CN104437573B - A kind of ZnFe2O4/Ag3PO4The preparation method of composite photo-catalyst - Google Patents
A kind of ZnFe2O4/Ag3PO4The preparation method of composite photo-catalyst Download PDFInfo
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Abstract
The present invention relates to a kind of ZnFe2O4/Ag3PO4The preparation method of composite photo-catalyst, belongs to technical field of environmental material preparation. The present invention adopts ion exchange technique, first by FeCl3?6H2O solid and ZnCl2Solid joins in ethylene glycol, is stirring evenly and then adding into NaAC and PEG and continues stirring, obtains ZnFe after reaction2O4Nanosphere; Then by this ZnFe2O4Nanosphere adds in deionized water, quick agitation and dropping disodium phosphate soln, drips silver nitrate solution after reaction again, and stirring makes it fully react, and product washing final vacuum dries to obtain ZnFe2O4/Ag3PO4Composite photo-catalyst; The present invention constructs a compounded visible light photocatalyst system; Improve activity and the stability of silver phosphate by building hetero-junctions system, and utilize ZnFe2O4The high efficiente callback of photocatalyst can be realized, and the antibiosis in waste water is have good degradation effect by this catalyst.
Description
Technical field
The present invention relates to a kind of ZnFe2O4/Ag3PO4The 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, brings leap to human civilization, and meanwhile, the pollution of environment is also increasingly sharpened by the waste water emitted in its production process, 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. And the traditional photocatalyst of major part can only absorb ultraviolet, for instance titanium dioxide, but strontium titanates etc. ultraviolet only accounts for the 4% of whole solar energy, and visible ray is 43%. Therefore, development has the important subject that visible light-responded photocatalyst is current photocatalysis field efficiently.
Leaf JINHUA seminar (NatureMaterials, 2010,9559-564) research finds that silver phosphate is to there being good response as seen, and quantum yield is up to 90%, and shows powerful oxidability under visible light illumination. Show that silver phosphate has a good application prospect in visible light catalytic field. But the electronics that silver phosphate produces in photocatalytic process is easily by the Ag of silver phosphate+It is reduced into atom A g. The composition causing silver phosphate affects it stably with destructurized. Additionally silver phosphate dissociating in water environment makes its easy loss by dissolution, also result in a large amount of losses of catalyst, and organic efficiency is poor. These unfavorable factors limit the large-scale practical application of silver phosphate.
In order to suppress catalyst loss to improve its stability. Graphene and silver phosphate compound are prepared for 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 phosphate particle, improve the separation efficiency of photocatalyst carriers, therefore improve photocatalytic activity and the stability of composite photo-catalyst.Silver phosphate granule and polychlorostyrene second compound alkene microgranule have after heat treatment been prepared silver phosphate/polyvinyl chloride-based conjugated polyene visible light catalyst by Luo Qingzhi etc. (Chinese invention patent CN103623870A). Being had by its gained conjugated polyene and improve visible absorption, sensitization silver phosphate, improve the separation efficiency in light induced electron/hole and reduce silver phosphate effect such as dissolubility in water, this composite catalyst has the photocatalytic of excellence under visible light. But this type of method improves the conduction velocity of light induced electron simply by the compound of silver phosphate and conductive material, the light stability of silver phosphate is improved with this, simultaneously, owing to it conducts the limited in one's ability of light induced electron, nor can effectively reduce silver phosphate dissolubility in water environment, it is difficult to make the visible light catalysis activity of silver phosphate and stability be greatly improved. Recovery difficulty, halfway drawback is still there is from the viewpoint of the recovery of catalyst.
Summary of the invention
It is an object of the invention to overcome deficiency of the prior art, it is provided that a kind of ZnFe2O4/Ag3PO4The preparation method of composite photo-catalyst, the present invention, with ion exchange technique for preparation means, prepares ZnFe2O4/Ag3PO4(zinc ferrite/silver phosphate) composite photo-catalyst. Have an advantage in that one compounded visible light photocatalyst system of structure; Improve activity and the stability of silver phosphate by building hetero-junctions system, utilize ZnFe2O4The high efficiente callback of photocatalyst can be realized.
