CN104437573A - Preparation method of ZnFe2O4/ Ag3PO4 composite photocatalyst - Google Patents

Preparation method of ZnFe2O4/ Ag3PO4 composite photocatalyst Download PDF

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CN104437573A
CN104437573A CN201410628070.1A CN201410628070A CN104437573A CN 104437573 A CN104437573 A CN 104437573A CN 201410628070 A CN201410628070 A CN 201410628070A CN 104437573 A CN104437573 A CN 104437573A
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CN104437573B (en
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赫明
闫永胜
逯子扬
霍鹏伟
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Jiangsu University
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Abstract

The invention relates to a preparation method of a ZnFe2O4/ Ag3PO4 composite photocatalyst, belonging to the technical field of environmental material preparation. An ion exchange technique is adopted for the invention, and the preparation method comprises the steps of firstly, feeding FeCl3.6H2O solid and ZnCl2 solid into ethylene glycol, evenly stirring, then feeding sodium acetate (NaAC) and polyethylene glycol (PEG) into the mixture, continuously mixing, and carrying out a reaction to obtain ZnFe2O4 nanospheres; after that, feeding the ZnFe2O4 nanospheres into deionized water, rapidly stirring, dropwise adding a disodium hydrogen phosphate solution, carrying out a reaction, then dropwise adding a silver nitrate solution, stirring until reactants have a full reaction, washing the product, and then carrying out vacuum drying on the washed product to obtain the ZnFe2O4/Ag3PO4 composite photocatalyst. A composite visible light photocatalyst system is established; a heterogeneous structure system is established, so that the activity and the stability of silver phosphate can be improved; furthermore, the photocatalyst can be efficiently recovered by using the ZnFe2O4; the composite photocatalyst has a better degrading effect for the antibiotics in waste water.

Description

A kind of ZnFe 2o 4/ Ag 3pO 4the preparation method of composite photo-catalyst
Technical field
The present invention relates to a kind of ZnFe 2o 4/ Ag 3pO 4the preparation method of composite photo-catalyst, belongs to technical field of environmental material preparation.
Background technology
The developing rapidly of medical industry in recent years, bring leap to human civilization, meanwhile, the pollution of the waste water emitted in its production process to environment also increasingly sharpens, and brings serious threat to human health.Photocatalysis receives extensive concern and the research of large quantities of scholar as a kind of novel oxidized technology.Such as, and the traditional photochemical catalyst of major part can only absorb ultraviolet, titanium dioxide, but strontium titanates etc. and ultraviolet only accounts for 4% of whole solar energy, and visible ray is 43%.Therefore, development has the important subject that visible light-responded photochemical catalyst is current photocatalysis field efficiently.
Leaf golden flower seminar (Nature Materials, 2010,9559-564) research finds that silver orthophosphate is to there being good response as seen, and quantum yield up to 90%, and shows powerful oxidability under visible light illumination.Show that silver orthophosphate has a good application prospect in visible light catalytic field.But the electronics that silver orthophosphate produces in photocatalytic process is easily by the Ag of silver orthophosphate +be reduced into atom A g.Cause the composition of silver orthophosphate and destructurized affect its stablize.Silver orthophosphate dissociating in water environment makes its easy loss by dissolution in addition, and also result in a large amount of losses of catalyst, organic efficiency is poor.These unfavorable factors limit the large-scale practical application of silver orthophosphate.
