CN106799238A - Converting photocatalysis material and preparation method thereof on a kind of CdS bases green glow - Google Patents
Converting photocatalysis material and preparation method thereof on a kind of CdS bases green glow Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 72
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 46
- 238000007146 photocatalysis Methods 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 24
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 24
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 24
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000005642 Oleic acid Substances 0.000 claims abstract description 24
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 24
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 24
- VFMUXPQZKOKPOF-UHFFFAOYSA-N 2,3,7,8,12,13,17,18-octaethyl-21,23-dihydroporphyrin platinum Chemical compound [Pt].CCc1c(CC)c2cc3[nH]c(cc4nc(cc5[nH]c(cc1n2)c(CC)c5CC)c(CC)c4CC)c(CC)c3CC VFMUXPQZKOKPOF-UHFFFAOYSA-N 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 41
- 239000008367 deionised water Substances 0.000 claims description 38
- 229910021641 deionized water Inorganic materials 0.000 claims description 38
- 239000000243 solution Substances 0.000 claims description 36
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 28
- 239000007864 aqueous solution Substances 0.000 claims description 15
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 12
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical class CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000004530 micro-emulsion Substances 0.000 claims description 10
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 9
- 238000005119 centrifugation Methods 0.000 claims description 9
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical class CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 6
- 150000001412 amines Chemical class 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- YKYOUMDCQGMQQO-UHFFFAOYSA-L Cadmium chloride Inorganic materials Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims 2
- 229910052697 platinum Inorganic materials 0.000 claims 2
- 150000004032 porphyrins Chemical class 0.000 claims 2
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 claims 1
- 229910000077 silane Inorganic materials 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 125000000446 sulfanediyl group Chemical group *S* 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 8
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 5
- 238000012546 transfer Methods 0.000 abstract description 5
- 229910052724 xenon Inorganic materials 0.000 abstract description 5
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- -1 rare earth fluoride Chemical class 0.000 abstract description 4
- 230000003595 spectral effect Effects 0.000 abstract description 4
- 239000004098 Tetracycline Substances 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 7
- 238000006555 catalytic reaction Methods 0.000 description 7
- 229960002180 tetracycline Drugs 0.000 description 7
- 229930101283 tetracycline Natural products 0.000 description 7
- 235000019364 tetracycline Nutrition 0.000 description 7
- 150000003522 tetracyclines Chemical class 0.000 description 7
- 238000001228 spectrum Methods 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000001934 delay Effects 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 2
- 229910002915 BiVO4 Inorganic materials 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- LRNIARMLUQJSEP-UHFFFAOYSA-N [Pt].C(C)C1=C2NC(=C1)C=C1C=CC(=N1)C=C1C=CC(N1)=CC=1C=CC(N1)=C2 Chemical compound [Pt].C(C)C1=C2NC(=C1)C=C1C=CC(=N1)C=C1C=CC(N1)=CC=1C=CC(N1)=C2 LRNIARMLUQJSEP-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical compound CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical group CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
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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
-
- 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
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Abstract
The present invention relates to converting photocatalysis material on a kind of CdS bases green glow and preparation method thereof, sensitizer used in the present invention is octaethylporphyrin platinum, and acceptor is 9,10 diphenylanthrancenes.Compared with converting photocatalysis technology on rare earth fluoride, the spectral absorption wide ranges of CdS base green glow up-conversions in the present invention, upper conversion excites threshold values low, and just good upper conversion and photocatalysis effect can be produced in the case where common xenon lamp green light band is excited.With with oleic acid as core, structure it is identical, in the absence of green glow upper conversion function CdS base optic catalytic materials compared with, converting photocatalysis material buries in oblivion upper transfer process low energy green photons is converted near ultraviolet high-energy photon by triplet state triplet state on CdS base green glows, substantially increases utilization ratios of the CdS to low energy green photons.