The technical solution used in the present invention is:
A kind of ZnFe2O4/Ag3PO4The preparation method of composite photo-catalyst, carries out as steps described below:
(1) FeCl is weighed36H2O solid and ZnCl2Solid joins in ethylene glycol, adds NaAC and PEG and continue stirring to uniformly after stirring; ZnFe is obtained after mixed liquor is transferred to reaction kettle for reaction2O4Nanosphere; Magnetic separation separation, deionized water and washing with alcohol, vacuum drying;
Wherein, described addition FeCl36H2The amount of O solid is 0.135g ~ 1.08g, ZnCl2Solid is 0.034g ~ 0.272g, and ethylene glycol is 50mL; The NaAC added is 0.9g ~ 7.2g, and the PEG of addition 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) weigh silver nitrate solid and be dissolved in deionized water, be made into silver nitrate solution; Separately weigh Na2HPO4·12H2O solid is dissolved in deionized water, is made into disodium phosphate soln;
Wherein, the silver nitrate solution concentration being 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 weighed2O4Nanosphere joins in deionized water, ultrasonic disperse; Mechanical agitator quickly stirs and drips with Dropping funnel the disodium phosphate soln prepared in step (2), continues reaction; Dripping, with Dropping funnel, the silver nitrate solution prepared in step (2) wherein again, continue stirring and make it fully react after dropwising, afterwards by product with deionized water and washing with alcohol, vacuum drying obtains ZnFe2O4/Ag3PO4Composite photo-catalyst.
Wherein, the ZnFe weighed described in2O4The 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 reaction 12h-36h;
Described dropping silver nitrate solution 3mL ~ 30mL, time for adding is 1min ~ 50min, continues stirring 4h ~ 10h after dropwising;
Described vacuum drying is dry at 50 DEG C.
Wherein, in step (1) and step (3), second alcohol and water respectively washs three times.
The technological merit of the present invention:
Composite catalyst performance prepared in the present invention is better than general with four ferrum oxides for the composite catalyst prepared by magnetic material. To have magnetic quasiconductor ZnFe2O4By simple method and Ag3PO4Prepare composite visible light catalyst, not only make catalyst with good magnetic, be beneficial to reclaiming rapidly and efficiently utilizing of catalyst. And due to ZnFe2O4There is suitable level of energy, with Ag3PO4The generation of electron transfer and free radical can be promoted after compound, and then improve photocatalytic activity and increase Ag3PO4Stability.
Accompanying drawing explanation
Fig. 1 is the SEM collection of illustrative plates of prepared sample, and wherein, a is ZnFe2O4SEM figure; B is Ag3PO4SEM figure; C is ZnFe2O4/Ag3PO4SEM figure.
Fig. 2 is ZnFe2O4/Ag3PO4EDS figure.
Fig. 3 is ZnFe2O4、Ag3PO4And ZnFe2O4/Ag3PO4The XRD figure spectrum of composite photo-catalyst.
Fig. 4 is ZnFe2O4、Ag3PO4And ZnFe2O4/Ag3PO4The 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 respectively2O4、Ag3PO4And ZnFe2O4/Ag3PO4Composite photo-catalyst.
Fig. 6 is for reclaiming degraded contrast experiment's design sketch.
Fig. 7 is for reclaiming five Ag3PO4And ZnFe2O4/Ag3PO4The XRD contrast effect figure of composite photo-catalyst.
Detailed description of the invention
Below in conjunction with being embodied as example, 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, 100mL20mg/L Danofloxacin mesylate simulated wastewater is added in reactor and measures its initial value, it is subsequently adding photocatalyst, magnetic agitation is opened aerator after secretly adsorbing 20min and is passed into 10min sample analysis in interval in air During Illumination, takes the supernatant at spectrophotometer λ after Magneto separatemax=275nm place measures absorbance.
