CN104759282A - Novel method for microwave-assisted preparation of zinc oxide/graphene/silver nano-composite photocatalyst - Google Patents
Novel method for microwave-assisted preparation of zinc oxide/graphene/silver nano-composite photocatalyst Download PDFInfo
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- CN104759282A CN104759282A CN201410719245.XA CN201410719245A CN104759282A CN 104759282 A CN104759282 A CN 104759282A CN 201410719245 A CN201410719245 A CN 201410719245A CN 104759282 A CN104759282 A CN 104759282A
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 48
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 35
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 20
- 239000004332 silver Substances 0.000 title claims abstract description 20
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 239000002114 nanocomposite Substances 0.000 title abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 230000005855 radiation Effects 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000002131 composite material Substances 0.000 claims description 16
- 239000002105 nanoparticle Substances 0.000 claims description 16
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 10
- BEAZKUGSCHFXIQ-UHFFFAOYSA-L zinc;diacetate;dihydrate Chemical compound O.O.[Zn+2].CC([O-])=O.CC([O-])=O BEAZKUGSCHFXIQ-UHFFFAOYSA-L 0.000 claims description 7
- 230000009467 reduction Effects 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000005516 engineering process Methods 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 238000007146 photocatalysis Methods 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000010842 industrial wastewater Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract 1
- 229960001296 zinc oxide Drugs 0.000 description 21
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 15
- 239000000047 product Substances 0.000 description 10
- 239000003054 catalyst Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 238000001237 Raman spectrum Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 3
- 229940012189 methyl orange Drugs 0.000 description 3
- 229910052984 zinc sulfide Inorganic materials 0.000 description 3
- 150000001721 carbon Chemical group 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
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Abstract
The invention discloses a novel method for microwave-assisted preparation of a zinc oxide/graphene/silver nano-composite photocatalyst. The method mainly comprises the following steps: 1) dissolving graphene oxide in water and carrying out ultrasonic peeling; and 2) uniformly mixing the prepared graphene oxide solution with each reaction component and placing the obtained mixture a microwave reaction instrument for microwave radiation so as to prepare the zinc oxide/graphene/silver nano-composite photocatalyst. The method provided by the invention has the advantages of simple preparation process, mild reaction conditions, full reaction of raw materials, low energy consumption and greatly shortened preparation time and improved preparation efficiency due to assist by microwaves; and the prepared zinc oxide/graphene/silver nano-composite photocatalyst has good photocatalytic performance and is expected to be applied to photocatalysis of industrial wastewater.
Description
Technical field
The invention belongs to field of new material preparation, be specially the new method that a kind of microwave radiation technology prepares zinc oxide/Graphene/silver nanoparticle composite photo-catalyst.
Background technology
Along with rapid industrial development, a large amount of industrial wastewater containing toxic organic pollutant flow in environment, brings serious harm to human health, and this impels people to strengthen exploitation sewage being contaminated to Treatment process.The outstanding advantages such as conductor photocatalysis degradable organic pollutant has low energy consumption, high efficiency, simple to operate, applicability is wide and contaminant degradation is thorough is a kind of green environmental protection technique having prospect.In numerous semiconductor light-catalyst, zinc oxide is because of safety non-toxic, and stability is high, photocatalysis performance good, and especially it is cheaply considered to one of photochemical catalyst of most application scenario and standby is popular.But serve as charge recombination center because zinc oxide exists exhibiting high surface defect, light induced electron and hole commute compound, cause its photocatalysis efficiency and service life reduction, limit its application.So the separative efficiency improving zinc-oxide nano photochemical catalyst electronics and hole becomes new study hotspot.Result of study in recent years shows, noble-metal-supported, ion doping, complex carbon material and other semi-conducting material all can suppress the compound of photo-generated carrier.
