CN106964366A - A kind of CdS/ZnFe2O4Composite photo-catalyst and preparation method thereof - Google Patents
A kind of CdS/ZnFe2O4Composite photo-catalyst and preparation method thereof Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229910001308 Zinc ferrite Inorganic materials 0.000 claims abstract description 35
- 239000002131 composite material Substances 0.000 claims abstract description 20
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- 239000000975 dye Substances 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 18
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims description 11
- 229940043267 rhodamine b Drugs 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 7
- 239000002244 precipitate Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 230000033228 biological regulation Effects 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 7
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 3
- 238000005215 recombination Methods 0.000 abstract 1
- 230000006798 recombination Effects 0.000 abstract 1
- 239000010865 sewage Substances 0.000 abstract 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 12
- 238000001228 spectrum Methods 0.000 description 10
- 239000011259 mixed solution Substances 0.000 description 8
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 8
- 230000015556 catabolic process Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000003708 ampul Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- NNGHIEIYUJKFQS-UHFFFAOYSA-L hydroxy(oxo)iron;zinc Chemical compound [Zn].O[Fe]=O.O[Fe]=O NNGHIEIYUJKFQS-UHFFFAOYSA-L 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
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- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000008236 heating water Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000006552 photochemical reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
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- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
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- 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
- B01J27/043—Sulfides with iron group metals or platinum group metals
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- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C02F2101/00—Nature of the contaminant
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- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention discloses a kind of CdS/ZnFe2O4Composite photo-catalyst and preparation method thereof, CdS nano particles are prepared by hydro-thermal method, then deposit ZnFe on CdS surfaces by hydro-thermal method2O4Nano particle.Emission in Cubic CdS is prepared according to the present invention, and as carrier, loads ZnFe2O4Nano particle, adds the specific surface area of photochemical catalyst, reduces electron-hole recombination rate, improves CdS photocatalytic activity, the organic dyestuff in the sewage that can effectively degrade.
Description
Technical field
The invention belongs to inorganic functional material technical field, it is related to a kind of photochemical catalyst and preparation method, and in particular to one
Plant CdS/ZnFe2O4Composite photo-catalyst and preparation method thereof.
Background technology
Various semiconductor light-catalysts such as TiO of current people's exploitation2, tantalates, the greater band gap such as niobates, make
Photochemical catalyst could only be responded in ultraviolet light range, and in sunshine gross energy only have 5% wavelength be located at 400nm with
Under ultraviolet portion, it is clear that be not enough to realize effective utilization, while it is understood that solar energy mainly concentrates visible ray model
Enclose, general wavelength is 400-700nm, this portion of energy accounts for 43% of gross energy or so.Therefore to improve solar energy utilization ratio,
Final to realize photocatalysis technology commercial application, developing, there is visible light-responded and higher conversion efficiency photochemical catalyst gesture to exist
It must go.
CdS is a kind of typical II-VI race's semi-conducting material, belongs to direct band-gap semicondictor compound, CdS forbidden band is wide
Spend for 2.4eV, with good luminescent properties and light transfer characteristic, Light-Emitting Diode, photoelectric device, solar cell,
The fields such as photocatalysis, nonlinear optics have a wide range of applications.When using CdS separately as photochemical catalyst, there is photoetch
Phenomenon, reduces the utilization rate of photohole.Jiali Zhai,et al.,(ACS Appl.Mater.,Interfaces,
2011,3,2253-2258) preparation of CdS nano wires is reported, with good photocatalysis effect.
Spinelle ZnFe2O4It is a kind of semiconductor of n-type, is that a class has visible light-responded catalysis material, commonly uses hydro-thermal
The synthesis of cubic phase such as method, solid phase method, sonochemical method and chemical deposition ZnFe2O4.Its response wave length reaches 570-
640nm, ZnFe2O4Conduction band current potential be -1.58eV, with extremely strong reducing power, but its photo-generated carrier easily be combined, and
And the poor-performing of adsorption reaction thing, it is seen that photolytic activity cannot be utilized sufficiently.In order to efficiently separate its photo-generate electron-hole
It is right, the second phase semiconductor doping frequently as composite or deposit to improve the catalytic performance of material.
The content of the invention
It is an object of the invention to provide the CdS/ZnFe that a kind of technique is simple, photocatalysis efficiency is higher2O4Composite photocatalyst
Agent and preparation method thereof.
