique of Semiconductor has before developing well as a kind of effective way for solving environment and energy problem
Scape.But traditional catalysis material deposits two key issues at present, influence catalyst photocatalytic activity and its actual answer
With：Photoresponse narrow range and quantum efficiency are low.
Semiconductor light sulfate ferroelectric functional material not only has important application in terms of solar cell, photocatalysis, and in sensor, life
Thing monitoring etc. also has important application.
Therefore, the light abstraction width of catalysis material is expanded, improves the separation rate of photo-generate electron-hole, suppresses photoproduction and carries
The compound of stream is the key factor for improving photocatalysis efficiency.It is the major issue that photocatalysis field needs to solve.
The content of the invention
The technical problems to be solved by the invention：For current traditional catalysis material photoresponse narrow range and quantum efficiency
A kind of the problem of low, there is provided V-N codopes TiO2/MoS2The preparation method of composite photocatalyst material.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
（1）Take butyl titanate, glacial acetic acid to add in absolute ethyl alcohol and be uniformly mixed, add diethanol amine, ammonium metavanadate stirring 2
~3h, obtains mixed liquor；
（2）Take molybdenum disulfide powder, sodium taurocholate add deionized water medium wave 6~8h of ultrasonic disperse, and low-speed centrifugal separation 30~
40min, takes supernatant, then the 30~40min that is centrifuged at a high speed, and takes precipitation, obtains class graphene-structured molybdenum disulfide；
（3）Take class graphene-structured molybdenum disulfide to add 30~40min of ultrasonic disperse in acetum, obtain matrix liquid；
（4）Mixed liquor is added dropwise in matrix liquid, at 0~4 DEG C, is stirred with 600~800r/min to being added dropwise, hydro-thermal is anti-
Should after filter to obtain filter residue, by filter residue washing and drying, obtain V-N codopes TiO2/MoS2Composite photocatalyst material.
Step（1）The butyl titanate, diethanol amine, the molar ratio of ammonium metavanadate are（10~20）：（1~2）：（1~
2）.
Step（1）The mass ratio of the glacial acetic acid and absolute ethyl alcohol is 1：10, dosage for butyl titanate quality 12~
60%。
Step（2）The molybdenum disulfide powder and the mass ratio of deionized water are 1：200, the dosage of sodium taurocholate is curing
The 25~36% of molybdenum powder quality.
Step（2）The low-speed centrifugal rate of departure is 3000~4000r/min, and the speed that is centrifuged at a high speed is
10000~12000r/min.
Step（3）The mass ratio of the class graphene-structured molybdenum disulfide and butyl titanate is（2~4）：（17~34）,
The mass fraction of the acetum is 1%, and dosage is 25~100 times of class graphene-structured molybdenum disulfide quality.
Step（4）The hydrothermal reaction process is heated to 120~160 DEG C, insulation reaction 12 to be transferred in hydrothermal reaction kettle
~15h.
Compared with other methods, advantageous effects are the present invention：
（1）The present invention with slotted mode by V-N by entering TiO2Lattice, and and MoS2Special construction is compounded to form, is urged in light
Change in reaction and more avtive spots are provided, be more conducive to the absorption and transmission of material in catalytic process, is i.e. absorbing synergic effect increases
Strong photocatalysis；
（2）The present invention reduces TiO by codope2Band gap, TiO2 is to ultraviolet-visible absorption ability for enhancing, and and MoS2It is multiple
Close, cause the very poor change of energy between the two, and sufficiently narrow band gap to absorb valence electron after visible ray and be excited to and leads
Band, strengthens photoresponse scope, strengthens photocatalysis performance；
（3）Composite material prepared by the present invention produces high electronics, hole separation rate through photoinduction, and light induced electron can be easy to
Ground migrates to surface from the interior zone of catalysis material and participates in reacting, and the enhancing of charge carrier separation will cause more activity
The increase of oxygen groups, strengthens photocatalytic degradation capability.