Its stability is improved in order to suppress catalyst loss.Graphene and silver orthophosphate compound have been prepared visible light catalyst by Yang little Fei etc. (Chinese invention patent CN102631939A), Ma Peiyan etc. (Chinese invention patent cN102921438A), the existence of Graphene decreases the reunion of silver orthophosphate particle, improve the separative efficiency of photochemical catalyst carriers, therefore improve photocatalytic activity and the stability of composite photo-catalyst.Silver orthophosphate particle and polychlorostyrene second compound alkene particulate have after heat treatment been prepared silver orthophosphate/polyvinyl chloride-based conjugated polyene visible light catalyst by Luo Qingzhi etc. (Chinese invention patent CN 103623870 A).By its gained conjugated polyene have improve visible absorption, sensitization silver orthophosphate, improve light induced electron/hole separative efficiency and reduce silver orthophosphate effect such as dissolubility in water, this composite catalyst has excellent photocatalytic under visible light.But these class methods just improve the conduction of velocity of light induced electron by the compound of silver orthophosphate and conductive material, the photostability of silver orthophosphate is improved with this, simultaneously, because it conducts the limited in one's ability of light induced electron, nor effectively can reduce the dissolubility of silver orthophosphate in water environment, be difficult to the visible light catalysis activity of silver orthophosphate and stability are greatly improved.Still exist from the viewpoint of the recovery of catalyst and reclaim difficulty, halfway drawback.
Summary of the invention
The object of the invention is to overcome deficiency of the prior art, a kind of ZnFe is provided 2o 4/ Ag 3pO 4the preparation method of composite photo-catalyst, the present invention is preparation means with ion exchange technique, prepares ZnFe 2o 4/ Ag 3pO 4(zinc ferrite/silver orthophosphate) composite photo-catalyst.Its advantage is structure compounded visible light photocatalyst system; Improving activity and the stability of silver orthophosphate by building hetero-junctions system, utilizing ZnFe 2o 4the high efficiente callback of photochemical catalyst can be realized.
The technical solution used in the present invention is:
A kind of ZnFe 2o 4/ Ag 3pO 4the preparation method of composite photo-catalyst, carries out according to following step:
(1) FeCl is taken 36H 2o solid and ZnCl 2solid joins in ethylene glycol, adds NaAC and PEG again and continue to be stirred to evenly after stirring; ZnFe is obtained after mixed liquor being transferred to reaction kettle for reaction 2o 4nanosphere; Magnetic separation is separated, deionized water and ethanol washing, vacuum drying;
Wherein, FeCl is added described in 36H 2the amount of O solid is 0.135g ~ 1.08g, ZnCl 2solid is 0.034g ~ 0.272g, and ethylene glycol is 50mL; The NaAC added is 0.9g ~ 7.2g, and the PEG added is 0.25g ~ 2g; Reactor reaction condition transferred to by described mixed liquor is 180 DEG C ~ 200 DEG C reaction 8h ~ 12h; Described vacuum drying is dry at 50 DEG C.
(2) taking silver nitrate solid is dissolved in deionized water, is made into liquor argenti nitratis ophthalmicus; Separately take Na 2hPO 412H 2o solid is dissolved in deionized water, is made into disodium phosphate soln;
Wherein, the liquor argenti nitratis ophthalmicus concentration be made into described in is 0.05M ~ 0.3M; Disodium phosphate soln concentration is 0.05M ~ 0.3M.
(3) ZnFe of preparation in step (1) is taken 2o 4nanosphere joins in deionized water, ultrasonic disperse; Mechanical agitator rapid stirring also drips the disodium phosphate soln prepared in step (2) with dropping funel, continue reaction; Drip with dropping funel the liquor argenti nitratis ophthalmicus prepared in step (2) wherein again, dropwise rear continuation stirring and make it fully react, washed with deionized water and ethanol by product afterwards, vacuum drying obtains ZnFe 2o 4/ Ag 3pO 4composite photo-catalyst.
Wherein, the ZnFe taken described in 2o 4the ratio of nanosphere and deionized water is 0.0241g ~ 0.1928g:60mL, and described ultrasonic time is 60min;
Described dropping disodium phosphate soln is 1mL ~ 10mL, time for adding 0.5min ~ 30min, continues reflection 12h-36h;
Described dropping liquor argenti nitratis ophthalmicus 3mL ~ 30mL, time for adding is 1min ~ 50min, dropwises rear continuation and stirs 4h ~ 10h;
Described vacuum drying is dry at 50 DEG C.
Wherein, step (1) and the middle second alcohol and water of step (3) respectively wash three times.