To achieve the above object, technical scheme is as follows：A kind of CdS/ZnFe2O4Composite photo-catalyst, wherein,
CdS/ZnFe2O4Middle CdS and ZnFe2O4Mol ratio be 1:1-3:1.
A kind of CdS/ZnFe2O4The preparation method of composite photo-catalyst, is comprised the following steps that：
By a certain amount of CdS ultrasonic disperses to Zn (NO3)2With Fe (NO3)3Mixed aqueous solution in, regulation pH value after carry out
Hydro-thermal reaction, obtained washing of precipitate is centrifuged and dried, CdS/ZnFe is obtained2O4Powder.
Preferably, CdS and ZnFe2O4Material amount ratio be 1:1-3:1.
Preferably, described pH value is adjusted to 12.5-13.5 using sodium hydroxide solution.
Preferably, hydrothermal temperature is 100 ± 10 DEG C, and the hydro-thermal time is 6 ± 0.5 hours.
The present invention also provides above-mentioned CdS/ZnFe2O4Application of the composite photo-catalyst in degradating organic dye.
Wherein, organic dyestuff is rhodamine B (RhB).
Compared with prior art, remarkable result of the invention is as follows：
(1)CdS/ZnFe2O4The energy gap of composite photo-catalyst between 1.96eV and 2.42eV, and with
ZnFe2O4The increase of content and increase, relative to energy gap for 2.42eV CdS for, band gap narrows, and having widened to respond
Visible-range；
(2) due to ZnFe2O4With CdS energy gap (ZnFe2O4Bandedge placement VB=0.38eV, CB=-1.58eV；
CdS bandedge placement is VB=1.76eV, CB=-0.66eV) more match, heterojunction structure can be formed, effectively suppresses electricity
Sub- hole it is compound, further increase the photocatalysis performance of semiconductor, being capable of effective degradable organic pollutant；
(3) raw material is simple and easy to get, and technique is simple, first prepares pure phase CdS, then by simple heating water bath, makes
ZnFe2O4Nanoparticle deposition is not required to by pre-treatment and post processing, technique is extremely simple, it is easy to operate, adjustable on CdS surfaces
Control property is strong.
(4) due to ZnFe2O4With superparamagnetism so that CdS/ZnFe2O4Can be by attraction, the powder being finished can
To carry out recycling using magnet.
Brief description of the drawings
Fig. 1 is CdS/ZnFe prepared by embodiment 1-42O4Composite photo-catalyst and comparative example CdS and ZnFe2O4XRD
Collection of illustrative plates.
Fig. 2 is CdS/ZnFe prepared by embodiment 32O4SEM (SEM) figure (a) of composite photo-catalyst and
Transmission electron microscope (TEM) figure (b).
Fig. 3 is CdS/ZnFe prepared by embodiment 1-42O4Composite photo-catalyst and comparative example CdS and ZnFe2O4Purple
Outside-visible diffusing reflection (DRS) spectrogram.
Fig. 4 is CdS/ZnFe prepared by embodiment 1-42O4The CdS and ZnFe of composite photo-catalyst, comparative example2O4It is right respectively
The degradation effect figure of organic dyestuff rhodamine B (RhB).
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples.
The CdS/ZnFe of the present invention2O4Composite photo-catalyst, its nominal component be CdS/ZFO-x, x represent CdS with
ZnFe2O4Mol ratio.
Embodiment 1
The CdS/ZnFe of the present embodiment2O4Composite photo-catalyst, wherein x=1:1, specific preparation process is as follows：
A) by 5mmol Cd (CH3COO)2, thiocarbamide is dissolved in 50mL ethylene glycol, is added 1g PVP-k30, is placed in magnetic force and stirs
Mix and stirred on device；Above-mentioned solution is stirred to being completely dissolved, mixed solution is transferred to autoclave, 180 DEG C of guarantors are heated to
Warm 4h；Natural cooling is taken out, by obtained solution centrifugal, washing, dries, obtains CdS；
B) by the Zn (NO of 1mmol CdS ultrasonic disperses to 50mL 1mmol3)2, 2mmol Fe (NO3)3Deionization it is water-soluble
In liquid, with NaOH deionized water solution (1mol L-1) pH is adjusted to 13, mixed solution is transferred to autoclave, heated
After being incubated 6 hours to 100 DEG C, room temperature is cooled to, obtained washing of precipitate is centrifuged and dried, CdS/ZFO-1 is obtained:1 powder.
