CN105195185A - Efficient light fenton catalyst Ag3PO4/CuO and preparation method thereof - Google Patents
Efficient light fenton catalyst Ag3PO4/CuO and preparation method thereof Download PDFInfo
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- CN105195185A CN105195185A CN201510599367.4A CN201510599367A CN105195185A CN 105195185 A CN105195185 A CN 105195185A CN 201510599367 A CN201510599367 A CN 201510599367A CN 105195185 A CN105195185 A CN 105195185A
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Abstract
The invention discloses an efficient light fenton catalyst Ag3PO4/CuO and a preparation method thereof. The Ag3PO4/CuO compound light fenton catalyst is characterized by being prepared from Ag3PO4 with a polyhedron structure and CuO nano spherical particles loaded on the surface of Ag3PO4. The preparation method comprises the steps of CuO preparation, wherein Cu(Ac)2 is adopted as a precursor, and a hydrothermal reaction is carried out to prepare CuO under the existence of PVP additives; 2, Ag3PO4/CuO preparation, wherein an AgNO3 water solution is added to CuO obtained in the step 1 for stirring at room temperature, then excessive Na3PO4 buffer solutions prepared from Na2HPO4 and NaH2PO4 are added dropwise, reacting is carried out along with stirring, CuO is generated in situ on Ag3PO4, and an Ag3PO4/CuO composite is obtained. The catalyst can improve the fenton catalytic performance of pure CuO, the defect that a single light catalyst Ag3PO4 is poor in stability and circulation performance is overcome, and when the catalyst is used for organic pollutant degradation, the advantages of being high in catalytic performance, stable in structure, high in circulating performance, free of pollution of degradation products and the like are achieved. The efficient light fenton catalyst Ag3PO4/CuO can be used for the fields of organic pollutant oxidative degradation, water decomposition hydrogen manufacturing and the like.
Description
Technical field
The invention belongs to catalysis material technical field, particularly a kind of efficiency light fenton catalyst Ag
3pO
4/ CuO and preparation method thereof.
Background technology
Enter 21 century; the a series of crisis of facing mankind: population expansion and resource consume excessively; a large amount of disappearances etc. of the pollution of air, water quality, the discharge of toxic waste, global warming that greenhouse gases cause and living species, global environment has been faced with ocean, fresh water, wetland, bio-diversity and the energy five and has challenged greatly.Sustainable development view discloses, and population, resource and environment are closely related, and comprehensive utilization of resources and environmental protection connect each other, form an organic whole.Environmental protection is the important content in development of resources, economy development advancement.In order to realize the sustainable development of economic society, control the important component part that water quality work becomes environmental protection work.The organic matter in effective means degradation water how is adopted to be a topic being worth inquiring into.
From 2010, leaf golden flower seminar found a kind ofly have that quantum yield is high, visible light catalytic performance is good, the novel visible catalyst Ag of non-secondary pollution
3pO
4, research finds that this indirect semiconductor is far away higher than the semiconductor catalytic performance that forefathers report, can quick and complete degradable organic pollutant, but it is partly dissolved in water, specific area is low, expensive, not only illumination is unstable, and electron-hole very easily compound, greatly limit the photocatalysis performance of self, so, researchers are around these problems, by various method, introduce new semiconductor, successfully synthesize various Ag
3pO
4composite, as Ag
3pO
4/ AgI, Ag
3pO
4/ Ag
2s, Ag
3pO
4/ In (OH)
3, Ag
3pO
4/ GO, Ag
3pO
4/ g-C
3n
4, Ag
3pO
4/ MoS
2, Ag
3pO
4/ WS
2, etc., nearly tens kinds, although this improves pure Ag to a great extent
3pO
4various weakness, but these thinkings all more single, be difficult to expand.