The carbon atom of Graphene is with sp
2hydridization links, form bi-dimensional cellular shape crystal structure, make it have great specific area, and show excellent electric conductivity, by itself and zinc-oxide nano photochemical catalyst compound, equally can not only play the effect of electron transmission passage with composite noble metal, and have good adsorption capacity to pollutant.Carrying out zinc oxide/Graphene/silver-colored tri compound can more effectively suppress light to become the quick compound of electron-hole pair, thus significantly improve photocatalysis efficiency and the recycling performance of zinc oxide, bibliographical information confirms this point [Dae-Hwang Y, Tran VC, Van HL, Nguyen TK, Eui JK, Seung HH, Sung HH.Photocatalytic Performance of a Ag/ZnO/CCG Multidimensional HeterostructurePrepared by a Solution-Based Method [J] .J.Phys.Chem.C, 2012, 116:7180-7184.S.Sarkar, D.Basak.One-step nano-engineering of dispersed Ag-ZnO nanoparticles ' hybrid in reduced grapheneoxide matrixand its superior photocatalytic property [J] .Cryst EngComm, 2013, 15:7606-7614].But preparation method's cost of material of zinc oxide/Graphene/silver nanoparticle composite photo-catalyst that document is reported is higher or friendly not, preparation process is loaded down with trivial details, and need high temperature or high pressure, especially reaction time is long, is unfavorable for popularization.Therefore, the preparation method developing simple, quick, eco-friendly zinc oxide/Graphene/silver nanoparticle composite photo-catalyst has important application value.
Summary of the invention
The object of the present invention is to provide that a kind of energy consumption is low, environmental friendliness, simple to operate, the preparation method of zinc oxide/Graphene/silver nanoparticle composite photo-catalyst that preparation efficiency is high.
Above-mentioned purpose of the present invention is achieved by following technical solution:
(1) be that Zinc diacetate dihydrate, citric acid and silver nitrate are dissolved in deionized water by 27:20:1:1600 ~ 1700 by the mass ratio of Zinc diacetate dihydrate, citric acid, silver nitrate, deionized water, obtain solution A;
(2) be that graphite oxide joins in deionized water by 1:600 ~ 720 by the mass ratio of graphite oxide and water, controlling ultrasonic power is 300W ~ 500W ultrasonic process 2h, obtains graphene oxide water solution B;
(3) being that solution A and solution B mix by 1:7.5 ~ 8 by the volume ratio of solution B and solution A, is that 1:1 drips 1molL wherein by the mass ratio of NaOH and Zinc diacetate dihydrate while stirring
-1sodium hydroxide solution, then be that 1:2 is added dropwise to absolute ethyl alcohol wherein by the volume ratio of absolute ethyl alcohol and sodium hydroxide solution, and continue under agitation to react 30min, obtain black suspension C;
(4) step (3) gained suspension C being placed in microwave reaction instrument, is 300W ~ 500W at ultrasonic power, and Microwave Power Density is 3kWm
-2~ 10kWm
-2condition under carry out the Microwave-assisted Reduction of 30min ~ 60min;
(5) by the centrifugation of step (4) gained reactant, and spend deionized water gained and precipitate three times, then the precipitation after washing is placed in 70 DEG C of dry 24h of baking oven, obtain zinc oxide/Graphene/silver nanoparticle composite photo-catalyst.
The present invention adopts Microwave-assisted Reduction to prepare zinc oxide/Graphene/silver nanoparticle composite photo-catalyst, there is the advantages such as mild condition, reaction rate is fast, output is large, overcome that current reported additive method preparation process is loaded down with trivial details, the reaction time is long, need the deficiency such as high temperature or high pressure, be applicable to a large amount of preparation.
Accompanying drawing explanation
Fig. 1 is the Raman spectrum of gained zinc oxide/Graphene/silver nanoparticle composite photo-catalyst and graphene oxide in embodiment 1.
Fig. 2 is the XRD diffracting spectrum of gained zinc oxide/Graphene/silver nanoparticle composite photo-catalyst in embodiment 1.
Fig. 3 is the SEM photo of gained zinc oxide/Graphene/silver nanoparticle composite photo-catalyst in embodiment 1.
Fig. 4 is the TEM photo of gained zinc oxide/Graphene/silver nanoparticle composite photo-catalyst in embodiment 1.
Fig. 5 be under UV-irradiation with gained zinc oxide/Graphene/silver in embodiment 1 for methyl orange degradation rate change curve in time during catalyst degradation methyl orange solution.
