CN105797753A - MoS2/TiO2 two-dimensional composite nanometer photocatalyst and preparation method and application thereof - Google Patents
MoS2/TiO2 two-dimensional composite nanometer photocatalyst and preparation method and application thereof Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 48
- 229910052961 molybdenite Inorganic materials 0.000 title claims abstract description 23
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 23
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title abstract description 26
- 239000002131 composite material Substances 0.000 title abstract description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 57
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000002105 nanoparticle Substances 0.000 claims abstract description 21
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 17
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 17
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 15
- 239000012265 solid product Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 8
- 150000001875 compounds Chemical class 0.000 claims description 39
- 239000007788 liquid Substances 0.000 claims description 36
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 16
- 239000000047 product Substances 0.000 claims description 14
- 238000000926 separation method Methods 0.000 claims description 13
- 238000005119 centrifugation Methods 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000003912 environmental pollution Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 230000006872 improvement Effects 0.000 claims description 4
- 238000011534 incubation Methods 0.000 claims description 4
- 230000003197 catalytic effect Effects 0.000 claims description 3
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 14
- 239000002243 precursor Substances 0.000 description 12
- 238000001035 drying Methods 0.000 description 8
- 238000007146 photocatalysis Methods 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 208000036626 Mental retardation Diseases 0.000 description 1
- 229910004619 Na2MoO4 Inorganic materials 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 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
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
-
- B01J35/39—
-
- B01J35/615—
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- 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
Abstract
The invention discloses a MoS2/TiO2 two-dimensional composite nanometer photocatalyst and a preparation method and application thereof. Tetrabutyl titanate and HF are subjected to a hydrothermal reaction, and TiO2 nano particles with exposed {001} faces are prepared; then, the TiO2 nano particles with the exposed {001} faces, sodium molybdate and thiourea are subjected to a hydrothermal reaction together, wherein the mass ratio of sodium molybdate to thiourea is 1:2, the solid products are dried and ground into powder, and the MoS2/TiO2 two-dimensional composite nanometer photocatalyst is obtained. The prepared MoS2/TiO2 two-dimensional composite nanometer photocatalyst is small in particle size, the specific area can reach 110 m<2>/g, and very high photocatalytic activity is achieved. The preparation method is simple in process, easy to control and high in production efficiency, and has important application prospects in the environment pollution treatment field.
Description
Technical field
The invention belongs to photocatalysis field, be specifically related to a kind of MoS2/TiO2Two dimension compound nanometer photocatalyst and its preparation method and application.
Background technology
Photocatalysis refers to utilize semiconductor absorber solar energy and convert it into the characteristic of chemical energy and carrys out degradation of organic substances, this mode efficiency is high and does not result in secondary pollution, the new direction of environmental improvement, and photocatalysis technology it is crucial that the selection of suitable catalyst and preparation.Transition metal oxide TiO2Have nontoxic, catalytic efficiency is high, good stability, the advantage such as with low cost, be a kind of ideal photocatalyst material, there is huge application prospect.
TiO2Having anatase and two stable crystalline phases of rutile, being generally used for light-catalysed is the Anatase that activity is higher.The different crystal plane surface of anatase can be widely different, and the surface of common several crystal faces can be successively: { 101}:0.43J/m2, { 010}:0.57J/m2, { 001}:0.95J/m2, { 111}:1.61J/m2.The crystal face such as 001} has significantly high crystal face energy, also correspondingly has a significantly high catalysis activity, but the TiO that commonsense method obtains2A large amount of crystal faces of exposing be mental retardation 101} face, and high energy { it is only small that 001} face exposes ratio.
In crystal growing process, surface can high, crystal face that chemism is big the speed of growth faster, thus causing that proportion is relatively low in the crystal generated.It is to say, in crystal prepared by commonsense method, the crystal face overwhelming majority being exposed to outside is that surface can minimum crystal face minimum, active.For Anatase TiO2, be exposed under general case the crystal face of outside be mainly surface can minimum 101} face (> 94%), rather than surface can higher, active better { the 001} face of catalysis.If it is possible to improve high energy crystal face to be exposed to the ratio of outside, then can be greatly improved TiO2Photocatalysis performance.{ the TiO that 001} crystal face exposes at present2Successfully prepared.