Embodiment 1:
(1) FeCl is weighed36H2O solid 0.54g and ZnCl2Solid 0.136g joins the PEG of NaAC and the 1g adding 3.6g after stirring in 50mL ethylene glycol and continues stirring to uniformly. Mixed liquor is transferred to 200 DEG C of reaction 10h in reactor and obtains ZnFe2O4Nanosphere. Magnetic separation separates, and deionized water and ethanol respectively wash three times, 50 DEG C of vacuum dryings.
(2) weigh silver nitrate solid 8.493g to be dissolved in 250mL deionized water, be made into the silver nitrate solution that concentration is 0.2M; Separately weigh Na2HPO4·12H2O solid 17.907g(amount to disodium hydrogen phosphate 7.093g) it is dissolved in 250mL deionized water, it is made into the disodium phosphate soln that concentration is 0.2M.
(3) ZnFe of preparation in step (1) is weighed2O4Nanosphere 0.0482g joins in 60mL deionized water, ultrasonic 60min. Mechanical agitator quickly stirs and drips with Dropping funnel the disodium phosphate soln 3mL prepared in step (2), time for adding 2min, continues reaction 24h. The silver nitrate solution 9mL prepared in step (2) is dripped wherein again with Dropping funnel. Time for adding is 20min. Continuing stirring 6h after dropwising makes it fully react. Afterwards product is respectively washed three times with deionized water and ethanol, 50 DEG C of vacuum dryings.
The SEM of the sample prepared schemes as it is shown in figure 1, as seen from the figure, independent ZnFe2O4Nanosphere surface is comparatively coarse and particle size is homogeneous, Ag3PO4Structure and smooth surface for regular multiaspect. From ZnFe2O4/Ag3PO4It can be seen that Ag in the SEM figure of composite photo-catalyst3PO4And ZnFe2O4Successfully it is combined with each other, the element peak of two kinds of quasiconductors can be found from the EDS collection of illustrative plates of Fig. 2, further illustrate compound success.
Prepare sample XRD figure as indicated at 3, as can be seen from the figure Ag3PO4And ZnFe2O4The characteristic peak that peak is typical two kinds of quasiconductors. At ZnFe2O4/Ag3PO4The XRD figure spectrum of composite photo-catalyst can simultaneously view ZnFe2O4And Ag3PO4Characteristic peak.
The ZnFe prepared2O4、Ag3PO4And ZnFe2O4/Ag3PO4Composite photo-catalyst uv drs spectrogram as shown in Figure 4, as can be seen from the figure Ag3PO4There is wider photo-absorption region, but absorption intensity is relatively low, and ZnFe2O4Good absorption is had in whole interval. ZnFe2O4/Ag3PO4Composite photo-catalyst shows stronger absorption, and especially visible region performance is especially prominent, ZnFe just because of this2O4/Ag3PO4Composite photo-catalyst can be good at degraded Danofloxacin mesylate under the irradiation of visible ray.
Embodiment 2:
(1) FeCl is weighed3·6H2O solid 0.135g and ZnCl2Solid 0.043g joins the PEG of NaAC and the 0.25g adding 0.9g after stirring in 50mL ethylene glycol and continues stirring to uniformly. Mixed liquor is transferred to 180 DEG C of reaction 8h in reactor and obtains ZnFe2O4Nanosphere. Magnetic separation separates, and deionized water and ethanol respectively wash three times, 50 DEG C of vacuum dryings.
(2) weigh silver nitrate solid 2.123g to be dissolved in 250mL deionized water, be made into the silver nitrate solution that concentration is 0.05M; Separately weigh Na2HPO4·12H2O solid 4.476g(amount to disodium hydrogen phosphate 1.773g) it is dissolved in 250mL deionized water, it is made into the disodium phosphate soln that concentration is 0.05M.