Technological merit of the present invention:
Composite catalyst performance prepared in the present invention is better than general with the composite catalyst of four iron oxide prepared by magnetic material.With the magnetic semiconductor ZnFe of tool 2o 4by simple method and Ag 3pO 4prepare composite visible light catalyst, not only make catalyst with good magnetic, be beneficial to rapid recovery and the efficiency utilization of catalyst.And due to ZnFe 2o 4there is suitable level of energy, with Ag 3pO 4the generation of electro transfer and free radical can be promoted after compound, and then improve photocatalytic activity and increase Ag 3pO 4stability.
Accompanying drawing explanation
Fig. 1 is the SEM collection of illustrative plates of prepared sample, and wherein, a is ZnFe 2o 4sEM figure; B is Ag 3pO 4sEM figure; C is ZnFe 2o 4/ Ag 3pO 4sEM figure.
Fig. 2 is ZnFe 2o 4/ Ag 3pO 4eDS figure.
Fig. 3 is ZnFe 2o 4, Ag 3pO 4and ZnFe 2o 4/ Ag 3pO 4the XRD collection of illustrative plates of composite photo-catalyst.
Fig. 4 is ZnFe 2o 4, Ag 3pO 4and ZnFe 2o 4/ Ag 3pO 4the uv drs spectrogram of composite photo-catalyst.
Fig. 5 is the light degradation design sketch adding different catalysts degraded Danofloxacin mesylate waste water, is blank, ZnFe respectively 2o 4, Ag 3pO 4and ZnFe 2o 4/ Ag 3pO 4composite photo-catalyst.
Fig. 6 is for reclaiming degraded contrast experiment design sketch.
Fig. 7 is recovery five Ag 3pO 4and ZnFe 2o 4/ Ag 3pO 4the XRD contrast effect figure of composite photo-catalyst.
Detailed description of the invention
Below in conjunction with concrete embodiment, the present invention will be further described.
Photocatalytic activity evaluation: carry out in DW-01 type photochemical reaction instrument (purchased from Educational Instrument Factory of Yangzhou University), visible lamp irradiates, 100mL 20mg/L Danofloxacin mesylate simulated wastewater to be added in reactor and to measure its initial value, then photochemical catalyst is added, magnetic agitation is opened aerator and is passed into 10min sample analysis in interval in air During Illumination after secretly adsorbing 20min, get supernatant liquor at spectrophotometer λ after Magneto separate max=275nm place measures absorbance.
embodiment 1:
(1) FeCl is taken 36H 2o solid 0.54g and ZnCl 2solid 0.136g adds NaAC and 1g of 3.6g again PEG after joining and stirring in 50mL ethylene glycol continues to be stirred to evenly.Mixed liquor is transferred to 200 DEG C of reaction 10h in reactor and obtain ZnFe 2o 4nanosphere.Magnetic separation is separated, and deionized water and ethanol respectively wash three times, 50 DEG C of vacuum drying.
(2) take silver nitrate solid 8.493g to be dissolved in 250mL deionized water, be made into the liquor argenti nitratis ophthalmicus that concentration is 0.2M; Separately take Na 2hPO 412H 2o solid 17.907g(amount to sodium hydrogen phosphate 7.093g) be dissolved in 250mL deionized water, be made into the disodium phosphate soln that concentration is 0.2M.
(3) ZnFe of preparation in step (1) is taken 2o 4nanosphere 0.0482g joins in 60mL deionized water, ultrasonic 60min.Mechanical agitator rapid stirring also drips the disodium phosphate soln 3mL prepared in step (2), time for adding 2min with dropping funel, continue reaction 24h.The liquor argenti nitratis ophthalmicus 9mL prepared in step (2) is dripped wherein again with dropping funel.Time for adding is 20min.Dropwising rear continuation stirring 6h makes it fully react.Afterwards product is respectively washed three times with deionized water and ethanol, 50 DEG C of vacuum drying.
The SEM of obtained sample schemes as shown in Figure 1, as seen from the figure, and independent ZnFe 2o 4nanosphere surface is comparatively coarse and particle size is homogeneous, Ag 3pO 4for the structure of the multiaspect of rule and smooth surface.From ZnFe 2o 4/ Ag 3pO 4ag can be seen in the SEM figure of composite photo-catalyst 3pO 4and ZnFe 2o 4successfully be combined with each other, the element peak of two kinds of semiconductors can be found from the EDS collection of illustrative plates of Fig. 2, further illustrate compound success.