But then, TiO2Quantum separation efficiency relatively low, and two-dimensional material MoS2It is a kind of desirably complex matrix, will { the TiO that 001} face exposes2Nanometer sheet and two-dimensional material MoS2Compound preparation two dimension composite photo-catalyst is expected to its performance is greatly improved.
Summary is discussed, it can be seen that the preparation of two dimension composite photo-catalyst remains a problem, particularly up to the present, yet there are no bibliographical information and is capable of technology and method prepared by two dimension composite photo-catalyst.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that a kind of MoS2/TiO2Two dimension compound nanometer photocatalyst and its preparation method and application.The present invention is with butyl titanate (C16H36O4Ti), Fluohydric acid. (HF), sodium molybdate (Na2MoO4) and thiourea (CH4N2S) for presoma, MoS is prepared by secondary hydro-thermal method2/TiO2Two dimension compound nanometer photocatalyst.The advantage of two-dimentional compound nanometer photocatalyst prepared by the present invention is in that: (1) has significantly high photocatalytic activity；(2) particle size is little, has very big specific surface area (110m2/g).Therefore, this two dimension compound nanometer photocatalyst has good application prospect in photocatalysis environmental improvement.
The present invention solves that the technical scheme that above-mentioned technical problem provides is specific as follows:
A kind of MoS2/TiO2Two dimension compound nanometer photocatalyst, has the pure Anatase structure of shell mould, and its kernel is TiO2Nanometer sheet, shell is MoS2, specific surface area is 110m2/g。
One prepares MoS2/TiO2The method of two dimension compound nanometer photocatalyst, comprises the following steps: butyl titanate and HF are carried out hydro-thermal reaction, prepares { the TiO that 001} face exposes2Nano-particle；Then will the { TiO that 001} face exposes2Nano-particle carries out hydro-thermal reaction together with sodium molybdate and thiourea, and wherein, the mass ratio of sodium molybdate and thiourea is 1:2；Solid product is dried, grind into powder, obtain MoS2/TiO2Two dimension compound nanometer photocatalyst.
Specifically include following steps:
(1) by butyl titanate and HF 10:(1～4 by volume) mix homogeneously, it is placed in hydrothermal reaction kettle and carries out incubation water heating reaction, the temperature of hydro-thermal reaction is 150～200 DEG C, and the time of hydro-thermal reaction is 15～30 hours；
(2) solidliquid mixture after step (1) hydro-thermal reaction is carried out solid-liquid centrifugation separation, discard liquid, by solid product deionized water wash 2～5 times, then dry 6～10 hours at 60～90 DEG C；
(3) the product grind into powder after step (2) being dried, obtains { the TiO that 001} face exposes2Nano-particle；
(4) will { TiO that 001} face exposes2Nano-particle and sodium molybdate and thiourea 100:(3～30 in mass ratio): (6～60) mix homogeneously, wherein, the mass ratio of sodium molybdate and thiourea is 1:2, it is placed in hydrothermal reaction kettle and carries out incubation water heating reaction, the temperature of hydro-thermal reaction is 150～200 DEG C, and the time of hydro-thermal reaction is 15～30 hours；
(5) solidliquid mixture after step (4) hydro-thermal reaction is carried out solid-liquid centrifugation separation, discard liquid, by solid product deionized water wash 2～5 times, then dry 6～10 hours at 60～90 DEG C；
(6) the product grind into powder after step (5) being dried, obtains MoS2/TiO2Two dimension compound nanometer photocatalyst.
Above-mentioned MoS2/TiO2Two dimension compound nanometer photocatalyst is in the application of catalytic field.
Above-mentioned MoS2/TiO2Two dimension compound nanometer photocatalyst application in environmental pollution improvement.
MoS prepared by the present invention2/TiO2Two dimension compound nanometer photocatalyst is for environmental pollution treatment, for instance the purification etc. of water and air.
The present invention has the following advantages and beneficial effect:
(1) present invention utilizes MoS prepared by hydro-thermal method2/TiO2Two dimension compound nanometer photocatalyst, with { the TiO that 001} face exposes2Nano-particle and standard sample P25 compare, and its photocatalysis performance is greatly enhanced.
(2) preparation method of the present invention is simple, and preparation process is easily controllable, and production efficiency is high, and photocatalyst will be played great impetus in the practical application of environmental pollution treatment.