Description
Technical field
The present invention relates to field of photocatalytic material, and in particular to converting photocatalysis material and its system on a kind of CdS bases green glow
Preparation Method.
Background technology
With the rapid propulsion of social process of industrialization, using the organic pollution in photocatalysis technology decomposition water (as resisted
Raw element, dyestuff etc.) receive extensive concern.With TiO2, ZnO etc. ground for the wide bandgap semiconductor photochemical catalyst of representative extensively
Study carefully.But ultraviolet light only accounts for the 5% of sunshine gross energy, wide bandgap semiconductor photochemical catalyst generally existing quantum efficiency is low to ask
Topic, does not reach the requirement of industrialization large-scale application.Therefore, researcher begins to focus on low-gap semiconductor photochemical catalyst (such as
C3N4、BiVO4, CdS etc.), to carry out fully absorbing utilization to visible ray and near infrared light.Wherein, the active high, systems of CdS
The excellent characteristic, the potentiality with heavy industrialization application such as standby process is simple, spectral response range be wide.
Research shows that wide spectrum responding ability does not necessarily mean that bloom catalytic reaction activity.In photochemical catalyst to short
The high-energy photon of wavelength and the lower energy photon of long wavelength have a case that under equal absorbability that high-energy photon compares lower energy photon
Light-catalyzed reaction is promoted with ability higher, efficiency can also be substantially improved.It can be seen that, fully widening photochemical catalyst spectral absorption
On the basis of scope, lower energy photon is converted into photochemical catalyst, and to can absorb the high-energy photon that utilizes very necessary.It is upper to turn based on this
Change catalysis material and have received extensive concern.At present, the upper conversion function matrix in upper converting photocatalysis material is mainly rare earth
Fluoride (such as NaYF4:Yb,Tm、NaGdF4:Yb, Er etc.), the absorption cross section of this kind of material generally existing rare earth sensitized ions
It is small by (about 10-22cm2), excitation threshold (more than about 3 orders of magnitude typically higher than sunlight intensity) high, photon are changed on two-photon
The low deficiency of conversion efficiency, practical application efficiency is low.
Triplet state-triplet state annihilation up-conversion luminescence can excite the lower significant anti-Stokes of presentation to make in low-power
With compared with the upper transfer process of rare earth fluoride, conversion has absorption cross section big (about 10 in triplet state-triplet state annihilation-17cm2), low excitation threshold and the advantages of quantum yield high.
In lower energy photon of the wavelength more than 500nm, green glow has a highest photon energy, but CdS to its utilization rate very
It is low.Low energy green photons are converted to by ultraviolet or near ultraviolet high-energy photon by transfer process in triplet state-triplet state annihilation,
It is expected to further improve the photocatalysis efficiency of CdS.So far, there is not yet based on converted in triplet state-triplet state annihilation
Preparing crafts and application study of the Cheng Tigao CdS to green glow utilization ratio catalysis material.
The content of the invention
It is an object of the invention to provide converting photocatalysis material on a kind of CdS bases green glow and preparation method thereof.
Sensitizer in triplet state-triplet state annihilation of the present invention used in transfer process is octaethylporphyrin
Platinum, acceptor is 9,10- diphenylanthrancenes.