The XRD of obtained sample schemes as indicated at 3, as can be seen from the figure Ag 3pO 4and ZnFe 2o 4peak be the characteristic peak of typical two kinds of semiconductors.At ZnFe 2o 4/ Ag 3pO 4znFe can be seen in the XRD collection of illustrative plates of composite photo-catalyst simultaneously 2o 4and Ag 3pO 4characteristic peak.
Obtained ZnFe 2o 4, Ag 3pO 4and ZnFe 2o 4/ Ag 3pO 4composite photo-catalyst uv drs spectrogram as shown in Figure 4, as can be seen from the figure Ag 3pO 4have wider photo-absorption region, but absorption intensity is lower, and ZnFe 2o 4good absorption is had in whole interval.ZnFe 2o 4/ Ag 3pO 4composite photo-catalyst shows stronger absorption, and especially visible region performance is particularly outstanding, ZnFe just because of this 2o 4/ Ag 3pO 4composite photo-catalyst can be good at Danofloxacin mesylate of degrading under the irradiation of visible ray.
embodiment 2:
(1) FeCl is taken 36H 2o solid 0.135g and ZnCl 2solid 0.043g adds NaAC and 0.25g of 0.9g again PEG after joining and stirring in 50mL ethylene glycol continues to be stirred to evenly.Mixed liquor is transferred to 180 DEG C of reaction 8h in reactor and obtain ZnFe 2o 4nanosphere.Magnetic separation is separated, and deionized water and ethanol respectively wash three times, 50 DEG C of vacuum drying.
(2) take silver nitrate solid 2.123g to be dissolved in 250mL deionized water, be made into the liquor argenti nitratis ophthalmicus that concentration is 0.05M; Separately take Na 2hPO 412H 2o solid 4.476g(amount to sodium hydrogen phosphate 1.773g) be dissolved in 250mL deionized water, be made into the disodium phosphate soln that concentration is 0.05M.
(3) ZnFe of preparation in step (1) is taken 2o 4nanosphere 0.0241g joins in 60mL deionized water, ultrasonic 60min.Mechanical agitator rapid stirring also drips the disodium phosphate soln 1mL prepared in step (2), time for adding 0.5min with dropping funel, continue reaction 12h.The liquor argenti nitratis ophthalmicus 3mL prepared in step (2) is dripped wherein again with dropping funel.Time for adding is 1min.Dropwising rear continuation stirring 6h makes it fully react.Afterwards product is respectively washed three times with deionized water and ethanol, 50 DEG C of vacuum drying.
embodiment 3:
(1) FeCl is taken 36H 2o solid 1.08g and ZnCl 2solid 0.272g adds NaAC and 2g of 7.2g again PEG after joining and stirring in 50mL ethylene glycol continues to be stirred to evenly.Mixed liquor is transferred to 200 DEG C of reaction 12h in reactor and obtain ZnFe 2o 4nanosphere.Magnetic separation is separated, and deionized water and ethanol respectively wash three times, 50 DEG C of vacuum drying.
(2) take silver nitrate solid 12.74g to be dissolved in 250mL deionized water, be made into the liquor argenti nitratis ophthalmicus that concentration is 0.3M; Separately take Na 2hPO 412H 2o solid 26.11g(amount to sodium hydrogen phosphate 10.639g) be dissolved in 250mL deionized water, be made into the disodium phosphate soln that concentration is 0.3M.
