CN106040262A - Preparation method and application for semiconductor composite nanometer material photocatalyst - Google Patents
Preparation method and application for semiconductor composite nanometer material photocatalyst Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 239000000463 material Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 11
- 239000004065 semiconductor Substances 0.000 title claims abstract description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 41
- 230000001699 photocatalysis Effects 0.000 claims abstract description 17
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims abstract description 8
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 claims abstract description 8
- 229940012189 methyl orange Drugs 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 5
- APQHKWPGGHMYKJ-UHFFFAOYSA-N Tributyltin oxide Chemical compound CCCC[Sn](CCCC)(CCCC)O[Sn](CCCC)(CCCC)CCCC APQHKWPGGHMYKJ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229940106691 bisphenol a Drugs 0.000 claims abstract description 4
- 239000000975 dye Substances 0.000 claims abstract description 3
- 239000003344 environmental pollutant Substances 0.000 claims abstract description 3
- 231100000719 pollutant Toxicity 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 238000006555 catalytic reaction Methods 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 229920002415 Pluronic P-123 Polymers 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000002086 nanomaterial Substances 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 6
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 6
- 238000007146 photocatalysis Methods 0.000 claims description 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- 229910052793 cadmium Inorganic materials 0.000 claims description 3
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 3
- CXKCTMHTOKXKQT-UHFFFAOYSA-N cadmium oxide Chemical compound [Cd]=O CXKCTMHTOKXKQT-UHFFFAOYSA-N 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 3
- 238000009415 formwork Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 229940002712 malachite green oxalate Drugs 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 229920000428 triblock copolymer Polymers 0.000 claims description 3
- 239000006227 byproduct Substances 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims description 2
- -1 rose-red Chemical compound 0.000 claims description 2
- 229910052980 cadmium sulfide Inorganic materials 0.000 abstract description 23
- 230000015556 catabolic process Effects 0.000 abstract description 20
- 238000006731 degradation reaction Methods 0.000 abstract description 20
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 abstract description 14
- 239000004408 titanium dioxide Substances 0.000 abstract description 12
- 230000007613 environmental effect Effects 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- 229910004874 Na2S 9H2O Inorganic materials 0.000 abstract description 2
- 238000006303 photolysis reaction Methods 0.000 abstract description 2
- 230000001954 sterilising effect Effects 0.000 abstract description 2
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 2
- 238000000802 evaporation-induced self-assembly Methods 0.000 abstract 2
- IICCLYANAQEHCI-UHFFFAOYSA-N 4,5,6,7-tetrachloro-3',6'-dihydroxy-2',4',5',7'-tetraiodospiro[2-benzofuran-3,9'-xanthene]-1-one Chemical compound O1C(=O)C(C(=C(Cl)C(Cl)=C2Cl)Cl)=C2C21C1=CC(I)=C(O)C(I)=C1OC1=C(I)C(O)=C(I)C=C21 IICCLYANAQEHCI-UHFFFAOYSA-N 0.000 abstract 1
- 125000004122 cyclic group Chemical group 0.000 abstract 1
- FDZZZRQASAIRJF-UHFFFAOYSA-M malachite green Chemical compound [Cl-].C1=CC(N(C)C)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](C)C)C=C1 FDZZZRQASAIRJF-UHFFFAOYSA-M 0.000 abstract 1
- 229940107698 malachite green Drugs 0.000 abstract 1
- 230000015843 photosynthesis, light reaction Effects 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 229940081623 rose bengal Drugs 0.000 abstract 1
- 229930187593 rose bengal Natural products 0.000 abstract 1
- STRXNPAVPKGJQR-UHFFFAOYSA-N rose bengal A Natural products O1C(=O)C(C(=CC=C2Cl)Cl)=C2C21C1=CC(I)=C(O)C(I)=C1OC1=C(I)C(O)=C(I)C=C21 STRXNPAVPKGJQR-UHFFFAOYSA-N 0.000 abstract 1
- 238000003980 solgel method Methods 0.000 abstract 1
- 229940116367 cadmium sulfide Drugs 0.000 description 13
- 239000003054 catalyst Substances 0.000 description 6
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 6
- 239000002096 quantum dot Substances 0.000 description 5
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 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 1
- 230000001413 cellular effect Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000029219 regulation of pH Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 239000003403 water pollutant Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- 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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The invention provides a preparation method and application for a semiconductor composite nanometer material photocatalyst. According to the invention, a sol-gel method is adopted to synthesize a mesoporous titanium dioxide composite photocatalytic material, and with tetra-n-butyl titanate TBOT, Cd(NO3)2-4H2O and Na2S-9H2O as main raw materials, a cadmium sulfide/titanium dioxide mesoporous composite photocatalytic material is prepared by one step through an evaporation induced self-assembly (EISA) method. Meanwhile, simulated sunlight is utilized to test performances of the prepared material, and through degradation of organic dyes and pollutants like methyl orange, rose bengal, bisphenol A and malachite green, supernormal photocatalytic performance of the material is testified. After cyclic degradation of the methyl orange for five times, a certain photocatalytic activity can be showed under visible light. The composite material belongs to an inorganic photocatalytic material and has the advantages of stable performance, high photocatalytic activity, chemical and photocorrosion resistance, and important significances in the fields of water photolysis, sterilization, preparation of sensitized solar cells, environmental protection, etc.