From 1894, French scientist H.J.H.Fenton found in acidic aqueous solution and H
2o
2under the condition coexisted, Fe
2+effectively tartaric acid can be oxidized, thus invented Fenton reagent, for analysis-reduction organic matter and organic selective oxidation provide a kind of new method, within 1964, Eisenhouser uses Fenton reagent process phenol and alkylbenzene waste water first, has started the precedent that Fenton reagent is applied in environmental contaminants process.Nowadays, people constantly study Fenton reagent and open up Fenton system, as FeOCl, CeO
2, Fe
3o
4, Cu
2(OH) PO
4, CeO
2/ Fe
3o
4, CuO/Cu
2o, efficient and a large amount of degradation of organic substances, looks for another way for solving problem of environmental pollution.Fenton reagent has obvious advantage as a kind of strong oxidizer for the persistent organic pollutants removed in organic industrial sewage, is a kind of wastewater processing technology having very much application potential.Having reaction starts fast, and reaction condition is gentle; Equipment is simple, less energy consumption, saves long journey expense; Fenton reagent oxidisability is strong, and in course of reaction, pollutant is thoroughly innoxious, oxidant H
2o
2disintegrate after reaction, does not stay remnants, is also good flocculant simultaneously; Running is reliable and stable, easy and simple to handle.
CuO is extensively studied by scientific research person as a kind of semi-conducting material, comprised gas sensor, superconductor, photoswitch, li-ion electrode, Flied emission transmitter etc. by the application that people report, but what have very much prospect but to be ignored by people is its efficient Fenton catalytic performance for degradable organic pollutant in environmental pollution always, research shows, CuO has higher plan Fenton catalytic activity.
Summary of the invention
The object of this invention is to provide the efficient and good efficiency light fenton catalyst Ag of stability
3pO
4/ CuO and preparation method thereof.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A kind of Ag is provided
3pO
4/ CuO complex light fenton catalyst, is characterized in that: it is by the Ag with polyhedral structure
3pO
4form with the CuO nanometer spherical particle of its area load.
By such scheme, the particle diameter of CuO nanometer spherical particle is 20-30nm, Ag
3pO
4particle diameter be 100-200nm.
By such scheme, CuO and Ag
3pO
4mol ratio 1:1 ~ 3:1.
A kind of above-mentioned Ag is provided
3pO
4the preparation method of/CuO complex light fenton catalyst, is characterized in that: comprise the steps:
(1) preparation of CuO: with Cu (Ac)
2for presoma, under the existence of PVP additive, hydro-thermal reaction prepares CuO;
(2) Ag
3pO
4the preparation of/CuO: at room temperature, adds AgNO in step (1) gained CuO
3the aqueous solution stirs, and it is excessive in Na dropwise to add afterwards
2hPO
4and NaH
2pO
4the pH of composition is the cushioning liquid of 7, stirring reaction, in-situ preparation Ag on CuO
3pO
4, obtain Ag
3pO
4/ CuO composite.
By such scheme, described hydrothermal temperature is 195-205 DEG C, and the hydro-thermal reaction time is 0.9-1.1h.
By such scheme, Cu (Ac) in described hydro-thermal reaction system
2concentration be 0.1mol/L.
By such scheme, every mM of Cu (Ac)
2the content of the PVP used is 0.0415-0.0443g.
By such scheme, the product washing, dry will obtained after described hydro-thermal reaction, obtains CuO.
By such scheme, the reaction time in step (2) is 4-6h.
By such scheme, step (2) carries out after having reacted washing, dry post processing.
Beneficial effect of the present invention:
This catalyst can improve the Fenton catalytic performance of pure CuO, can solve again single photochemical catalyst Ag
3pO
4stability and the defect of cyclicity difference, for organic pollutant degradation, there is the advantages such as catalytic performance is high, Stability Analysis of Structures, cyclicity are high, the product of degraded is pollution-free.This novel plan Fenton/photochemical catalyst has potential application prospect in fields such as organic pollution oxidative degradation, water decomposition hydrogen manufacturing.Catalyst preparing experiment condition is gentle, simple and convenient, be easy to operation.