The present invention provide technical scheme be：
A kind of converting photocatalysis material on CdS bases green glow, preparation method is comprised the following steps：
(1) tetrahydrofuran solution of octaethylporphyrin platinum and the tetrahydrofuran solution of 9,10- diphenylanthrancenes are respectively configured；
(2) take the octaethylporphyrin platinum solution in step (1) and 9,10- diphenylanthrancene solution are scattered in oleic acid, drying
Being placed in case makes tetrahydrofuran volatilize completely, and the concentration of octaethylporphyrin platinum is 0.2mmol/L-2mol/L, eight in final oleic acid
The mol ratio of ethyl porphyrin platinum and 9,10- diphenylanthrancenes is 1:2-1:10；
(3) oleic acid solutions in step (2) are taken in deionized water, microemulsion is formed by ultrasonic disperse；
(4) to addition 3- aminopropyl trimethoxysilanes or 3- aminopropyl triethoxysilanes in the microemulsion of step (3)；
(5) to tetraethyl orthosilicate is slowly added in the solution of step (4), the mixed solution of gained is at 45 DEG C -60 DEG C
It is slowly stirred 36h；The material of gained is washed with deionized water, and in 60 DEG C of vacuum drying, obtains changing work(on green glow
Can material；
(6) the green glow upper conversion function material in step (5) is scattered in ethanol, adds a certain amount of 3- aminopropyls three
Methoxy silane or 3- aminopropyl triethoxysilanes, are stirred at room temperature 12h, using deionized water centrifugation, washing；
(7) material in step (6) is distributed to CdCl2In the aqueous solution, 4h is stirred at room temperature, be centrifuged using deionized water,
Washing；
(8) material of gained in step (7) is distributed in thioacetyl amine aqueous solution, 24h is stirred at room temperature, using go from
Sub- water is centrifuged to converting photocatalysis material on the CdS base green glows of gained, is washed, and is finally vacuum dried 24h at 60 DEG C.
In step (1), the concentration of octaethylporphyrin platinum solution is 1mmol/L-10mmol/L；9,10- diphenylanthrancene solution
Concentration be 1mmol/L-10mmol/L.
In step (2), oleic acid solutions place 12h in 75 DEG C of baking oven makes tetrahydrofuran volatilize completely.
In step (3), the volume ratio of oleic acid solutions and deionized water is 1:100-1:500.
In step (4), 3- aminopropyl trimethoxysilanes or 3- aminopropyl triethoxysilanes with gone step (3) described from
The mass ratio of sub- water is 1:500.
In step (5), the mass ratio of tetraethyl orthosilicate and step (3) described deionized water is 1:30-1:100.
In step (6), 0.1mL-1mL 3- aminopropyl front threes are added in every 0.05g-0.2g green glow upper conversion function materials
TMOS or 3- aminopropyl triethoxysilanes.
In step (7), CdCl2The aqueous solution is 20mL, and concentration is 0.1M.
In step (8), thioacetyl amine aqueous solution is 10mL-40mL, and concentration is 0.1M.
Beneficial effect：
The present invention relates to converting photocatalysis material on a kind of CdS bases green glow and preparation method thereof, on rare earth fluoride
Converting photocatalysis technology is compared, and the spectral absorption wide ranges of CdS base green glow up-conversions in the present invention, upper conversion excites threshold values
It is low, just can produce good upper conversion and photocatalysis effect in the case where common xenon lamp green light band is excited.With with oleic acid as core, structure
CdS base optic catalytic materials identical, in the absence of green glow upper conversion function are compared, and converting photocatalysis material passes through on CdS base green glows
Low energy green photons are converted near ultraviolet high-energy photon by transfer process in triplet state-triplet state annihilation, substantially increase CdS pairs
The utilization ratio of low energy green photons.
Brief description of the drawings
Fig. 1 is the SEM photograph of converting photocatalysis material on CdS base green glows in embodiment 1.
Fig. 2 is the abosrption spectrogram of converting photocatalysis material on CdS base green glows in embodiment 1.
Fig. 3 is under converting photocatalysis material different wave length green glow in the xenon lamp spectrum is excited on CdS base green glows in embodiment 1
Up-conversion emission spectrogram.
Fig. 4 is the effect of converting photocatalysis material catalytic degradation tetracycline under green glow irradiation on CdS base green glows in embodiment 1
Rate curve map.
Fig. 5 is photocatalysis green spectrum distribution map.
Specific embodiment
The content of the invention of the invention is further described with reference to the accompanying drawings and examples.
Raw material used in the present invention for analysis is pure and more than, outermost CdS photochemical catalysts are in low temperature even normal temperature
Lower fabricated in situ, size is less than 20nm, good stability.