Embodiment
Taking 0.1~0.2mol butyl titanates, 10~20g glacial acetic acid, adds in 100~200g absolute ethyl alcohols, with 300~
400r/min stirs 20~30min, adds 0.01~0.02mol diethanol amine, 0.01~0.02mol ammonium metavanadates, continue
2~3h is stirred, obtains mixed liquor, takes 10~12g molybdenum disulfide powders, 3.0~3.6g sodium taurocholates, add 2.0~2.4L deionizations
In water, under 40~50 DEG C of waters bath with thermostatic control, 6~8h is disperseed with 300W ultrasonic echographies, then be transferred in centrifuge with 3000~
4000r/min centrifuges 30~40min, takes supernatant, and centrifuges 30~40min with 10000~12000r/min, takes
Class graphene-structured molybdenum disulfide is precipitated to obtain, takes 4~8g class graphene-structured molybdenum disulfide, adds 200~400g mass fractions
In 1% acetum, to disperse 30~40min with 300W ultrasonic echographies, obtaining matrix liquid, by mixed liquor with 1~2ml/min drops
Add in matrix liquid, at 0~4 DEG C, stirred with 600~800r/min to being added dropwise, and be transferred in hydrothermal reaction kettle, heat
To 120~160 DEG C, 12~15h of insulation reaction, filters to obtain filter residue after being cooled to room temperature, and filter residue is washed with deionized 3~5 times,
It is placed in drying box, is dried at 60~80 DEG C to constant weight, obtain V-N codopes TiO2/MoS2Composite photocatalyst material.
Example 1
0.1mol butyl titanates are taken, 10g glacial acetic acid, adds in 100g absolute ethyl alcohols, stirs 20min with 300r/min, then add
Enter 0.01mol diethanol amine, 0.01mol ammonium metavanadates, continue to stir 2h, obtain mixed liquor, take 10g molybdenum disulfide powders, 3.0g
Sodium taurocholate, adds in 2.0L deionized waters, under 40 DEG C of waters bath with thermostatic control, disperses 6h with 300W ultrasonic echographies, then be transferred to centrifugation
30min is centrifuged with 3000r/min in machine, takes supernatant, and 30min is centrifuged with 10000r/min, takes and precipitates to obtain class
Graphene-structured molybdenum disulfide, takes 4g class graphene-structured molybdenum disulfide, adds 200g mass fractions and is in 1% acetum, with
300W ultrasonic echographies disperse 30min, obtain matrix liquid, and mixed liquor is added dropwise in matrix liquid with 1ml/min, at 0 DEG C, with
600r/min is stirred to being added dropwise, and is transferred in hydrothermal reaction kettle, is heated to 120 DEG C, insulation reaction 12h, is cooled to room temperature
After filter to obtain filter residue, filter residue is washed with deionized 3 times, is placed in drying box, at 60 DEG C dry to constant weight, obtain V-N and be total to
Adulterate TiO2/MoS2Composite photocatalyst material.
Example 2
0.1mol butyl titanates are taken, 15g glacial acetic acid, adds in 150g absolute ethyl alcohols, stirs 25min with 350r/min, then add
Enter 0.01mol diethanol amine, 0.01mol ammonium metavanadates, continue to stir 2h, obtain mixed liquor, take 11g molybdenum disulfide powders, 3.3g
Sodium taurocholate, adds in 2.2L deionized waters, under 45 DEG C of waters bath with thermostatic control, disperses 7h with 300W ultrasonic echographies, then be transferred to centrifugation
35min is centrifuged with 3500r/min in machine, takes supernatant, and 35min is centrifuged with 11000r/min, takes and precipitates to obtain class
Graphene-structured molybdenum disulfide, takes 6g class graphene-structured molybdenum disulfide, adds 300g mass fractions and is in 1% acetum, with
300W ultrasonic echographies disperse 35min, obtain matrix liquid, and mixed liquor is added dropwise in matrix liquid with 1ml/min, at 2 DEG C, with
700r/min is stirred to being added dropwise, and is transferred in hydrothermal reaction kettle, is heated to 140 DEG C, insulation reaction 13h, is cooled to room temperature
After filter to obtain filter residue, filter residue is washed with deionized 4 times, is placed in drying box, at 70 DEG C dry to constant weight, obtain V-N and be total to
Adulterate TiO2/MoS2Composite photocatalyst material.