(3) ZnFe of preparation in step (1) is weighed2O4Nanosphere 0.0241g joins in 60mL deionized water, ultrasonic 60min. Mechanical agitator quickly stirs and drips with Dropping funnel the disodium phosphate soln 1mL prepared in step (2), time for adding 0.5min, continues reaction 12h. The silver nitrate solution 3mL prepared in step (2) is dripped wherein again with Dropping funnel. Time for adding is 1min. Continuing stirring 6h after dropwising makes it fully react. Afterwards product is respectively washed three times with deionized water and ethanol, 50 DEG C of vacuum dryings.
Embodiment 3:
(1) FeCl is weighed3·6H2O solid 1.08g and ZnCl2Solid 0.272g joins the PEG of NaAC and the 2g adding 7.2g after stirring in 50mL ethylene glycol and continues stirring to uniformly. Mixed liquor is transferred to 200 DEG C of reaction 12h in reactor and obtains ZnFe2O4Nanosphere. Magnetic separation separates, and deionized water and ethanol respectively wash three times, 50 DEG C of vacuum dryings.
(2) weigh silver nitrate solid 12.74g to be dissolved in 250mL deionized water, be made into the silver nitrate solution that concentration is 0.3M; Separately weigh Na2HPO4·12H2O solid 26.11g(amount to disodium hydrogen phosphate 10.639g) it is dissolved in 250mL deionized water, it is made into the disodium phosphate soln that concentration is 0.3M.
(3) ZnFe of preparation in step (1) is weighed2O4Nanosphere 0.1928g joins in 60mL deionized water, ultrasonic 60min. Mechanical agitator quickly stirs and drips with Dropping funnel the disodium phosphate soln 10mL prepared in step (2), time for adding 30min, continues reaction 36h. The silver nitrate solution 30mL prepared in step (2) is dripped wherein again with Dropping funnel. Time for adding is 50min. Continuing stirring 6h after dropwising makes it fully react. Afterwards product is respectively washed three times with deionized water and ethanol, 50 DEG C of vacuum dryings.
Embodiment 4:
Weigh the photocatalyst prepared in 0.02g embodiment 1 and join in photocatalysis bottle, being added thereto to 100mL20mg/L Danofloxacin mesylate solution, lucifuge magnetic agitation 30min again, after sampling, ventilation is turned on light and is carried out light degradation process, every 10min samples once, continues 1h.Magneto separate goes out solution ultraviolet spectrophotometer and surveys its absorbance, keeps with the above experimentation constant, and only changing catalyst is ZnFe2O4、Ag3PO4、ZnFe2O4/Ag3PO4Composite photo-catalyst and be added without catalyst and carry out light degradation process respectively. The catalytic action that different catalysts is degraded is investigated for Danofloxacin mesylate 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 ZnFe2O4/Ag3PO4Composite photo-catalyst has best photocatalysis effect.
Embodiment 5:
By Ag used in the light degradation in embodiment 43PO4And ZnFe2O4/Ag3PO4Reclaim, dried with deionized water wash respectively, weigh the 0.02g catalyst reclaimed respectively join in photocatalysis bottle and add the Danofloxacin mesylate solution 100mL20mg/L prepared, lucifuge magnetic agitation 30min, after sampling, ventilation is turned on light and is carried out light degradation process, every 10min samples once, continues 1h. Magneto separate goes out solution ultraviolet spectrophotometer and surveys its absorbance, again reclaim the catalyst in above-mentioned experiment and do second time recovery experiment, altogether carry out five times by that analogy, keep other conditions constant, its result as shown in Figure 6, as can be seen from the figure prepared ZnFe2O4/Ag3PO4Composite photo-catalyst stability compares Ag3PO4Good, reclaim all to show for five times and be better than Ag3PO4Degrading activity.