Description
Technical field
The invention belongs to optic catalytic composite material preparation field, particularly to a kind of semiconductor composite nano material light catalysis
The preparation method and applications of agent.
Background technology
Along with the extensive style of domestic industry develops and social developing rapidly, industry and the increasing of urban waste discharge
Adding, the problem of water pollution becomes increasingly conspicuous.Difficult degradation organic contamination such as EDCs, POPs, PPCPs etc. of some trace can not be by
Conventional traditional water treatment system is effectively removed, and titanium dioxide is nontoxic, stable performance, is a kind of important inorganic material, its
There is higher refraction coefficient and stable physical and chemical performance, and it is high, right to have anti-chemistry and photoetch, photocatalytic activity
The advantage such as organic matter degradation non-selectivity, thorough, the non-secondary pollution of mineralising, TiO in water pollutant2It is widely used for photodissociation
Water, sterilize and prepare solar energy sensitized cells etc., particularly in terms of environmental conservation, TiO2Present especially as photocatalyst
Wide application prospect.This composite photo-catalyst demonstrates that in test experiments the photocatalysis performance of excellence and separation and recovery repeat
, there is potential using value in utility, processes waste water for following heavy industrialization application and make theoretical place mat.
The present invention is by adding cadmiumsulfide quantum dot in titanium dioxide, making this composite have excellent photocatalytic
Can, prepare the catalysis material that combination property is superior.
Summary of the invention
It is an object of the invention to provide the preparation method and applications of a kind of semiconductor composite nano material light catalysis agent, use
Requirement with satisfied solution environmental problem.
The present invention is achieved like this, and concrete preparation method is as follows:
(1) weigh the triblock copolymer pluronic P123 of 0.5-2.0g, be dissolved in 15ml dehydrated alcohol, room
0.5-1h is stirred, then supersound process 5-20min under temperature；
(2) simultaneously, in another beaker, the concentrated hydrochloric acid of 2-4ml is added dropwise to the tetra-n-butyl titanate TBOT solution of 4.0g
In, and add a certain amount of Cd (NO3)2·4H2(this experiment comprises four groups to O, by controlling Cd (NO3)2·4H2The consumption of O, and
It is converted into the quality of CdO, is made CdO/TiO2Mass ratio be respectively 1%, 2%, 4%, and 8%), corresponding subsequently add
Equimolar Na2S·9H2O；
(3) mix with above-mentioned solution after P123/EtOH mixed solution stirring 0.5-1h, under room temperature, stir at least 6h energetically,
Being poured into by the sol solution of synthesis in a unlimited culture dish, keeping ambient humidity, light and temperature is 50% 60%, the most quiet
Put surrounding；
(4) after it becomes wet powder, at 170-220 DEG C, calcine 4h carry out rock-steady structure；
(5) grinding after, make powder reflux in ethylenediamine solution 48h, temperature is maintained at 100-130 DEG C, PH regulation
11 12, reflux complete, be centrifuged and be washed with deionized, by product at 50-70 DEG C of dry 12h；
(6) subsequently, gained powder is first ground, then N at 320-360 DEG C2Middle calcining 2-4h makes meso-hole structure stable；
(7) the last 2h that calcines in air at 480-520 DEG C removes organic formwork and improves degree of crystallinity.
The quality pressing Aska-Rid. in described step (2) is calculated, and makes CdO/TiO2Mass ratio be respectively 1%, 2%, 4%,
And 8%.The molal quantity of Na2S 9H2O is equal with the molal quantity of the cadmium added respectively.
This described composite catalyzing material demonstrates photocatalysis performance and the separation and recovery recycling performance of excellence, permissible
Multiple organic dyestuff and the pollutant such as degraded methyl orange, rose-red, bisphenol-A, malachite green oxalate, circulate five times under simulated solar irradiation
After degraded methyl orange, moreover it is possible to show certain photocatalytic activity under visible light.