Accompanying drawing explanation
Fig. 1 is the MoS of embodiment 1 preparation2/TiO2Transmission electron microscope (TEM) figure of two dimension compound nanometer photocatalyst；
Fig. 2 is the MoS of embodiment 5, embodiment 6 and embodiment 2 preparation2/TiO2X-ray diffraction (XRD) comparison diagram of two dimension compound nanometer photocatalyst；
Fig. 3 is the MoS of embodiment 5, embodiment 6 and embodiment 3 preparation2/TiO2Ultraviolet-visible (UV-Vis) the absorption spectrum comparison diagram of two dimension compound nanometer photocatalyst；
Fig. 4 is the MoS of embodiment 4 preparation2/TiO2X-ray photoelectron power spectrum (XPS) figure of two dimension compound nanometer photocatalyst；
Fig. 5 is the MoS of embodiment 5, embodiment 6 and embodiment 2 preparation2/TiO2Two dimension compound nanometer photocatalyst degradation effect comparison diagram to methylene blue under light illumination.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is expanded on further, but does not therefore limit the present invention within described scope of embodiments.
Embodiment 1
According to volume ratio 10:1, butyl titanate and HF being mixed into precursor liquid, is placed in hydrothermal reaction kettle by precursor liquid and carries out hydro-thermal reaction, the temperature of hydro-thermal reaction is 160 DEG C, and constant temperature time is 15 hours；Solidliquid mixture after hydro-thermal reaction is carried out solid-liquid centrifugation separation, discards liquid, by solid product deionized water wash 2 times, then dry 6 hours at 60 DEG C；By the product grind into powder after drying, obtain { the TiO that 001} face exposes2Nano-particle；Will { the TiO that 001} face exposes2Nano-particle is mixed into precursor liquid with sodium molybdate and thiourea according to mass ratio 100:3:6, is placed in hydrothermal reaction kettle and carries out hydro-thermal reaction, and the temperature of hydro-thermal reaction is 150 DEG C, and constant temperature time is 15 hours；Solidliquid mixture after hydro-thermal reaction is carried out solid-liquid centrifugation separation, discards liquid, by solid product deionized water wash 2 times, then dry 6 hours at 60 DEG C；By the product grind into powder after drying, obtain MoS2/TiO2Two dimension compound nanometer photocatalyst.
Embodiment 2
According to volume ratio 10:2, butyl titanate and HF being mixed into precursor liquid, is placed in hydrothermal reaction kettle by precursor liquid and carries out hydro-thermal reaction, the temperature of hydro-thermal reaction is 170 DEG C, and constant temperature time is 18 hours；Solidliquid mixture after hydro-thermal reaction is carried out solid-liquid centrifugation separation, discards liquid, by solid product deionized water wash 3 times, then dry 7 hours at 70 DEG C；By the product grind into powder after drying, obtain { the TiO that 001} face exposes2Nano-particle；Will { the TiO that 001} face exposes2Nano-particle is mixed into precursor liquid with sodium molybdate and thiourea according to mass ratio 100:6:12, is placed in hydrothermal reaction kettle and carries out hydro-thermal reaction, and the reaction temperature of hydro-thermal is 160 DEG C, and constant temperature time is 20 hours；Solidliquid mixture after hydro-thermal reaction is carried out solid-liquid centrifugation separation, discards liquid, by solid product deionized water wash 3 times, then dry 7 hours at 70 DEG C；By the product grind into powder after drying, obtain MoS2/TiO2Two dimension compound nanometer photocatalyst.
Embodiment 3
According to volume ratio 10:3, butyl titanate and HF being mixed into precursor liquid, is placed in hydrothermal reaction kettle by precursor liquid and carries out hydro-thermal reaction, hydrothermal temperature is 180 DEG C, and constant temperature time is 24 hours；Solidliquid mixture after hydro-thermal reaction is carried out solid-liquid centrifugation separation, discards liquid, by solid product deionized water wash 4 times, then dry 8 hours at 80 DEG C；By the product grind into powder after drying, obtain { the TiO that 001} face exposes2Nano-particle；Will { the TiO that 001} face exposes2Nano-particle is mixed into precursor liquid with sodium molybdate and thiourea according to mass ratio 100:15:30, is placed in hydrothermal reaction kettle and carries out hydro-thermal reaction, and the reaction temperature of hydro-thermal is 170 DEG C, and constant temperature time is 25 hours；Solidliquid mixture after hydro-thermal reaction is carried out solid-liquid centrifugation separation, discards liquid, by solid product deionized water wash 4 times, then dry 8 hours at 80 DEG C；By the product grind into powder after drying, obtain MoS2/TiO2Two dimension compound nanometer photocatalyst.