(3) ZnFe of preparation in step (1) is taken 2o 4nanosphere 0.1928g joins in 60mL deionized water, ultrasonic 60min.Mechanical agitator rapid stirring also drips the disodium phosphate soln 10mL prepared in step (2), time for adding 30min with dropping funel, continue reaction 36h.The liquor argenti nitratis ophthalmicus 30mL prepared in step (2) is dripped wherein again with dropping funel.Time for adding is 50min.Dropwising rear continuation stirring 6h makes it fully react.Afterwards product is respectively washed three times with deionized water and ethanol, 50 DEG C of vacuum drying.
embodiment 4:
Taking photochemical catalyst obtained in 0.02g embodiment 1 joins in photocatalysis bottle, add 100mL 20mg/L Danofloxacin mesylate solution more wherein, lucifuge magnetic agitation 30min, after sampling, ventilation is turned on light and is carried out light degradation process, every 10min sampling once, continues 1h.Magneto separate goes out solution ultraviolet specrophotometer and surveys its absorbance, keeps above experimentation constant, and only changing catalyst is ZnFe 2o 4, Ag 3pO 4, ZnFe 2o 4/ Ag 3pO 4composite photo-catalyst and do not add catalyst and carry out light degradation process respectively.The catalytic action that different catalysts degrades for Danofloxacin mesylate is investigated with this, Fig. 5 is the light degradation design sketch adding different catalysts degraded Danofloxacin mesylate waste water, as can be seen from the figure Danofloxacin mesylate is more stable when not having catalyst illumination, obtained ZnFe 2o 4/ Ag 3pO 4composite photo-catalyst has best photocatalysis effect.
embodiment 5:
By Ag used in the light degradation in embodiment 4 3pO 4and ZnFe 2o 4/ Ag 3pO 4reclaim, after spending deionized water drying respectively, take the catalyst that 0.02g reclaims respectively to join in photocatalysis bottle and to add the Danofloxacin mesylate solution 100mL 20mg/L prepared, lucifuge magnetic agitation 30min, after sampling, ventilation is turned on light and is carried out light degradation process, every 10min sampling once, continues 1h.Magneto separate goes out solution ultraviolet specrophotometer and surveys its absorbance, the catalyst again reclaimed in above-mentioned experiment does second time recovery experiment, altogether carries out five times by that analogy, keeps other conditions constant, its result as shown in Figure 6, as can be seen from the figure prepared ZnFe 2o 4/ Ag 3pO 4composite photo-catalyst stability compares Ag 3pO 4good, reclaim all to show for five times and be better than Ag 3pO 4degrading activity.
embodiment 6:
By Ag used in the light degradation in embodiment 5 3pO 4and ZnFe 2o 4/ Ag 3pO 4reclaim, after deionized water washing drying, record its XRD and scheme as shown with 7, as can be seen from the figure Ag after five times are reclaimed degradation experiment 3pO 4part is decomposed and creates the characteristic peak of obvious Ag, and ZnFe 2o 4/ Ag 3pO 4only create a small amount of Ag and show ZnFe 2o 4and Ag 3pO 4compound improve the stability of catalyst.

Claims (10)

1. a ZnFe 2o 4/ Ag 3pO 4the preparation method of composite photo-catalyst, carries out according to following step:
(1) FeCl is taken 36H 2o solid and ZnCl 2solid joins in ethylene glycol, adds NaAC and PEG again and continue to be stirred to evenly after stirring; ZnFe is obtained after mixed liquor being transferred to reaction kettle for reaction 2o 4nanosphere; Magnetic separation is separated, deionized water and ethanol washing, vacuum drying;
(2) taking silver nitrate solid is dissolved in deionized water, is made into liquor argenti nitratis ophthalmicus; Separately take Na 2hPO 412H 2o solid is dissolved in deionized water, is made into disodium phosphate soln;
(3) ZnFe of preparation in step (1) is taken 2o 4nanosphere joins in deionized water, ultrasonic disperse; Mechanical agitator rapid stirring also drips the disodium phosphate soln prepared in step (2) with dropping funel, continue reaction; Drip with dropping funel the liquor argenti nitratis ophthalmicus prepared in step (2) wherein again, dropwise rear continuation stirring and make it fully react, washed with deionized water and ethanol by product afterwards, vacuum drying obtains ZnFe 2o 4/ Ag 3pO 4composite photo-catalyst.