Detailed description of the invention
Embodiment 1:
(1) 0.8g Zinc diacetate dihydrate, 0.6g citric acid and 0.03g silver nitrate are dissolved in 50mL deionized water, obtain solution A;
(2) getting 0.15g graphite oxide joins in 100mL deionized water, and control ultrasonic power is 500W, and ultrasonic process 2h, obtains graphene oxide water solution B;
(3) 6.6mL solution B and 50mL solution A are mixed, dropwise adding 20mL concentration while stirring is wherein 1molL
-1sodium hydroxide solution, and then dropwise add 10mL absolute ethyl alcohol, and continue under agitation to react 30min, obtain black suspension C;
(4) step (3) gained suspension C is placed in microwave reaction instrument, control microwave power is 6.3kWm
-2, ultrasonic power is the Microwave-assisted Reduction that 500W carries out 30min;
(5) by the centrifugation of step (4) gained reactant, and spend deionized water gained and precipitate three times, then the precipitation after washing is placed in 70 DEG C of dry 24h of baking oven, obtain zinc oxide/Graphene/silver nanoparticle composite photo-catalyst.
Graphene oxide is shown in accompanying drawing 1 with the Raman spectrum preparing product.As can be seen from accompanying drawing 1, graphene oxide has two main Raman peaks: D peak and G peak, lay respectively at 1350cm
-1and 1594cm
-1.D peak is caused by the defect in graphite-structure, and G peak is owing to the SP of carbon atom
2key vibrations in the plane.Compared with graphene oxide, the D peak intensity preparing the Raman spectrum of product increases, and D/G (ID/IG) value becomes large, shows that graphene oxide is reduced in microwave reaction process.
Accompanying drawing 2 is shown in by the XRD collection of illustrative plates preparing product.The ZnO (100) marked in accompanying drawing 2, ZnO (002), ZnO (101), ZnO (102), ZnO (110), ZnO (103), ZnO (200), ZnO (112), ZnO (201) each crystal face, corresponding lattice paprmeter a=0.3249nm respectively, the corresponding Miller index of the hexagonal wurtzite structure ZnO of c=0.5206nm, its peak position peak standard diagram JCPDS (36-1451) that is strong and hexagonal wurtzite structure ZnO matches, and showing to prepare in product has hexagonal wurtzite structure ZnO.The Ag (111) marked in accompanying drawing 2, Ag (200), Ag (220) each crystal face, corresponding lattice paprmeter a=4.086 respectively, the Miller index of cube Ag of α=β=γ=90 °, its peak position peak is strong consistent with the standard spectrogram (JCPDS Card.No.04-0783) of cubic metal Ag, and showing to prepare in product has cubic structure Ag.In addition, there is not any impurity diffraction maximum.Relatively more sharp-pointed by the diffraction maximum in accompanying drawing 2, halfwidth is narrow can judge that prepared product has higher crystallinity.
Accompanying drawing 3 is shown in by the SEM photo preparing product different amplification.As can be seen from accompanying drawing 3a, preparing high content component ZnO in product is flower type structure, diameter about 1 μm.And Fig. 3 b shows flower pattern ZnO further by ZnO nano sheet forms, and there are many granules on surface, may be the Ag being attached to ZnO surface.
Accompanying drawing 4 is shown in by the TEM photo preparing product.In accompanying drawing 4, the material of sheet structure is ZnO, and the material of sheet layer film structure is Graphene, and the granule of high contrast is Ag.Visible Ag particle is attached to Graphene and ZnO surface.
Above-mentioned characterization result confirms that preparing product is zinc oxide/Graphene/argentum nano composite material.
With prepared zinc oxide/Graphene/argentum nano composite material for photochemical catalyst, 100W mercury lamp (luminous intensity is 63000lux) is light source, and Photocatalytic Degradation On Methyl Orange Solution, methyl orange degradation rate in time change curve is shown in accompanying drawing 5.From accompanying drawing 5, degraded 20min, the degradation rate of methyl orange reaches 92.7%.