Using tetracycline as simulation organic pollution, concentration of aqueous solution is 20mg/L, volume for photocatalysis experiment of the invention
It is 100mL；The addition of catalysis material is 0.1g；Light source is 300W xenon lamps (middle religion Jin Yuan), green spectrum used by photocatalysis
Distribution is referring to Fig. 5；The temperature constant state of reactor is kept in photocatalytic process using recirculated cooling water.
Embodiment 1
(1) tetrahydrofuran solution of octaethylporphyrin platinum and 9,10- diphenylanthrancene is respectively configured, concentration is respectively 1mmol/
L and 2mmol/L.
(2) solution taken in step (1) is scattered in oleic acid, and 12h is placed in 75 DEG C of baking oven, makes tetrahydrofuran complete
Volatilization, in final oleic acid the concentration of octaethylporphyrin platinum is 0.25mmol/L, and octaethylporphyrin platinum and 9,10- diphenylanthrancene rub
You are than being 1:3.
(3) oleic acid solutions in step (2) are taken in deionized water, microemulsion, oleic acid solutions is formed by ultrasonic disperse
It is 1 with the volume ratio of deionized water:450.
(4) in the microemulsion of step (3) add 3- aminopropyl trimethoxysilanes, 3- aminopropyl trimethoxysilanes and
The mass ratio of deionized water is 1:500.
(5) to tetraethyl orthosilicate is slowly added in the solution of step (4), the mixed solution of gained is slowly stirred at 50 DEG C
Mix 36h, the mass ratio of tetraethyl orthosilicate and deionized water is 1:90.The material of gained is washed using deionized water,
And in 60 DEG C of vacuum drying, obtain green glow upper conversion function material.
(6) the green glow upper conversion function material in 0.08g steps (5) is scattered in ethanol, adds 0.2mL 3- ammonia third
Base trimethoxy silane, is stirred at room temperature 12h, using deionized water centrifugation, washing.
(7) material in step (6) is distributed to the CdCl that 20mL concentration is 0.1M2In the aqueous solution, 4h is stirred at room temperature, profit
It is centrifuged with deionized water, is washed.
(8) material of gained in step (7) is distributed in the thioacetyl amine aqueous solution that 15mL concentration is 0.1M, room temperature
Stirring 24h, using deionized water centrifugation, washing, 24h is vacuum dried at 60 DEG C, obtains converting photocatalysis material on CdS base green glows.
In embodiment 1, the SEM photograph of converting photocatalysis material is respectively referring to Fig. 1 on gained CdS base green glows.It is with xenon lamp
Light source, on CdS base green glows on the green glow of converting photocatalysis material conversion performance referring to Fig. 2.Converting photocatalysis material on CdS base green glows
The absorption spectrum of material is referring to Fig. 3.Converting photocatalysis material light catalysis degraded on CdS base green glows in this example of conversion promotion on green glow
Referring to Fig. 4, under green glow irradiation, converting photocatalysis material can be catalyzed the efficiency curve of tetracycline in 100min on CdS base green glows
The tetracycline of degraded 45%, and structure is identical, catalysis material without green glow upper conversion function can only photocatalytic degradation
32% tetracycline.
Embodiment 2
(1) tetrahydrofuran solution of octaethylporphyrin platinum and 9,10- diphenylanthrancene is respectively configured, concentration is respectively 3mmol/
L and 6mmol/L.
(2) solution taken in step (1) is scattered in oleic acid, and 12h is placed in 75 DEG C of baking oven, makes tetrahydrofuran complete
Volatilization, in final oleic acid the concentration of octaethylporphyrin platinum is 0.8mmol/L, and octaethylporphyrin platinum and 9,10- diphenylanthrancene rub
You are than being 1:5.
(3) oleic acid solutions in step (2) are taken in deionized water, microemulsion, oleic acid solutions is formed by ultrasonic disperse
It is 1 with the volume ratio of deionized water:300.