Advantages of the present invention: cadmiumsulfide quantum dot, from the angle of composite, is embedded into titanium dioxide by the present invention
In, prepare a kind of composite photocatalyst material.This composite photocatalyst material is compared with pure titinium dioxide, under simulated solar irradiation
There is higher photocatalysis performance.There is higher refraction coefficient and stable physical and chemical performance, and anti-chemistry and light rotten
Erosion, photocatalytic activity higher.Additionally, the most certain stability, by five degraded methyl oranges of circulation, its catalytic effect does not has yet
Have and at all weaken, after circulating three times, remain to methyl orange of degrading under visible light.Making therefore, this composite is in photocatalytic water, sterilization
With prepare the aspects such as solar energy sensitized cells, particularly in terms of environmental conservation, have broad application prospects.
Accompanying drawing explanation
Fig. 1 is degraded methyl orange solution efficiency chart；
Fig. 2 is 2%CdS/TiO2SEM figure.
Detailed description of the invention
Below by embodiment, the invention will be further described.
Embodiment 1
(1) weigh the triblock copolymer pluronic P123 of 1.0g, be dissolved in 15ml dehydrated alcohol, under room temperature
Stirring 0.5h, then supersound process 10min.
(2) simultaneously, in another beaker, the concentrated hydrochloric acid of 3.2ml is added dropwise to the tetra-n-butyl titanate TBOT solution of 4.0g
In, and add the Cd (NO of 0.0225g3)2·4H2O is (by controlling Cd (NO3)2·4H2The consumption of O, and it is converted into CdO's
Quality, makes CdO/TiO2Mass ratio be 1%), be subsequently added equimolar Na2S·9H2O i.e. 0.0176g.
(3) mix with above-mentioned solution after P123/EtOH mixed solution stirring 0.5h, under room temperature, stir at least 6h energetically.Will
The sol solution of synthesis is poured in a unlimited culture dish, and keeping ambient humidity, light and temperature is 50% 60%, stands at room temperature
Several weeks.
(4) after it becomes wet powder, at 200 DEG C, calcine 4h carry out rock-steady structure.
(5) grinding after, make powder reflux in ethylenediamine solution 48h, temperature is maintained at 125 DEG C, and PH regulates and exists
11——12.Reflux complete, be centrifuged and be washed with deionized, product is drying over night at 60 DEG C.
(6) subsequently, gained powder is first ground, then N at 350 DEG C2Middle calcining 3h makes meso-hole structure stable.
(7) the last 2h that calcines in air at 500 DEG C removes organic formwork and improves degree of crystallinity, obtains cadmium sulfide/bis-
Titanium oxide composite photocatalyst material.Take 50mg cadmium sulfide/titanium dioxide CdS/TiO2It is used for, under simulated solar irradiation, the 50ml that degrades
The methyl orange solution of 10PPm, after 75min, degradation rate reaches 100%.
Embodiment 2
Embed the preparation of mesoporous TiO 2 composite photocatalyst material of cadmiumsulfide quantum dot with step in embodiment 1, step
(2) add the Cd (NO of 0.0451g suddenly3)2·4H2O (makes the CdO/TiO prepared2Mass ratio be 2%) and 0.0351g
Na2S·9H2O, prepares cadmium sulfide/titanium dioxide CdS/TiO2Composite.Take 50mg cadmium sulfide/titanium dioxide CdS/TiO2
For the methyl orange solution of the 50ml 10PPm that degrades under simulated solar irradiation, after 30min, degradation rate reaches 100%.
Embodiment 3
Embed the preparation of mesoporous TiO 2 composite photocatalyst material of cadmiumsulfide quantum dot with step in embodiment 1, step
(2) add the Cd (NO of 0.0902g suddenly3)2·4H2O (makes the CdO/TiO prepared2Mass ratio be 4%) and 0.0702g
Na2S·9H2O, prepares cadmium sulfide/titanium dioxide CdS/TiO2Composite.Take 50mg cadmium sulfide/titanium dioxide CdS/TiO2
For the methyl orange solution of the 50ml 10PPm that degrades under simulated solar irradiation, after 60min, degradation rate reaches 100%.
Embodiment 4
Embed the preparation of mesoporous TiO 2 composite photocatalyst material of cadmiumsulfide quantum dot with step in embodiment 1, step
(2) add the Cd (NO of 0.1804g suddenly3)2·4H2O (makes the CdO/TiO prepared2Mass ratio be 8%) and 0.1404g
Na2S·9H2O, prepares cadmium sulfide/titanium dioxide CdS/TiO2Composite.Take 50mg cadmium sulfide/titanium dioxide CdS/TiO2
For the methyl orange solution of the 50ml 10PPm that degrades under simulated solar irradiation, after 65min, degradation rate reaches 100%.