Claims (2)
1. microwave radiation technology prepares a new method for zinc oxide/Graphene/silver nanoparticle composite photo-catalyst, it is characterized in that the concrete steps of the method are:
(1) be that Zinc diacetate dihydrate, citric acid and silver nitrate are dissolved in deionized water by 27:20:1:1600 ~ 1700 by the mass ratio of Zinc diacetate dihydrate, citric acid, silver nitrate, deionized water, obtain solution A;
(2) be that graphite oxide joins in deionized water by 1:600 ~ 720 by the mass ratio of graphite oxide and water, be ultrasonic process 2h under the condition of 300W ~ 500W at ultrasonic power, obtain solution B;
(3) being that solution A and solution B mix by 1:7.5 ~ 8 by the volume ratio of solution B and solution A, is that to drip concentration be wherein 1molL to 1:1 by the mass ratio of NaOH and Zinc diacetate dihydrate while stirring
-1sodium hydroxide solution, then be that 1:2 drips absolute ethyl alcohol wherein by the volume ratio of absolute ethyl alcohol and sodium hydroxide solution, and continue under agitation to react 30min, obtain black suspension C;
(4) step (3) gained suspension C is placed in microwave reaction instrument, carries out Microwave-assisted Reduction;
(5) by the centrifugation of step (4) gained reactant, and spend deionized water gained and precipitate three times, then the precipitation after washing is placed in 70 DEG C of dry 24h of baking oven, obtain zinc oxide/Graphene/silver nanoparticle composite photo-catalyst.
2. a kind of microwave radiation technology as claimed in claim 1 prepares the new method of zinc oxide/Graphene/silver nanoparticle composite photo-catalyst, it is characterized in that, when carrying out using Microwave-assisted Reduction in step (4), need control ultrasonic power is 300W ~ 500W, and Microwave Power Density is 3kWm
-2~ 10kWm
-2, radiated time is 30min ~ 60min.
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Cited By (6)
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| CN105498689A (en) * | 2015-12-09 | 2016-04-20 | 唐山冀东石墨烯科技发展有限公司 | Graphene loaded nano ZnO/Ag composite material and preparation method thereof |
| CN105561965A (en) * | 2015-12-31 | 2016-05-11 | 宿州学院 | Preparation method of flower shaped ZnO/graphene composite microsphere |
| CN105833853A (en) * | 2016-06-10 | 2016-08-10 | 苏州巨联环保科研有限公司 | Preparation method of calcium alginate fiber-based adsorbing material |
| CN106191985A (en) * | 2016-06-30 | 2016-12-07 | 武汉科技大学 | A kind of preparation method of stainless steel surfaces nanometic zinc oxide rod array |
| CN111205513A (en) * | 2020-03-16 | 2020-05-29 | 厦门捌斗新材料科技有限公司 | Graphene-based heat-conducting composite filler and preparation method and application thereof |
| CN115282960A (en) * | 2022-07-22 | 2022-11-04 | 皖西学院 | Method for synthesizing silver-doped nano ZnO with lasting high-efficiency photocatalytic performance by microwave method |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105498689A (en) * | 2015-12-09 | 2016-04-20 | 唐山冀东石墨烯科技发展有限公司 | Graphene loaded nano ZnO/Ag composite material and preparation method thereof |
| CN105498689B (en) * | 2015-12-09 | 2018-03-06 | 唐山冀东石墨烯科技发展有限公司 | Graphene-supported nano-ZnO/Ag composites and preparation method thereof |
| CN105561965A (en) * | 2015-12-31 | 2016-05-11 | 宿州学院 | Preparation method of flower shaped ZnO/graphene composite microsphere |
| CN105561965B (en) * | 2015-12-31 | 2018-04-03 | 宿州学院 | A kind of preparation method of flower-shaped ZnO/ graphenes complex microsphere |
| CN105833853A (en) * | 2016-06-10 | 2016-08-10 | 苏州巨联环保科研有限公司 | Preparation method of calcium alginate fiber-based adsorbing material |
| CN106191985A (en) * | 2016-06-30 | 2016-12-07 | 武汉科技大学 | A kind of preparation method of stainless steel surfaces nanometic zinc oxide rod array |
| CN106191985B (en) * | 2016-06-30 | 2019-03-19 | 武汉科技大学 | A kind of preparation method of stainless steel surface nanometic zinc oxide rod array |
| CN111205513A (en) * | 2020-03-16 | 2020-05-29 | 厦门捌斗新材料科技有限公司 | Graphene-based heat-conducting composite filler and preparation method and application thereof |
| CN111205513B (en) * | 2020-03-16 | 2021-08-31 | 厦门捌斗新材料科技有限公司 | Graphene-based heat-conducting composite filler and preparation method and application thereof |
| CN115282960A (en) * | 2022-07-22 | 2022-11-04 | 皖西学院 | Method for synthesizing silver-doped nano ZnO with lasting high-efficiency photocatalytic performance by microwave method |
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| CN104759282B (en) | 2017-10-20 |
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