(4) in the microemulsion of step (3) add 3- aminopropyl triethoxysilanes, 3- aminopropyl triethoxysilanes and
The mass ratio of deionized water is 1:500.
(5) to tetraethyl orthosilicate is slowly added in the solution of step (4), the mixed solution of final gained delays at 60 DEG C
The mass ratio of slow stirring 36h, tetraethyl orthosilicate and deionized water is 1:70.The material of final gained is entered using deionized water
Row washing, and in 60 DEG C of vacuum drying, obtain green glow upper conversion function material.
(6) the green glow upper conversion function material in 0.12g steps (5) is scattered in ethanol, adds 0.5mL3- aminopropyls
Triethoxysilane, is stirred at room temperature 12h, using deionized water centrifugation, washing.
(7) material in step (6) is distributed to the CdCl that 20mL concentration is 0.1M2In the aqueous solution, 4h is stirred at room temperature, profit
It is centrifuged with deionized water, is washed.
(8) material of gained in step (7) is distributed in the thioacetyl amine aqueous solution that 25mL concentration is 0.1M, room temperature
Stirring 24h, using deionized water centrifugation, washing, 24h is vacuum dried at 60 DEG C, obtains converting photocatalysis material on CdS base green glows.
In example 2, under green glow irradiation, converting photocatalysis material can be in 100min catalytic degradations 60% on CdS base green glows
Tetracycline.
Embodiment 3
(1) tetrahydrofuran solution of octaethylporphyrin platinum and 9,10- diphenylanthrancene is respectively configured, concentration is respectively 4mmol/
L and 8mmol/L.
(2) solution taken in step (1) is scattered in oleic acid, and 12h is placed in 75 DEG C of baking oven, makes tetrahydrofuran complete
Volatilization, in final oleic acid the concentration of octaethylporphyrin platinum is 1.2mmol/L, and octaethylporphyrin platinum and 9,10- diphenylanthrancene rub
You are than being 1:8.
(3) oleic acid solutions in step (2) are taken in deionized water, microemulsion, oleic acid solutions is formed by ultrasonic disperse
It is 1 with the volume ratio of deionized water:150.
(4) in the microemulsion of step (3) add 3- aminopropyl triethoxysilanes, 3- aminopropyl triethoxysilanes and
The mass ratio of deionized water is 1:500.
(5) to tetraethyl orthosilicate is slowly added in the solution of step (4), the mixed solution of final gained delays at 55 DEG C
The mass ratio of slow stirring 36h, tetraethyl orthosilicate and deionized water is 1:40.The material of final gained is entered using deionized water
Row washing, and in 60 DEG C of vacuum drying, obtain green glow upper conversion function material.
(6) the green glow upper conversion function material in 0.18g steps (5) is scattered in ethanol, adds 0.5mL3- aminopropyls
Triethoxysilane, is stirred at room temperature 12h, using deionized water centrifugation, washing.
(7) material in step (6) is distributed to the CdCl that 20mL concentration is 0.1M2In the aqueous solution, 4h is stirred at room temperature, profit
It is centrifuged with deionized water, is washed.
(8) material of gained in step (7) is distributed in the thioacetyl amine aqueous solution that 35mL concentration is 0.1M, room temperature
Stirring 24h, using deionized water centrifugation, washing, 24h is vacuum dried at 60 DEG C, obtains converting photocatalysis material on CdS base green glows.
In example 3, under green glow irradiation, converting photocatalysis material can be in 100min catalytic degradations 74% on CdS base green glows
Tetracycline.
The invention is not restricted to above example.The bound of each parameter, interval value can realize the present invention, herein not one by one
Enumerate.Any those skilled in the art, without departing from the scope of the present invention, according to technology reality of the invention
Matter, any simple modification made to above example, equivalent and improvement etc., still fall within technical solution of the present invention
Within protection domain.
