CN105195185B - A kind of efficiency light fenton catalyst Ag3PO4/ CuO and preparation method thereof - Google Patents
A kind of efficiency light fenton catalyst Ag3PO4/ CuO and preparation method thereof Download PDFInfo
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- CN105195185B CN105195185B CN201510599367.4A CN201510599367A CN105195185B CN 105195185 B CN105195185 B CN 105195185B CN 201510599367 A CN201510599367 A CN 201510599367A CN 105195185 B CN105195185 B CN 105195185B
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Abstract
The invention discloses a kind of efficiency light fenton catalyst Ag3PO4/ CuO and preparation method thereof.Ag3PO4/ CuO complex light fenton catalysts, it is characterised in that：It is by the Ag with polyhedral structure3PO4It is formed with the CuO nanometer spherical particles of its area load.Preparation method：(1) preparation of CuO：With Cu (Ac)2For presoma, hydro-thermal reaction prepares CuO in the presence of PVP additives；(2)Ag3PO4The preparation of/CuO：At room temperature, AgNO is added in CuO obtained by step (1)3Aqueous solution stirs, and is added dropwise later excessive by Na2HPO4And NaH2PO4The Na that the pH of composition is 73PO4Buffer solution is stirred to react, in Ag3PO4Upper in-situ preparation CuO obtains Ag3PO4/ CuO composite materials.The catalyst can improve the Fenton catalytic performance of pure CuO and solve single photochemical catalyst Ag3PO4Stability and cyclicity difference defect, for organic pollutant degradation have many advantages, such as catalytic performance height, stable structure, cyclicity height, degrade product it is pollution-free.It can be used for the fields such as organic pollution oxidative degradation, water decomposition hydrogen manufacturing.
Description
Technical field
The invention belongs to catalysis material technical field, more particularly to a kind of efficiency light fenton catalyst Ag3PO4/ CuO and
Preparation method.
Background technology
A series of crises of in the 21st century, facing mankind：Population expansion and resource consume excessively, air, water quality pollution,
A large amount of disappearances etc. of global warming caused by the discharge of toxic waste, greenhouse gases and biological species, global environment is
It is challenged greatly through being faced with ocean, fresh water, wetland, bio-diversity and the energy five.Sustainable development view disclose, population, resource with
Environment is closely related, and comprehensive utilization of resources connects each other with environmental protection, constitutes an organic whole.Environmental protection is that resource is opened
Important content in hair, economy development advancement.In order to realize that the sustainable development of economic society, control water quality work become environment
Protect an important component of work.How to be one using the organic matter in effective means degradation water is worth if inquiring into
Topic.
From 2010, leaf golden flower seminars found a kind of with quantum yield is high, visible light catalytic performance is good, without secondary dirt
The novel visible catalyst Ag of dye3PO4, research finds that this indirect semiconductor is significantly larger than the semiconductor that forefathers are reported and urges
Change performance, can be with quick and complete degradable organic pollutant, but it is partly dissolved in water, specific surface area is low, expensive, no
But illumination is unstable, and electron-hole is easily compound, greatly limits the photocatalysis performance of itself, then, researcher
Introduce new semiconductor by various methods around these problems, successfully synthesize various Ag3PO4Composite material, such as
Ag3PO4/AgI、Ag3PO4/Ag2S、Ag3PO4/In(OH)3、Ag3PO4/GO、Ag3PO4/g-C3N4、 Ag3PO4/MoS2、Ag3PO4/
WS2, etc., up to tens kinds, although this largely improves pure Ag3PO4Various weakness, but these thinkings are all
It is relatively simple, be difficult to expand.
From 1894, French scientist H.J.H.Fenton is found in acidic aqueous solution and H2O2Under conditions of coexisting,
Fe2+Can be the choosing of analysis-reduction organic matter and organic matter effectively by winestone acid oxidase, to invent Fenton reagent
The oxidation of selecting property provides a kind of new method, and Eisenhouser in 1964 uses Fenton reagent processing phenol and alkyl for the first time
Benzene waste water has started the precedent that Fenton reagent is applied in environmental contaminants processing.Nowadays, people constantly study Fenton examinations
Agent simultaneously opens up Fenton systems, such as FeOCl, CeO2、Fe3O4、Cu2(OH)PO4、CeO2/Fe3O4、CuO/Cu2O, it is efficiently and a large amount of
Degradation of organic substances looks for another way to solve problem of environmental pollution.Fenton reagent is organic for removing as a kind of strong oxidizer
Persistent organic pollutants in industrial wastewater have obvious advantage, are a kind of wastewater processing technologies having very much application potential.Tool
There is reaction to start fast, reaction condition is mild；Equipment is simple, less energy consumption, saves long journey expense；Fenton reagent oxidisability is strong, instead
Pollutant is thoroughly innoxious during answering, oxidant H2O2It voluntarily decomposes, leaves no residue after reaction, while being also good flocculation
Agent；Operational process is reliable and stable, easy to operate.