Accompanying drawing explanation
Fig. 1 is different proportion Ag
3pO
4the XRD figure of/CuO catalyst, a, b, c are respectively the Ag of different proportion
3pO
4/ CuO, is respectively 1:1,1:2,1:3;
Fig. 2 is pure CuO, different proportion CuO/Ag
3pO
4fESEM figure, the FESEM figure of a is pure CuO, b, c, d to be molar ratio be respectively 1:1,2:1,3:1;
Fig. 3 is CuO, Ag
3pO
4, Ag
3pO
4the performance test figure of/CuO, a, b, c are respectively CuO, Ag
3pO
4, Ag
3pO
4the performance test figure of/CuO, wherein H
2o
2consumption be 200 μ L;
Fig. 4 is the Ag of performance the best
3pO
4/ CuO adds different H
2o
2performance test figure;
Fig. 5 is the Ag of performance the best
3pO
4the cyclical stability experiment of the sample of/CuO;
Detailed description of the invention
Below in conjunction with drawings and Examples, further detailed description is done to the present invention
Embodiment 1
(1) preparation method's (hydro-thermal method) of CuO fenton catalyst: 0.1M, 35mLCu (Ac)
2solution, as presoma, dropwise adds 150mg, 35mLPVP, 200 DEG C of hydro-thermal 1h, by the product washing obtained, after drying, obtains CuO and intends fenton catalyst;
(2) Ag
3pO
4preparation method's (in-situ synthesized) of/CuO: at room temperature, gets step (1) gained CuO0.000835mol, dropwise adds 0.0167M, 50mLAgNO
3the aqueous solution dropwise adds 50mLNa after stirring 30min
2hPO4, NaH
2pO
4cushioning liquid (Na
2hPO
4and NaH
2pO
4each 0.000835mol, pH=7) stir 5h after, washing, dry, the product of gained is CuO and Ag
3pO
4mol ratio be the Ag of 3:1
3pO
4/ CuO composite.
With reference to said method, preparation CuO and Ag
3pO
4mol ratio be the Ag of 2:1 and 1:1
3pO
4/ CuO composite.
The Microstructure characterization of catalyst: by the crystalline phase of X-ray powder diffraction (XRD) Experimental Characterization catalyst, by FESEM, characterize the pattern of catalyst, comprises pure CuO, pure Ag
3pO
4and Ag
3pO
4/ CuO.Intend the experiment of Fenton/photocatalytic activity:
A () intends Fenton Catalysis experiments
In each Fenton catalytic performance test, all the sample of 10mg is placed in the aqueous solution (1 × 10 of 10ml rhodamine B
-5m), being first uniformly mixed solution 30min at dark condition lower magnetic force, by measuring the absorption value of dyestuff, judging the H adding 0.1ml after dyestuff reaches absorption-desorption balance
2o
2(wt30%) lucifuge stirs, and takes out 5ml dyestuff at set intervals, gets supernatant and measure its absorption value after centrifugal, when rhodamine B absorbs in 554nm place nothing, illustrates that it is degraded completely.
B () visible light catalytic is tested
In each photocatalysis test, the sample of 10mg is placed in the aqueous solution (1 × 10 of 10ml rhodamine B
-5m), being first uniformly mixed solution 30min at dark condition lower magnetic force, by measuring the absorption value of dyestuff, judging to start illumination after dyestuff reaches absorption-desorption balance.With in 300W xenon lamp (band optical filter elimination ultraviolet portion) During Illumination, take out 5ml dyestuff at set intervals, get supernatant after centrifugal and measure its absorption value, when rhodamine B absorbs in 554nm place nothing, illustrate that it is degraded completely.