As seen from Figure 1 in four groups of parallel tests, make CdO/TiO when the cadmium content added is converted into Aska-Rid.2Quality
Than when being 2%, the catalytic performance of this composite is best.
The methylene blue 15min degradation rate of 50mg this catalyst degradation 50ml 5mg/L reaches 100%.
The rose-red 30min degradation rate of 50mg this catalyst degradation 50ml 10ppm reaches 100%.
The bisphenol-A 75min degradation rate of 50mg this catalyst degradation 50ml 10ppm reaches 100%.
The malachite green oxalate 15min degradation rate of 50mg this catalyst degradation 50ml 20ppm reaches 100%.
The methyl orange of 50mg this catalyst degradation 50ml 10ppm, after five times circulate, degradation rate remains to when 30min
Reach 100%.This catalyst after 50mg tri-times circulation is degraded the methyl orange solution of 50ml 10PPm under visible light, after 60min,
Degradation rate reaches 100%.
Fig. 2 is 2%CdS/TiO2SEM figure, figure it is cellular for being clearly visible prepared sample, say, that institute
Preparation sample be porous nanometer structure, exactly because this structure, when degradation of contaminant could preferably with the thing that is degraded
It is fully contacted, contributes to carrying out sufficient photocatalytic redox reaction.
Claims (3)
1. the preparation method of a semiconductor composite nano material light catalysis agent, it is characterised in that the system of this composite photocatalyst material
For comprising the steps of
(1) weigh the triblock copolymer pluronic P123 of 0.5-2.0g, be dissolved in 15ml dehydrated alcohol, under room temperature
Stirring 0.5-1h, then supersound process 5-20min；
(2) simultaneously, in another beaker, the concentrated hydrochloric acid of 2-4ml is added dropwise in the tetra-n-butyl titanate TBOT solution of 4.0g,
And add a certain amount of Cd (NO3)2·4H2O, the subsequently equimolar Na of corresponding addition2S·9H2O；
(3) mix with above-mentioned solution after P123/EtOH mixed solution stirring 0.5-1h, under room temperature, stir at least 6h energetically, will close
The sol solution become is poured in a unlimited culture dish, and keeping ambient humidity, light and temperature is 50% 60%, stands four at room temperature
Week；
(4) after it becomes wet powder, at 170-220 DEG C, calcine 4h carry out rock-steady structure；
(5) grinding after, make powder reflux in ethylenediamine solution 48h, temperature is maintained at 100-130 DEG C, and PH regulates and exists
11 12, reflux complete, be centrifuged and be washed with deionized, by product at 50-70 DEG C of dry 12h；
(6) subsequently, gained powder is first ground, then N at 320-360 DEG C2Middle calcining 2-4h makes meso-hole structure stable；
(7) the last 2h that calcines in air at 480-520 DEG C removes organic formwork and improves degree of crystallinity.
2. according to the preparation method of a claim 1 semiconductor composite nano material light catalysis agent, it is characterised in that: described
The quality pressing Aska-Rid. in step (2) is calculated, and makes CdO/TiO2Mass ratio be respectively 1%, 2%, 4%, and 8%.Na2S·
The molal quantity of 9H2O is equal with the molal quantity of the cadmium added respectively.
3. an application for the preparation method of a kind of semiconductor composite nano material light catalysis agent described in claim 1, it is special
Levy and be: this described composite catalyzing material demonstrates photocatalysis performance and the separation and recovery recycling performance of excellence, permissible
Multiple organic dyestuff and the pollutant such as degraded methyl orange, rose-red, bisphenol-A, malachite green oxalate, circulate five times under simulated solar irradiation
After degraded methyl orange, moreover it is possible to show certain photocatalytic activity under visible light.
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| CN105107489A (en) * | 2015-08-25 | 2015-12-02 | 南昌航空大学 | Method for preparing CdS/TiO2 mesoporous composite photocatalytic material |
| CN105363477A (en) * | 2015-10-23 | 2016-03-02 | 南昌航空大学 | Method for preparing silver/cadmium sulfide/titanium dioxide composite photocatalytic material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101306357A (en) * | 2007-05-16 | 2008-11-19 | 北京化工大学 | Binary nano composite photo-catalyst preparation method |
| CN105107489A (en) * | 2015-08-25 | 2015-12-02 | 南昌航空大学 | Method for preparing CdS/TiO2 mesoporous composite photocatalytic material |
| CN105363477A (en) * | 2015-10-23 | 2016-03-02 | 南昌航空大学 | Method for preparing silver/cadmium sulfide/titanium dioxide composite photocatalytic material |
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Application publication date: 20161026 |