Embodiment 4
According to volume ratio 10:4, butyl titanate and HF being mixed into precursor liquid, is placed in hydrothermal reaction kettle by precursor liquid and carries out hydro-thermal reaction, the temperature of hydro-thermal reaction is 200 DEG C, and constant temperature time is 30 hours；Solidliquid mixture after hydro-thermal reaction is carried out solid-liquid centrifugation separation, discards liquid, by solid product deionized water wash 5 times, then dry 10 hours at 90 DEG C；By the product grind into powder after drying, obtain { the TiO that 001} face exposes2Nano-particle；Will { the TiO that 001} face exposes2Nano-particle is mixed into precursor liquid with sodium molybdate and thiourea according to mass ratio 100:30:60, is placed in hydrothermal reaction kettle and carries out hydro-thermal reaction, and the temperature of hydro-thermal reaction is 200 DEG C, and constant temperature time is 30 hours；Solidliquid mixture after hydro-thermal reaction is carried out solid-liquid centrifugation separation, discards liquid, by solid product deionized water wash 5 times, then dry 10 hours at 90 DEG C；By the product grind into powder after drying, obtain MoS2/TiO2Two dimension compound nanometer photocatalyst.
Embodiment 5
25L butyl titanate and 3L Fluohydric acid. are placed in hydrothermal reaction kettle, 180 DEG C of hydro-thermal reactions 24 hours.After question response still is cooled to room temperature, takes out hydrothermal product, and be sequentially carried out washing, dry, namely obtain { the TiO that 001} face exposes2Nano-particle.
Embodiment 6
600g sodium molybdate and 1200g thiourea are placed in hydrothermal reaction kettle, 180 DEG C of hydro-thermal reactions 24 hours.After question response still is cooled to room temperature, takes out hydrothermal product, and be sequentially carried out washing, dry, namely obtain MoS2Nano-particle.
Fig. 1 is the MoS of embodiment 1 preparation2/TiO2Transmission electron microscope (TEM) figure of two dimension compound nanometer photocatalyst.From figure 1 it appears that the MoS of embodiment 1 preparation2/TiO2Two dimension compound nanometer photocatalyst is two dimension shell karyomorphism looks, and lattice demarcates the MoS confirming two dimension2It is wrapped in TiO2Nanometer sheet forms Two-dimensional Composites.
Fig. 2 is the MoS of embodiment 5, embodiment 6 and embodiment 2 preparation2/TiO2X-ray diffraction (XRD) comparison diagram of two dimension compound nanometer photocatalyst；From figure 2 it can be seen that the MoS of embodiment 2 preparation2/TiO2Two dimension compound nanometer photocatalyst is pure Anatase structure.
Fig. 3 is the MoS of embodiment 5, embodiment 6 and embodiment 3 preparation2/TiO2Ultraviolet-visible (UV-Vis) the absorption spectrum comparison diagram of two dimension compound nanometer photocatalyst；As can be seen from Figure 3: the MoS of embodiment 3 preparation2/TiO2Two dimension compound nanometer photocatalyst spectral absorption situation is between embodiment 5 and embodiment 6.
Fig. 4 is the MoS of embodiment 4 preparation2/TiO2X-ray photoelectron power spectrum (XPS) figure of two dimension compound nanometer photocatalyst；As can be seen from Figure 4: the MoS of embodiment 4 preparation2/TiO2Two dimension compound nanometer photocatalyst contains Mo.
Fig. 5 is the MoS of embodiment 5, embodiment 6 and embodiment 2 preparation2/TiO2Two dimension compound nanometer photocatalyst degradation effect comparison diagram to aqueous dye solutions methylene blue under light illumination；As can be seen from Figure 5: the MoS of embodiment 2 preparation2/TiO2Two dimension compound nanometer photocatalyst photocatalysis performance is greatly improved.