C () intends Fenton catalysis/visible light catalytic experiment
In plan Fenton catalysis/visible light catalytic experiment, the sample of 10mg is placed in the aqueous solution (1 × 10 of 10ml rhodamine B
-5m), being first uniformly mixed solution 30min at dark condition lower magnetic force, by measuring the absorption value of dyestuff, judging the H adding 0.1ml after dyestuff reaches absorption-desorption balance
2o
2(wt30%) illumination is started after.With in 300W xenon lamp (band optical filter elimination ultraviolet portion) During Illumination, take out 5ml dyestuff at set intervals, get supernatant after centrifugal and measure its absorption value, when rhodamine B absorbs in 554nm place nothing, illustrate that it is degraded completely.
Plan Fenton Catalysis experiments (the CuO/200 μ LH of CuO
2o
2), visible light catalytic experiment (vis/CuO) and plan Fenton catalysis/visible light catalytic (vis/CuO/200 μ LH
2o
2) experimental performance is shown in Fig. 3 a.
Ag
3pO
4plan Fenton Catalysis experiments (Ag
3pO
4/ 200 μ LH
2o
2), visible light catalytic experiment (vis/Ag
3pO
4) and intend Fenton catalysis/visible light catalytic experimental performance (vis/Ag
3pO
4/ 200 μ LH
2o
2) see Fig. 3 b.
CuO and Ag
3pO
4mol ratio be the Ag of 1:1
3pO
4the plan Fenton Catalysis experiments (Dark/CuO/Ag of/CuO composite
3pO
4/ H
2o
2), visible light catalytic experiment (Vis/CuO/Ag
3pO
4) and intend Fenton catalysis/visible light catalytic (vis/CuO/Ag
3pO
4/ H
2o
2) experimental performance is shown in Fig. 3 c.In figure: Dark/CuO/Ag
3pO
4for blank test.
Different proportion Ag
3pO
4fig. 3 d is shown in the plan Fenton catalysis/visible light catalytic experiment of/CuO, and wherein AA1, AA2, AA3 represent Ag respectively
3pO
4be the Ag of 1:1,1:2 and 1:3 with the mol ratio of CuO
3pO
4the catalytic performance of/CuO composite.
Shown by contrast: better by the performance of photocatalysis and the effect of Fenton catalyzing cooperation, and Ag
3pO
4with composite property the best that the mol ratio of CuO is 1:1.
(3) evaluation of catalytic performance
At room temperature, take RhB as substrate, the visible ray being greater than 420nm with wavelength irradiates, and evaluates same H
2o
2during addition, the activity of catalyst degradation RhB as shown in Figure 4.Result shows, as composite A g
3pO
4the H that the mol ratio of/CuO is 1:1, add
2o
2amount when being 100 μ L, the Ag of gained
3pO
4the catalytic activity of/CuO is higher than CuO and Ag under same case
3pO
4catalytic activity, can be degradable by dyestuff in 20 minutes.
(4) evaluation of catalyst stability:
Get CuO and the Ag of optimum performance
3pO
4mol ratio be the CuO/Ag of 1:1
3pO
4sample, after once light Fenton Catalysis experiments terminates, centrifuge washing, takes out sample, continues test, repeat 5 times, circulate successively after oven dry.The results are shown in Figure 5, Fig. 5 to show: CuO/Ag of the present invention
3pO
4composite catalyst stability is excellent, is efficiently a kind of and the good light fenton catalyst of stability.Compare Ag
3pO
4, pure Ag
3pO
4although photocatalysis performance is higher, the problems such as because its illumination is unstable, electron-hole recombinations probability is high, specific area is low, be easily partly dissolved in water, all make its stability not high, cycle performance is poor, can bibliography YuHongjian, YuYong,
maPeiyanetal.Space-confinedgrowthAg
3pO
4nanoparticleswithinWS2sheets:Ag3PO4/WS2compositesasvisib le-light-drivenphotocatalystsfordecomposingdyes [J] .J.Mater.Chem.A, 2015.