CuO is studied as a kind of semi-conducting material by scientific research person extensively, and the application reported by people includes gas
Body sensor, superconductor, photoswitch, li-ion electrode, Flied emission transmitter etc., but have very much foreground but by people always
What is ignored is that it is used for the efficient Fenton catalytic performance of degradable organic pollutant in environmental pollution, studies have shown that CuO has
Higher quasi- Fenton catalytic activity.
Invention content
The object of the present invention is to provide the preferable efficiency light fenton catalyst Ag of efficient and stability3PO4/ CuO and its preparation
Method.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
A kind of Ag is provided3PO4/ CuO complex light fenton catalysts, it is characterised in that：It is by with polyhedral structure
Ag3PO4It is formed with the CuO nanometer spherical particles of its area load.
By said program, the grain size of CuO nanometers of spherical particles is 20-30nm, Ag3PO4Grain size be 100-200nm.
By said program, CuO and Ag3PO4Molar ratio 1:1~3:1.
A kind of above-mentioned Ag is provided3PO4The preparation method of/CuO complex light fenton catalysts, it is characterised in that：Including walking as follows
Suddenly：
(1) preparation of CuO：With Cu (Ac)2For presoma, hydro-thermal reaction prepares CuO in the presence of PVP additives；
(2)Ag3PO4The preparation of/CuO：At room temperature, AgNO is added in CuO obtained by step (1)3Aqueous solution stirs, it
After be added dropwise it is excessive by Na2HPO4And NaH2PO4The buffer solution that the pH of composition is 7, is stirred to react, is given birth in situ on CuO
At Ag3PO4, obtain Ag3PO4/ CuO composite materials.
By said program, the hydrothermal temperature is 195-205 DEG C, the hydro-thermal reaction time 0.9-1.1h.
By said program, Cu (Ac) in the hydro-thermal reaction system2A concentration of 0.1mol/L.
By said program, every mM of Cu (Ac)2The content of used PVP is 0.0415-0.0443g.
By said program, by the washing of obtained product, drying to get CuO after the hydro-thermal reaction.
By said program, the reaction time in step (2) is 4-6h.
By said program, is washed after the completion of step (2) reaction, dries post-processing.
Beneficial effects of the present invention：
The catalyst can improve the Fenton catalytic performance of pure CuO and solve single photochemical catalyst Ag3PO4Stability
With the defect of cyclicity difference, there is the production that catalytic performance height, stable structure, cyclicity are high, degrade for organic pollutant degradation
The advantages that object is pollution-free.This novel quasi- Fenton/photochemical catalyst is in fields such as organic pollution oxidative degradation, water decomposition hydrogen manufacturing
There is potential application prospect.Catalyst preparation experiment condition is mild, simple and convenient, easily operated.
Description of the drawings
Fig. 1 is different proportion Ag3PO4The XRD diagram of/CuO catalyst, a, b, c are respectively the Ag of different proportion3PO4/ CuO,
Respectively 1:1、1:2、1:3；
Fig. 2 is pure CuO, different proportion CuO/Ag3PO4FESEM figure, a be pure CuO, b, c, d are that molar ratio is respectively
1:1、2:1、3:1 FESEM figures；
Fig. 3 is CuO, Ag3PO4、Ag3PO4The performance test figure of/CuO, a, b, c are respectively CuO, Ag3PO4、 Ag3PO4/CuO
Performance test figure, wherein H2O2Dosage be 200 μ L；
Fig. 4 is the best Ag of performance3PO4Different H are added in/CuO2O2Performance test figure；
Fig. 5 is the best Ag of performance3PO4The cyclical stability of the sample of/CuO is tested；
Specific implementation mode
Further detailed description is done to the present invention below in conjunction with drawings and examples
Embodiment 1
(1) preparation method (hydro-thermal method) of CuO fenton catalysts：0.1M、35mL Cu(Ac)2Solution as presoma, by
It is added dropwise to 150mg, 35mL PVP, 200 DEG C of hydro-thermal 1h will intend fenton catalyst after the washing of obtained product, drying to get CuO；
(2)Ag3PO4The preparation method (in-situ synthesized) of/CuO：At room temperature, CuO obtained by step (1) is taken
0.0167M, 50mL AgNO is added dropwise in 0.000835mol3After aqueous solution stirs 30min, 50mL Na are added dropwise2HPO4、
NaH2PO4Buffer solution (Na2HPO4And NaH2PO4Each 0.000835mol, pH=7) after stirring 5h, washing, dry, the production of gained
Object is CuO and Ag3PO4Molar ratio be 3:1 Ag3PO4/ CuO composite materials.