Claims (9)
1. converting photocatalysis material on a kind of CdS bases green glow, it is characterised in that：Preparation method is comprised the following steps：
(1) tetrahydrofuran solution of octaethylporphyrin platinum and the tetrahydrofuran solution of 9,10- diphenylanthrancenes are respectively configured；
(2) take the octaethylporphyrin platinum solution in step (1) and 9,10- diphenylanthrancene solution are scattered in oleic acid, in an oven
Placement makes tetrahydrofuran volatilize completely, and the concentration of octaethylporphyrin platinum is 0.2mmol/L-2mol/L, octaethyl in final oleic acid
The mol ratio of porphyrin platinum and 9,10- diphenylanthrancenes is 1:2-1:10；
(3) oleic acid solutions in step (2) are taken in deionized water, microemulsion is formed by ultrasonic disperse；
(4) to addition 3- aminopropyl trimethoxysilanes or 3- aminopropyl triethoxysilanes in the microemulsion of step (3)；
(5) to tetraethyl orthosilicate is slowly added in the solution of step (4), the mixed solution of gained is slow at 45 DEG C -60 DEG C
Stirring 36h；The material of gained is washed with deionized water, and in 60 DEG C of vacuum drying, obtains green glow upper conversion function material
Material；
(6) the green glow upper conversion function material in step (5) is scattered in ethanol, adds a certain amount of 3- aminopropyls trimethoxy
Base silane or 3- aminopropyl triethoxysilanes, are stirred at room temperature 12h, using deionized water centrifugation, washing；
(7) material in step (6) is distributed to CdCl2In the aqueous solution, 4h is stirred at room temperature, using deionized water centrifugation, washing；
(8) material of gained in step (7) is distributed in thioacetyl amine aqueous solution, 24h is stirred at room temperature, using deionized water
Converting photocatalysis material on the CdS base green glows of gained is centrifuged, is washed, be finally vacuum dried 24h at 60 DEG C.
2. converting photocatalysis material on CdS bases green glow according to claim 1, it is characterised in that：In step (1), eight second
The concentration of base porphyrin platinum solution is 1mmol/L-10mmol/L；The concentration of 9,10- diphenylanthrancene solution is 1mmol/L-10mmol/
L。
3. converting photocatalysis material on CdS bases green glow according to claim 1, it is characterised in that：In step (2), oleic acid
Solution places 12h in 75 DEG C of baking oven makes tetrahydrofuran volatilize completely.
4. converting photocatalysis material on CdS bases green glow according to claim 1, it is characterised in that：In step (3), oleic acid
The volume ratio of solution and deionized water is 1:100-1:500.
5. converting photocatalysis material on CdS bases green glow according to claim 1, it is characterised in that：In step (4), 3- ammonia
Propyl trimethoxy silicane or 3- aminopropyl triethoxysilanes and the mass ratio of step (3) described deionized water are 1:500.
6. converting photocatalysis material on CdS bases green glow according to claim 1, it is characterised in that：In step (5), positive silicon
The mass ratio of sour tetra-ethyl ester and step (3) described deionized water is 1:30-1:100.
7. converting photocatalysis material on CdS bases green glow according to claim 1, it is characterised in that：In step (6), often
0.1mL-1mL 3- aminopropyl trimethoxysilanes or 3- aminopropyls three are added in 0.05g-0.2g green glow upper conversion function materials
Ethoxysilane.
8. converting photocatalysis material on CdS bases green glow according to claim 1, it is characterised in that：In step (7), CdCl2
The aqueous solution is 20mL, and concentration is 0.1M.
9. converting photocatalysis material on CdS bases green glow according to claim 1, it is characterised in that：It is thio in step (8)
Acetyl amine aqueous solution is 10mL-40mL, and concentration is 0.1M.
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| CN112316936A (en) * | 2020-11-23 | 2021-02-05 | 华中科技大学 | BiVO4Interface photocatalyst, preparation method and application thereof |
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