Its XRD spectrum is as shown in figure 1, ZnFe can be seen in XRD spectrum2O4And CdS characteristic peak, its DRS spectrum such as Fig. 3
It is shown, it is seen that it absorbs limit at 620nm, can corresponding visible ray.
Embodiment 2
The CdS/ZnFe of the present embodiment2O4Composite photo-catalyst, wherein x=2:1, specific preparation process is as follows：
A) by 5mmol Cd (CH3COO)2, thiocarbamide is dissolved in 50mL ethylene glycol, is added 1g PVP-k30, is placed in magnetic force and stirs
Mix and stirred on device；Above-mentioned solution is stirred to being completely dissolved, mixed solution is transferred to autoclave, 180 DEG C of guarantors are heated to
Warm 4h；Natural cooling is taken out, by obtained solution centrifugal, washing, dries, obtains CdS；
B) by the Zn (NO of 1mmol CdS ultrasonic disperses to 50mL 0.5mmol3)2, 1mmol Fe (NO3)3Deionized water
In solution, with NaOH deionized water solution (1mol L-1) pH is adjusted to 13, mixed solution is transferred to autoclave, plus
After heat is incubated 6 hours to 100 DEG C, room temperature is cooled to, obtained washing of precipitate is centrifuged and dried, CdS/ZFO-2 is obtained:1 powder.
Its XRD spectrum is as shown in figure 1, ZnFe can be seen in XRD spectrum2O4And CdS characteristic peak, its SEM figures and TEM
Image is as shown in Fig. 2 can be concluded that CdS is nanometer chondritic, area load size is 5-10nm ZnFe2O4Nanoparticle
Son.Its DRS spectrum is as shown in Figure 3, it is seen that it absorbs limit at 610nm, can corresponding visible ray.
Embodiment 3
The CdS/ZnFe of the present embodiment2O4Composite photo-catalyst, wherein x=3:1, specific preparation process is as follows：
A) by 5mmol Cd (CH3COO)2, thiocarbamide is dissolved in 50mL ethylene glycol, is added 1g PVP-k30, is placed in magnetic force and stirs
Mix and stirred on device；Above-mentioned solution is stirred to being completely dissolved, mixed solution is transferred to autoclave, 180 DEG C of guarantors are heated to
Warm 4h；Natural cooling is taken out, by obtained solution centrifugal, washing, dries, obtains CdS；
B) by the Zn (NO of 1mmol CdS ultrasonic disperses to 50mL 0.33mmol3)2, 0.66mmol Fe (NO3)3Go from
In the sub- aqueous solution, with NaOH deionized water solution (1mol L-1) pH is adjusted to 13, mixed solution is transferred to reaction under high pressure
Kettle, be heated to 100 DEG C insulation 6 hours after, be cooled to room temperature, by obtained washing of precipitate centrifuge dry, obtain CdS/ZFO-3:1
Powder.
Its XRD spectrum is as shown in figure 1, ZnFe can be seen in XRD spectrum2O4And CdS characteristic peak, its DRS spectrum such as Fig. 3
It is shown, it is seen that it absorbs limit at 590nm, can corresponding visible ray.
Comparative example
The preparation of CdS nano particles
By 5mmol Cd (CH3COO)2, thiocarbamide is dissolved in 50mL ethylene glycol, is added 1g PVP-k30, is placed in magnetic agitation
Stirred on device；Above-mentioned solution is stirred to being completely dissolved, mixed solution is transferred to autoclave, 180 DEG C of insulations are heated to
4h；Natural cooling is taken out, by obtained solution centrifugal, washing, dries, obtains CdS.
ZnFe2O4Preparation
1mmol Zn (NO3)2, 2mmol Fe (NO3)3Deionized water solution in, with NaOH deionized water solution
(1mol L-1) pH is adjusted to 13, mixed solution is transferred to autoclave, be heated to 100 DEG C insulation 6 hours after, be cooled to
Room temperature, obtained washing of precipitate is centrifuged and dried, ZnFe is obtained2O4Nanometer powder.