Claims (5)
1. a MoS2/TiO2Two dimension compound nanometer photocatalyst, it is characterised in that: having the pure Anatase structure of shell mould, its kernel is TiO2Nanometer sheet, shell is MoS2, specific surface area is 110m2/g。
2. the MoS prepared described in claim 12/TiO2The method of two dimension compound nanometer photocatalyst, it is characterised in that comprise the following steps: butyl titanate and HF are carried out hydro-thermal reaction, prepares { the TiO that 001} face exposes2Nano-particle；Then will the { TiO that 001} face exposes2Nano-particle carries out hydro-thermal reaction together with sodium molybdate and thiourea, and wherein, the mass ratio of sodium molybdate and thiourea is 1:2；Solid product is dried, grind into powder, obtain the MoS described in claim 12/TiO2Two dimension compound nanometer photocatalyst.
3. method according to claim 2, it is characterised in that specifically include following steps:
(1) by butyl titanate and HF 10:(1～4 by volume) mix homogeneously, it is placed in hydrothermal reaction kettle and carries out incubation water heating reaction, the temperature of hydro-thermal reaction is 150～200 DEG C, and the time of hydro-thermal reaction is 15～30 hours；
(2) solidliquid mixture after step (1) hydro-thermal reaction is carried out solid-liquid centrifugation separation, discard liquid, by solid product deionized water wash 2～5 times, then dry 6～10 hours at 60～90 DEG C；
(3) the product grind into powder after step (2) being dried, obtains { the TiO that 001} face exposes2Nano-particle；
(4) will { TiO that 001} face exposes2Nano-particle and sodium molybdate and thiourea 100:(3～30 in mass ratio): (6～60) mix homogeneously, wherein, the mass ratio of sodium molybdate and thiourea is 1:2, it is placed in hydrothermal reaction kettle and carries out incubation water heating reaction, the temperature of hydro-thermal reaction is 150～200 DEG C, and the time of hydro-thermal reaction is 15～30 hours；
(5) solidliquid mixture after step (4) hydro-thermal reaction is carried out solid-liquid centrifugation separation, discard liquid, by solid product deionized water wash 2～5 times, then dry 6～10 hours at 60～90 DEG C；
(6) the product grind into powder after step (5) being dried, obtains the MoS described in claim 12/TiO2Two dimension compound nanometer photocatalyst.
4. the MoS described in claim 12/TiO2Two dimension compound nanometer photocatalyst application in catalytic field.
5. the MoS described in claim 12/TiO2Two dimension compound nanometer photocatalyst application in environmental pollution improvement.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106423217A (en) * | 2016-09-18 | 2017-02-22 | 南昌航空大学 | Preparing method for TiO2/MoS2/Au/Cu composite photocatalyst for preparing hydrogen |
| CN106513019A (en) * | 2016-09-19 | 2017-03-22 | 长沙学院 | Process for preparing TiO2 two-dimensional flake-like composite photocatalytic material with MoS2 / exposed (001) surface |
| CN106824229A (en) * | 2017-01-18 | 2017-06-13 | 盱眙县中材凹凸棒石粘土有限公司 | A kind of preparation method and application of attapulgite/vulcanization molybdenum composite material |
| CN106902846A (en) * | 2017-03-20 | 2017-06-30 | 中国科学院宁波材料技术与工程研究所 | A kind of hollow TiO2/MoS2Composite and preparation method thereof |
| CN107138169A (en) * | 2017-04-25 | 2017-09-08 | 杭州电子科技大学 | A kind of two-dimentional sulfide nano junction hydrogen production photocatalyst of low cost with and its preparation method and application |
| CN107297214A (en) * | 2017-07-06 | 2017-10-27 | 陕西科技大学 | A kind of preparation method of the titanium dioxide composite photocatalyst of molybdenum disulfide modification |
| CN108181366A (en) * | 2017-12-13 | 2018-06-19 | 河南大学 | Using titanium dioxide-molybdenum disulfide-gold trielement composite material as the construction method of the optical electro-chemistry aptamer sensor of stent |
| CN109465018A (en) * | 2017-09-07 | 2019-03-15 | 中国科学院大连化学物理研究所 | A kind of preparation method of nanoscale load type molybdenum sulfide catalyst |