Example 3
0.2mol butyl titanates are taken, 20g glacial acetic acid, adds in 200g absolute ethyl alcohols, stirs 30min with 400r/min, then add
Enter 0.02mol diethanol amine, 0.02mol ammonium metavanadates, continue to stir 3h, obtain mixed liquor, take 12g molybdenum disulfide powders, 3.6g
Sodium taurocholate, adds in 2.4L deionized waters, under 50 DEG C of waters bath with thermostatic control, disperses 8h with 300W ultrasonic echographies, then be transferred to centrifuge
In 40min centrifuged with 4000r/min, take supernatant, and 40min is centrifuged with 12000r/min, take and precipitate to obtain class stone
Black alkene structure molybdenum disulfide, takes 8g class graphene-structured molybdenum disulfide, adds 400g mass fractions and is in 1% acetum, with
300W ultrasonic echographies disperse 40min, obtain matrix liquid, and mixed liquor is added dropwise in matrix liquid with 2ml/min, at 4 DEG C, with
800r/min is stirred to being added dropwise, and is transferred in hydrothermal reaction kettle, is heated to 160 DEG C, insulation reaction 15h, is cooled to room temperature
After filter to obtain filter residue, filter residue is washed with deionized 5 times, is placed in drying box, at 80 DEG C dry to constant weight, obtain V-N and be total to
Adulterate TiO2/MoS2Composite photocatalyst material.
Reference examples：The composite photocatalyst material of Hebei company production.
The composite photocatalyst material of example and reference examples is detected, specific detection is as follows：
100mgAg/ZnO/C catalyst is distributed in quadracycline (TC-HC1) aqueous solution that 100mL concentration is 20mg/L.
Using the xenon lamp of the mercury lamp of 250W and 500W as ultraviolet light and the light source of visible ray, and xenon lamp is filtered off by wave chopping glass
Ultraviolet light in light source under 400nm.Before light source opening, dispersion liquid stirs 40 minutes in the dark to be reached to TC-HC1 and catalyst
Adsorption-desorption balances.It is then turned on light source and triggers light-catalyzed reaction, reacts at interval of one section of regular time, with disposable pin
Pipe takes 3mL reaction solutions, filters solid particle by the PTFE filters of 0.45um, obtains supernatant liquid.Use UV-Vis spectrophotometry
Absorbance of the TC-HC1l solution filtered out every time at wavelength 355nm is measured at photometer.According to Lambert-Beer's law, solution
Absorbance and solution concentration it is proportional, its concentration is detected according to the change Come of differential responses time TC-HC1 absorbances
Change, and calculate the degradation rate of TC-HC1.
Specific testing result such as table 1.
Table 1
| Detection project | Example 1 | Example 2 | Example 3 | Reference examples |
| Degradation rate % | 95.8 | 90.3 | 90.6 | 81.0 |
| Adsorbance % | 40.0 | 41.9 | 42.1 | 10.0 |
As shown in Table 1, the composite photocatalyst material that prepared by the present invention is more stable under visible light.Due to the energy gap of ZnO
It is bigger, it is anticipated that the simple active very littles of ZnO under visible light.Meanwhile photocatalysis stability test has been carried out to sample,
Find that sample still has very high photocatalytic activity after 4 light-catalyzed reactions, illustrate that catalysis material prepared by the present invention has
Preferable photocatalysis stability and it is not susceptible to photoetch phenomenon.
Claims (7)
- A kind of 1. V-N codopes TiO2/MoS2The preparation method of composite photocatalyst material, it is characterised in that concretely comprise the following steps：（1）Take butyl titanate, glacial acetic acid to add in absolute ethyl alcohol and be uniformly mixed, add diethanol amine, ammonium metavanadate stirring 2 ~3h, obtains mixed liquor；（2）Take molybdenum disulfide powder, sodium taurocholate add deionized water medium wave 6~8h of ultrasonic disperse, and low-speed centrifugal separation 30~ 40min, takes supernatant, then the 30~40min that is centrifuged at a high speed, and takes precipitation, obtains class graphene-structured molybdenum disulfide；（3）Take class graphene-structured molybdenum disulfide to add 30~40min of ultrasonic disperse in acetum, obtain matrix liquid；（4）Mixed liquor is added dropwise in matrix liquid, at 0~4 DEG C, is stirred with 600~800r/min to being added dropwise, hydro-thermal is anti- Should after filter to obtain filter residue, by filter residue washing and drying, obtain V-N codopes TiO2/MoS2Composite photocatalyst material.