Embodiment 5
CdS/ZnFe prepared by embodiment 1-32O4ZnFe in composite photo-catalyst and comparative example2O4With CdS difference
Degradation experiment is carried out to organic dyestuff rhodamine (RhB), comprised the following steps that：
(a) CdS/BiVO of 10mg embodiments 1-4 preparations is weighed respectively4(it is labeled as CdS/ZFO-X, wherein X=1:1,1:
2,1:3) and comparative example prepare CdS and ZnFe2O4；
(b) 10mL RhB solution is measured respectively in quartz ampoule (RhB concentration is 5mg/L), respectively by the upper of 10mg
State sample to add into quartz ampoule, quartz ampoule is transferred to the photochemical reaction instrument than the bright types of BL- V, and by suspension in dark
Middle stirring 60min ensures that pollutant adsorbs dissociation equilibrium with photochemical catalyst at room temperature.
(c) light source is opened, makes radiation of visible light suspension, every 30min, by sample take out it is a small amount of and with centrifuge from
The heart, rotating speed is 7000r/min, and the time is 1min, with the composite photo-catalyst nano particle in suspended liquid.Take what is centrifuged
Supernatant liquor, uses the UV-vis that solution after illumination degrading is obtained on Shimadzu UV-2450 ultraviolet-visible spectrophotometers
Spectrum.And according to the absorbance at characteristic absorption peak, obtain degradation curve.
Fig. 4 is embodiment 1-3 and pure CdS and ZnFe2O4To RhB degradation experiment figure, synthesize as we can see from the figure multiple
Compound CdS/ZnFe2O4Photocatalysis effect compared to pure CdS and ZnFe2O4Compare, have the raising of different levels, especially
It is CdS/ZFO-2 prepared by embodiment 2:1 degradation effect significantly, 92% or so is can reach during 120min to RhB degraded.With
ZnFe2O4The increase of content, CdS/ZnFe2O4The degradation efficiency of composite photo-catalyst, which shows, first increases the trend reduced afterwards,
This is probably because excess ZnFe2O4Reunion the reason for cause to decline the utilization rate of light.
Claims (8)
1. a kind of CdS/ZnFe2O4Composite photo-catalyst, it is characterised in that wherein, CdS/ZnFe2O4Middle CdS and ZnFe2O4Rub
You are than being 1:1-3:1.
2. photochemical catalyst as claimed in claim 1, it is characterised in that prepared by following steps：
By a certain amount of CdS ultrasonic disperses to Zn (NO3)2With Fe (NO3)3Mixed aqueous solution in, regulation pH value laggard water-filling heat
Reaction, obtained washing of precipitate is centrifuged and dried, CdS/ZnFe is obtained2O4Powder.
3. photochemical catalyst as claimed in claim 2, it is characterised in that CdS and ZnFe2O4Material amount ratio be 1:1-3:1.
4. photochemical catalyst as claimed in claim 2, it is characterised in that using sodium hydroxide solution adjust described pH value to
12.5-13.5。
5. photochemical catalyst as claimed in claim 2, it is characterised in that hydrothermal temperature is 100 ± 10 DEG C, the hydro-thermal time is 6 ±
0.5 hour.
6. the preparation method of the photochemical catalyst as described in claim 1-5 is any.
7. application of the photochemical catalyst as described in claim 1-5 is any in degradating organic dye.
8. application as claimed in claim 7, it is characterised in that organic dyestuff is rhodamine B.
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Cited By (5)
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| CN107684914A (en) * | 2017-08-14 | 2018-02-13 | 浙江工业大学 | A kind of magnetic Bi2MoO6/CuFe2O4Composite photocatalyst material and preparation method thereof |
| CN108043417A (en) * | 2018-01-06 | 2018-05-18 | 中南大学 | A kind of vanadic acid indium-zinc ferrite composite material and its preparation and the application in photocatalysis |
| CN109264787A (en) * | 2018-09-20 | 2019-01-25 | 济南大学 | A kind of ZnFe2O4The preparation method and products obtained therefrom of cube block structure |
| CN110560091A (en) * | 2019-09-27 | 2019-12-13 | 南京工业大学 | Preparation method of zinc ferrite-cadmium sulfide nanosphere composite visible-light-driven photocatalyst |
| CN110592596A (en) * | 2019-08-02 | 2019-12-20 | 西北师范大学 | Ternary semiconductor composite film and preparation method and application thereof |
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