Embodiment 6:
By Ag used in the light degradation in embodiment 53PO4And ZnFe2O4/Ag3PO4Reclaiming, deionized water wash is dried, records its XRD figure as shown with 7, as can be seen from the figure Ag after five times are reclaimed degradation experiment3PO4Part is decomposed and creates the characteristic peak of obvious Ag, and ZnFe2O4/Ag3PO4Only create a small amount of Ag and show ZnFe2O4And Ag3PO4Compound improve the stability of catalyst.
Claims (9)
1. a ZnFe2O4/Ag3PO4The preparation method of composite photo-catalyst, carries out as steps described below:
(1) FeCl is weighed3·6H2O solid and ZnCl2Solid joins in ethylene glycol, adds NaAC and PEG and continue stirring to uniformly after stirring; ZnFe is obtained after mixed liquor is transferred to reaction kettle for reaction2O4Nanosphere; Magnetic separation separation, deionized water and washing with alcohol, vacuum drying;
(2) weigh silver nitrate solid and be dissolved in deionized water, be made into silver nitrate solution; Separately weigh Na2HPO4·12H2O solid is dissolved in deionized water, is made into disodium phosphate soln;
(3) ZnFe of preparation in step (1) is weighed2O4Nanosphere joins in deionized water, ultrasonic disperse; Mechanical agitator quickly stirs and drips with Dropping funnel the disodium phosphate soln prepared in step (2), continues reaction; Dripping, with Dropping funnel, the silver nitrate solution prepared in step (2) wherein again, continue stirring and make it fully react after dropwising, afterwards by product with deionized water and washing with alcohol, vacuum drying obtains ZnFe2O4/Ag3PO4Composite photo-catalyst;
Reactor reaction condition transferred to by mixed liquor described in step (1) is 180 DEG C ~ 200 DEG C reaction 8h ~ 12h.
2. a kind of ZnFe according to claim 12O4/Ag3PO4The preparation method of composite photo-catalyst, it is characterised in that add FeCl described in step (1)3·6H2The amount of O solid is 0.135g ~ 1.08g, ZnCl2Solid is 0.034g ~ 0.272g, and ethylene glycol is 50mL; The NaAC added is 0.9g ~ 7.2g, and the PEG of addition is 0.25g ~ 2g.
3. a kind of ZnFe according to claim 12O4/Ag3PO4The preparation method of composite photo-catalyst, it is characterised in that the silver nitrate solution concentration being made into described in step (2) is 0.05M ~ 0.3M;Disodium phosphate soln concentration is 0.05M ~ 0.3M.
4. a kind of ZnFe according to claim 12O4/Ag3PO4The preparation method of composite photo-catalyst, it is characterised in that the ZnFe weighed described in step (3)2O4The ratio of nanosphere and deionized water is 0.0241g ~ 0.1928g:60mL, and described ultrasonic time is 60min.
5. a kind of ZnFe according to claim 12O4/Ag3PO4The preparation method of composite photo-catalyst, it is characterised in that dripping disodium phosphate soln described in step (3) is 1mL ~ 10mL, time for adding 0.5min ~ 30min continues reaction 12h-36h.
6. a kind of ZnFe according to claim 12O4/Ag3PO4The preparation method of composite photo-catalyst, it is characterised in that dripping silver nitrate solution 3mL ~ 30mL described in step (3), time for adding is 1min ~ 50min, continues stirring 4h ~ 10h after dropwising.
7. a kind of ZnFe according to claim 12O4/Ag3PO4The preparation method of composite photo-catalyst, it is characterised in that step (1) and vacuum drying described in step (3) are dry at 50 DEG C.
8. a kind of ZnFe according to claim 12O4/Ag3PO4The preparation method of composite photo-catalyst, it is characterised in that step (1) and in step (3) second alcohol and water respectively wash three times.
9. an a kind of ZnFe according to claim 12O4/Ag3PO4The ZnFe of the preparation method gained of composite photo-catalyst2O4/Ag3PO4Composite photo-catalyst.
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