2. a kind of ZnFe according to claim 1 2o 4/ Ag 3pO 4the preparation method of composite photo-catalyst, is characterized in that, step adds FeCl described in (1) 36H 2the amount of O solid is 0.135g ~ 1.08g, ZnCl 2solid is 0.034g ~ 0.272g, and ethylene glycol is 50mL; The NaAC added is 0.9g ~ 7.2g, and the PEG added is 0.25g ~ 2g.
3. a kind of ZnFe according to claim 1 2o 4/ Ag 3pO 4the preparation method of composite photo-catalyst, is characterized in that, reactor reaction condition transferred to by mixed liquor described in step (1) is 180 DEG C ~ 200 DEG C reaction 8h ~ 12h.
4. a kind of ZnFe according to claim 1 2o 4/ Ag 3pO 4the preparation method of composite photo-catalyst, is characterized in that, the liquor argenti nitratis ophthalmicus concentration be made into described in step (2) is 0.05M ~ 0.3M; Disodium phosphate soln concentration is 0.05M ~ 0.3M.
5. a kind of ZnFe according to claim 1 2o 4/ Ag 3pO 4the preparation method of composite photo-catalyst, is characterized in that, the ZnFe taken described in step (3) 2o 4the ratio of nanosphere and deionized water is 0.0241g ~ 0.1928g:60mL, and described ultrasonic time is 60min.
6. a kind of ZnFe according to claim 1 2o 4/ Ag 3pO 4the preparation method of composite photo-catalyst, is characterized in that, dripping disodium phosphate soln described in step (3) is 1mL ~ 10mL, time for adding 0.5min ~ 30min, continues reflection 12h-36h.
7. a kind of ZnFe according to claim 1 2o 4/ Ag 3pO 4the preparation method of composite photo-catalyst, is characterized in that, step drips liquor argenti nitratis ophthalmicus 3mL ~ 30mL described in (3), and time for adding is 1min ~ 50min, dropwises rear continuation and stirs 4h ~ 10h.
8. a kind of ZnFe according to claim 1 2o 4/ Ag 3pO 4the preparation method of composite photo-catalyst, is characterized in that, vacuum drying described in step (1) and step (3) is dry at 50 DEG C.
9. a kind of ZnFe according to claim 1 2o 4/ Ag 3pO 4the preparation method of composite photo-catalyst, is characterized in that, step (1) and the middle second alcohol and water of step (3) respectively wash three times.
10. an a kind of ZnFe according to claim 1 2o 4/ Ag 3pO 4the ZnFe of preparation method's gained of composite photo-catalyst 2o 4/ Ag 3pO 4composite photo-catalyst.
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CN110354887A (en) * 2019-08-05 2019-10-22 生态环境部华南环境科学研究所 A kind of catalyst capable of magnetic separating and its preparation method and application for photocatalytic degradation antibiotic
CN110354887B (en) * 2019-08-05 2022-06-21 生态环境部华南环境科学研究所 Magnetically separable catalyst for photocatalytic degradation of antibiotics and preparation method and application thereof
CN111167466A (en) * 2020-02-14 2020-05-19 辽宁大学 Z-type catalyst CdWO with dual-response activity4/ZnFe2O4And preparation method and application thereof
CN111167466B (en) * 2020-02-14 2021-10-22 辽宁大学 Z-type catalyst CdWO with dual-response activity4/ZnFe2O4And preparation method and application thereof
CN111659412A (en) * 2020-07-08 2020-09-15 中北大学 La0.7Sr0.3MnO3/α-Fe2O3Preparation and photocatalytic action thereof
CN111659412B (en) * 2020-07-08 2023-03-14 中北大学 Perovskite type composite oxide La 0.7 Sr 0.3 MnO 3 /α-Fe 2 O 3 Preparation method of (1)
CN111977696A (en) * 2020-08-13 2020-11-24 吉林化工学院 Preparation method and application of pomegranate-shaped magnetic visible light heterogeneous Fenton catalyst material
CN111977696B (en) * 2020-08-13 2022-06-07 吉林化工学院 Preparation method and application of pomegranate-shaped magnetic visible light heterogeneous Fenton catalyst material
CN112044456A (en) * 2020-09-16 2020-12-08 合肥学院 Ag3PO4/α-Fe2O3Preparation method and application of composite material

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