With reference to the above method, CuO and Ag is prepared3PO4Molar ratio be 2:1 and 1:1 Ag3PO4/ CuO composite materials.
The Microstructure characterization of catalyst：By the crystalline phase of X-ray powder diffraction (XRD) Experimental Characterization catalyst, pass through
FESEM characterizes the pattern of catalyst, including pure CuO, pure Ag3PO4And Ag3PO4/CuO.Quasi- Fenton/photocatalytic activity
Experiment：
(a) intend Fenton Catalysis experiments
In the experiment of each Fenton catalytic performance, the sample of 10mg is placed in the aqueous solution of 10ml rhodamine Bs (1 ×
10-5M), first magnetic agitation mixed solution 30min judges to reach when dyestuff by measuring the absorption value of dyestuff under dark condition
The H of 0.1ml is added after absorption-desorption balance2O2(wt 30%) is protected from light stirring, 5ml dyestuffs is taken out at regular intervals, after centrifugation
Take supernatant to measure its absorption value, when rhodamine B at 554nm without absorb when, illustrate that it is degraded completely.
(b) visible light catalytic is tested
In each photocatalysis experiment, the sample of 10mg is placed in (1 × 10 in the aqueous solution of 10ml rhodamine Bs-5M), first
The magnetic agitation mixed solution 30min under dark condition judges to reach absorption-solution when dyestuff by measuring the absorption value of dyestuff
Start illumination after inhaling balance.With in 300W xenon lamps (band optical filter filters off ultraviolet portion) During Illumination, take at regular intervals
Go out 5ml dyestuffs, supernatant taken to measure its absorption value after centrifugation, when rhodamine B at 554nm without absorb when, illustrate its quilt completely
Degradation.
(c) intend Fenton catalysis/visible light catalytic experiment
In quasi- Fenton catalysis/visible light catalytic experiment, the sample of 10mg is placed in the aqueous solution of 10ml rhodamine Bs
(1×10-5M), first the magnetic agitation mixed solution 30min under dark condition judges to work as dyestuff by measuring the absorption value of dyestuff
Reach the H that 0.1ml is added after absorption-desorption balances2O2(wt 30%) starts illumination afterwards.With 300W xenon lamps, (band optical filter filters off
Ultraviolet portion) in During Illumination, 5ml dyestuffs are taken out at regular intervals, takes supernatant to measure its absorption value after centrifugation, works as sieve
Red bright B, without absorption, illustrates that it is degraded completely at 554nm.
Quasi- Fenton Catalysis experiments (the CuO/200 μ L H of CuO2O2), it is seen that (vis/CuO) is tested in photocatalysis and quasi- Fenton is urged
Change/visible light catalytic (vis/CuO/200 μ L H2O2) experimental performance is shown in Fig. 3 a.
Ag3PO4Quasi- Fenton Catalysis experiments (Ag3PO4/200μLH2O2), it is seen that (vis/Ag is tested in photocatalysis3PO4) and it is quasi-
Fenton catalysis/visible light catalytic experimental performance (vis/Ag3PO4/200μL H2O2) see Fig. 3 b.
CuO and Ag3PO4Molar ratio be 1:1 Ag3PO4The quasi- Fenton Catalysis experiments (Dark/CuO/ of/CuO composite materials
Ag3PO4/H2O2), it is seen that (Vis/CuO/Ag is tested in photocatalysis3PO4) and quasi- Fenton catalysis/visible light catalytic (vis/CuO/
Ag3PO4/H2O2) experimental performance is shown in Fig. 3 c.In figure：Dark/CuO/Ag3PO4For blank control test.
Different proportion Ag3PO4The quasi- Fenton catalysis of/CuO/visible light catalytic experiment is shown in that Fig. 3 d, wherein AA1, AA2, AA3 divide
Ag is not indicated3PO4Molar ratio with CuO is 1:1,1:2 and 1:3 Ag3PO4The catalytic performance of/CuO composite materials.
Shown by comparison：The performance acted on by photocatalysis and Fenton catalyzing cooperation is more preferable, and Ag3PO4With mole of CuO
Than being 1:1 composite property is best.
(3) evaluation of catalytic performance
At room temperature, using RhB as substrate, the visible light with wavelength more than 420nm is irradiated, and evaluates same H2O2Addition
When, the activity of catalyst degradation RhB is as shown in Figure 4.The result shows that as composite A g3PO4The molar ratio of/CuO is 1:1, add
The H entered2O2Amount be 100 μ L when, the Ag of gained3PO4The catalytic activity of/CuO is higher than CuO and Ag under same case3PO4Urge
Change activity, it can be degradable by dyestuff in 20 minutes.