| CN110038592A (en) * | 2019-04-25 | 2019-07-23 | 南昌航空大学 | A kind of Ce2S3/TiO2The preparation method of nanometer sheet compound photochemical catalyst |
| CN111471189A (en) * | 2020-05-11 | 2020-07-31 | 武汉大学 | Three-dimensional frame material constructed by connecting molybdenum disulfide through two-connection ligand and preparation method |
| CN112774695A (en) * | 2021-01-28 | 2021-05-11 | 南京大学 | Direct Z-type heterojunction photocatalyst capable of being used for decomposing water and preparation method thereof |
| CN114733503A (en) * | 2022-04-29 | 2022-07-12 | 合肥职业技术学院 | hydrotalcite/TiO loaded diatomite2/MoS2Composite photocatalyst and preparation method and application thereof |
| CN114931936A (en) * | 2022-05-19 | 2022-08-23 | 西南科技大学 | 1T-MoS 2 /TiO 2 Preparation and application of/rGO composite photocatalytic material |
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| CN106423217B (en) * | 2016-09-18 | 2019-01-22 | 南昌航空大学 | A kind of hydrogen manufacturing TiO2/MoS2The preparation method of/Au/Cu compound photochemical catalyst |
| CN106423217A (en) * | 2016-09-18 | 2017-02-22 | 南昌航空大学 | Preparing method for TiO2/MoS2/Au/Cu composite photocatalyst for preparing hydrogen |
| CN106513019A (en) * | 2016-09-19 | 2017-03-22 | 长沙学院 | Process for preparing TiO2 two-dimensional flake-like composite photocatalytic material with MoS2 / exposed (001) surface |
| CN106824229A (en) * | 2017-01-18 | 2017-06-13 | 盱眙县中材凹凸棒石粘土有限公司 | A kind of preparation method and application of attapulgite/vulcanization molybdenum composite material |
| CN106824229B (en) * | 2017-01-18 | 2019-04-30 | 盱眙县中材凹凸棒石粘土有限公司 | A kind of preparation method and application of attapulgite/vulcanization molybdenum composite material |
| CN106902846A (en) * | 2017-03-20 | 2017-06-30 | 中国科学院宁波材料技术与工程研究所 | A kind of hollow TiO2/MoS2Composite and preparation method thereof |
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| CN107138169A (en) * | 2017-04-25 | 2017-09-08 | 杭州电子科技大学 | A kind of two-dimentional sulfide nano junction hydrogen production photocatalyst of low cost with and its preparation method and application |
| CN107138169B (en) * | 2017-04-25 | 2020-03-03 | 杭州电子科技大学 | Two-dimensional sulfide nano-junction hydrogen production photocatalyst, and preparation method and application thereof |
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| CN109465018B (en) * | 2017-09-07 | 2021-12-07 | 中国科学院大连化学物理研究所 | Preparation method of nano-scale supported molybdenum sulfide catalyst |
| CN108181366A (en) * | 2017-12-13 | 2018-06-19 | 河南大学 | Using titanium dioxide-molybdenum disulfide-gold trielement composite material as the construction method of the optical electro-chemistry aptamer sensor of stent |
| CN110038592A (en) * | 2019-04-25 | 2019-07-23 | 南昌航空大学 | A kind of Ce2S3/TiO2The preparation method of nanometer sheet compound photochemical catalyst |
| CN111471189B (en) * | 2020-05-11 | 2021-06-15 | 武汉大学 | Three-dimensional frame material constructed by connecting molybdenum disulfide through two-connection ligand and preparation method |
| CN111471189A (en) * | 2020-05-11 | 2020-07-31 | 武汉大学 | Three-dimensional frame material constructed by connecting molybdenum disulfide through two-connection ligand and preparation method |
| CN112774695A (en) * | 2021-01-28 | 2021-05-11 | 南京大学 | Direct Z-type heterojunction photocatalyst capable of being used for decomposing water and preparation method thereof |
| CN112774695B (en) * | 2021-01-28 | 2021-12-17 | 南京大学 | Direct Z-type heterojunction photocatalyst capable of being used for decomposing water and preparation method thereof |
| CN114733503A (en) * | 2022-04-29 | 2022-07-12 | 合肥职业技术学院 | hydrotalcite/TiO loaded diatomite2/MoS2Composite photocatalyst and preparation method and application thereof |
| CN114931936A (en) * | 2022-05-19 | 2022-08-23 | 西南科技大学 | 1T-MoS 2 /TiO 2 Preparation and application of/rGO composite photocatalytic material |
| CN114931936B (en) * | 2022-05-19 | 2024-01-30 | 西南科技大学 | Preparation and application of MoS2/TiO2/rGO composite photocatalytic material |
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