- A kind of 2. V-N codopes TiO as claimed in claim 12/MoS2The preparation method of composite photocatalyst material, its feature exist In step（1）The butyl titanate, diethanol amine, the molar ratio of ammonium metavanadate are（10~20）：（1~2）：（1~2）.
- A kind of 3. V-N codopes TiO as claimed in claim 12/MoS2The preparation method of composite photocatalyst material, its feature exist In step（1）The mass ratio of the glacial acetic acid and absolute ethyl alcohol is 1：10, dosage is the 12~60% of butyl titanate quality.
- A kind of 4. V-N codopes TiO as claimed in claim 12/MoS2The preparation method of composite photocatalyst material, its feature exist In step（2）The molybdenum disulfide powder and the mass ratio of deionized water are 1：200, the dosage of sodium taurocholate is molybdenum disulphide powder The 25~36% of last quality.
- A kind of 5. V-N codopes TiO as claimed in claim 12/MoS2The preparation method of composite photocatalyst material, its feature exist In step（2）The low-speed centrifugal rate of departure is 3000~4000r/min, the speed that is centrifuged at a high speed for 10000~ 12000r/min。
- A kind of 6. V-N codopes TiO as claimed in claim 12/MoS2The preparation method of composite photocatalyst material, its feature exist In step（3）The mass ratio of the class graphene-structured molybdenum disulfide and butyl titanate is（2~4）：（17~34）, it is described The mass fraction of acetum is 1%, and dosage is 25~100 times of class graphene-structured molybdenum disulfide quality.
- A kind of 7. V-N codopes TiO as claimed in claim 12/MoS2The preparation method of composite photocatalyst material, its feature exist In step（4）The hydrothermal reaction process is heated to 120~160 DEG C to be transferred in hydrothermal reaction kettle, and insulation reaction 12~ 15h。
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111495372A (en) * | 2019-01-31 | 2020-08-07 | 中国科学院上海高等研究院 | NiO/TiO2Composite and preparation method and application thereof |
| CN112811523A (en) * | 2020-12-14 | 2021-05-18 | 南昌航空大学 | Preparation method and application of nanocomposite oxygen-doped molybdenum disulfide/titanium dioxide nanotube array |
| CN113262772A (en) * | 2021-05-13 | 2021-08-17 | 岭南师范学院 | Preparation method of high photocatalytic efficiency nano composite material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103357425A (en) * | 2013-07-10 | 2013-10-23 | 黑龙江大学 | Preparation method of molybdenum disulfide/titanium dioxide composite material with nano thorn hierarchical structure |
| CN103990482A (en) * | 2014-05-16 | 2014-08-20 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of vanadium and nitrogen co-doped titanium dioxide/activated carbon photocatalyst |
| CN104560347A (en) * | 2014-12-29 | 2015-04-29 | 北京航空航天大学 | In-situ preparation method of water-based lubricant containing molybdenum disulfide nanosheet |
-
2017
- 2017-11-21 CN CN201711161800.1A patent/CN107899599A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103357425A (en) * | 2013-07-10 | 2013-10-23 | 黑龙江大学 | Preparation method of molybdenum disulfide/titanium dioxide composite material with nano thorn hierarchical structure |
| CN103990482A (en) * | 2014-05-16 | 2014-08-20 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of vanadium and nitrogen co-doped titanium dioxide/activated carbon photocatalyst |
| CN104560347A (en) * | 2014-12-29 | 2015-04-29 | 北京航空航天大学 | In-situ preparation method of water-based lubricant containing molybdenum disulfide nanosheet |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111495372A (en) * | 2019-01-31 | 2020-08-07 | 中国科学院上海高等研究院 | NiO/TiO2Composite and preparation method and application thereof |
| CN112811523A (en) * | 2020-12-14 | 2021-05-18 | 南昌航空大学 | Preparation method and application of nanocomposite oxygen-doped molybdenum disulfide/titanium dioxide nanotube array |
| CN113262772A (en) * | 2021-05-13 | 2021-08-17 | 岭南师范学院 | Preparation method of high photocatalytic efficiency nano composite material |
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