Claims (10)
1. an Ag
3pO
4/ CuO complex light fenton catalyst, is characterized in that: it is by the Ag with polyhedral structure
3pO
4form with the CuO nanometer spherical particle of its area load.
2. Ag according to claim 1
3pO
4/ CuO complex light fenton catalyst, is characterized in that: the particle diameter of CuO nanometer spherical particle is 20-30nm, Ag
3pO
4particle diameter be 100-200nm.
3. Ag according to claim 1
3pO
4/ CuO complex light fenton catalyst, is characterized in that: CuO and Ag
3pO
4mol ratio 1:1 ~ 3:1.
4. Ag according to claim 1
3pO
4the preparation method of/CuO complex light fenton catalyst, is characterized in that: comprise the steps:
(1) preparation of CuO: with Cu (Ac)
2for presoma, under the existence of PVP additive, hydro-thermal reaction prepares CuO;
(2) Ag
3pO
4the preparation of/CuO: at room temperature, adds AgNO in step (1) gained CuO
3the aqueous solution stirs, and it is excessive in Na dropwise to add afterwards
2hPO
4and NaH
2pO
4the pH of composition is the Na of 7
3pO
4cushioning liquid, stirring reaction, in-situ preparation Ag on CuO
3pO
4, obtain Ag
3pO
4/ CuO composite.
5. preparation method according to claim 4, is characterized in that: described hydrothermal temperature is 195-205 DEG C, and the hydro-thermal reaction time is 0.9-1.1h.
6. preparation method according to claim 4, is characterized in that: Cu (Ac) in described hydro-thermal reaction system
2concentration be 0.1mol/L.
7. preparation method according to claim 4, is characterized in that: every mM of Cu (Ac)
2the content of the PVP used is 0.0415-0.0443g.
8. preparation method according to claim 4, is characterized in that: the product washing, dry will obtained after described hydro-thermal reaction, obtains CuO.
9. preparation method according to claim 4, is characterized in that: the reaction time in step (2) is 4-6h.
10. preparation method according to claim 4, is characterized in that: step (2) carries out after having reacted washing, dry post processing.
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CN106540721A (en) * | 2016-10-19 | 2017-03-29 | 常州大学 | A kind of preparation method of copper oxide compound phosphoric acid yttrium catalyst |
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CN106540721A (en) * | 2016-10-19 | 2017-03-29 | 常州大学 | A kind of preparation method of copper oxide compound phosphoric acid yttrium catalyst |
CN107029791A (en) * | 2017-04-25 | 2017-08-11 | 河南农业大学 | A kind of fenton catalyst and preparation method thereof, the application in lignocellulosic pretreatment |
CN107029791B (en) * | 2017-04-25 | 2019-04-30 | 河南农业大学 | A kind of fenton catalyst and preparation method thereof, the application in lignocellulosic pretreatment |
CN107233926A (en) * | 2017-07-17 | 2017-10-10 | 南京大学 | A kind of preparation method of carbon nanotube loaded heterogeneous Fenton System Catalyst |
CN107233926B (en) * | 2017-07-17 | 2019-11-22 | 南京大学 | A kind of preparation method of carbon nanotube loaded heterogeneous Fenton System Catalyst |
WO2019043404A1 (en) * | 2017-08-31 | 2019-03-07 | Cambridge Enterprise Limited | Method for selective oxidation with a catalytic composite |
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CN113318766A (en) * | 2021-06-07 | 2021-08-31 | 湖北工业大学 | Ag3PO4/g-C3N4Fenton-like catalytic material and preparation method and application thereof |
US20230226107A1 (en) * | 2022-01-19 | 2023-07-20 | Imam Abdulrahman Bin Faisal University | Method of preparing nanoparticles for cancer treatments |
US11980638B2 (en) * | 2022-01-19 | 2024-05-14 | Imam Abdulrahman Bin Faisal University | Method of preparing nanoparticles for cancer treatments |
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