(4) evaluation of catalyst stability：
Take the CuO and Ag of optimum performance3PO4Molar ratio be 1:1 CuO/Ag3PO4Sample is catalyzed in primary light Fenton
After experiment, centrifuge washing takes out sample, continues to test after drying, be repeated 5 times, recycle successively.As a result see Fig. 5, Fig. 5 tables
It is bright：The CuO/Ag of the present invention3PO4Composite catalyst stability is excellent, is a kind of preferable light Fenton catalysis of efficient and stability
Agent.Compared to Ag3PO4For, pure Ag3PO4Although photocatalysis performance is higher, because its illumination is unstable, electron-hole recombinations are several
Rate is high, specific surface area is low, the problems such as being easily partly dissolved in water, all makes its stability not high, cycle performance is poor, can refer to document
Yu Hongjian,Yu Yong,Ma Peiyan et al.Space-confined growth Ag3PO4 nanoparticles
within WS2 sheets:Ag3PO4/WS2 composites as visible-light-driven
photocatalysts for decomposing dyes[J].J.Mater.Chem.A,2015。
Claims (8)
1. a kind of Ag3PO4/ CuO complex light fenton catalysts, it is characterised in that：It is by the Ag with polyhedral structure3PO4And its
The CuO nanometer spherical particles of area load form；CuO and Ag3PO4Molar ratio 1:1~ 3:1；Preparation method includes following step
Suddenly：
（1）The preparation of CuO：With Cu (Ac)2For presoma, hydro-thermal reaction prepares CuO in the presence of PVP additives；The water
Thermal response temperature is 195-205oC, the hydro-thermal reaction time 0.9-1.1h；Every mM of Cu (Ac)2The content of used PVP
For 0.0415-0.0443g；
（2）Ag3PO4The preparation of/CuO：At room temperature, in step（1）AgNO is added in gained CuO3Aqueous solution stir, later by
It is added dropwise to excessive by Na2HPO4And NaH2PO4The buffer solution that the pH of composition is 7, is stirred to react, the in-situ preparation on CuO
Ag3PO4, obtain Ag3PO4/ CuO composite materials.
2. Ag according to claim 13PO4/ CuO complex light fenton catalysts, it is characterised in that：CuO nanometers of pelletoids
The grain size of son is 20-30nm, Ag3PO4Grain size be 100-200nm.
3. Ag described in claim 13PO4The preparation method of/CuO complex light fenton catalysts, it is characterised in that：Including as follows
Step：
（1）The preparation of CuO：With Cu (Ac)2For presoma, hydro-thermal reaction prepares CuO in the presence of PVP additives；The water
Thermal response temperature is 195-205oC, the hydro-thermal reaction time 0.9-1.1h；Every mM of Cu (Ac)2The content of used PVP
For 0.0415-0.0443g；
（2）Ag3PO4The preparation of/CuO：At room temperature, in step（1）AgNO is added in gained CuO3Aqueous solution stir, later by
It is added dropwise to excessive by Na2HPO4And NaH2PO4The buffer solution that the pH of composition is 7, is stirred to react, the in-situ preparation on CuO
Ag3PO4, obtain Ag3PO4/ CuO composite materials.
4. preparation method according to claim 3, it is characterised in that：Cu (Ac) in the hydro-thermal reaction system2It is a concentration of
0.1mol/L。
5. preparation method according to claim 3, it is characterised in that：Wash obtained product after the hydro-thermal reaction,
Drying is to get CuO.
6. preparation method according to claim 3, it is characterised in that：Step（2）In reaction time be 4-6h.
7. preparation method according to claim 3, it is characterised in that：Step（2）After being washed, dried after the completion of reaction
Processing.
8. Ag described in claim 13PO4/ CuO complex light fenton catalyst light Fenton catalytic degradation organic pollutions are answered
With.
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| 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 |
| GB201713951D0 (en) * | 2017-08-31 | 2017-10-18 | Cambridge Entpr Ltd | A catalytic composite and a method of use thereof |
| CN110694655A (en) * | 2019-11-28 | 2020-01-17 | 长春工业大学 | Preparation method of silver sulfide/silver phosphate/graphene oxide composite photocatalyst |
| 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 |
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| CN101940937B (en) * | 2010-10-21 | 2012-04-25 | 武汉理工大学 | High-efficiency visible light catalyst silver phosphate and preparation method thereof |
| CN102125848B (en) * | 2011-01-18 | 2013-01-16 | 苏州科技学院 | Preparation of magnetic heterogeneous light Fenton catalyst and method for degrading organic pollutants |
| CN102513138B (en) * | 2011-11-11 | 2014-04-02 | 深圳职业技术学院 | Multi-phase light-assisted Fenton catalyst and preparation method thereof |
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