CN106238049A - A kind of Ag doping 3DOM CeO2zrO2the preparation of material - Google Patents
A kind of Ag doping 3DOM CeO2zrO2the preparation of material Download PDFInfo
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- CN106238049A CN106238049A CN201610695458.2A CN201610695458A CN106238049A CN 106238049 A CN106238049 A CN 106238049A CN 201610695458 A CN201610695458 A CN 201610695458A CN 106238049 A CN106238049 A CN 106238049A
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- 239000000463 material Substances 0.000 title description 7
- 238000002360 preparation method Methods 0.000 title description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 69
- 239000002131 composite material Substances 0.000 claims abstract description 33
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000011941 photocatalyst Substances 0.000 claims abstract description 21
- 230000006837 decompression Effects 0.000 claims abstract description 12
- 229910002492 Ce(NO3)3·6H2O Inorganic materials 0.000 claims abstract description 8
- 238000010189 synthetic method Methods 0.000 claims abstract 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims 1
- IQFVPQOLBLOTPF-HKXUKFGYSA-L congo red Chemical compound [Na+].[Na+].C1=CC=CC2=C(N)C(/N=N/C3=CC=C(C=C3)C3=CC=C(C=C3)/N=N/C3=C(C4=CC=CC=C4C(=C3)S([O-])(=O)=O)N)=CC(S([O-])(=O)=O)=C21 IQFVPQOLBLOTPF-HKXUKFGYSA-L 0.000 abstract description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 10
- 239000004793 Polystyrene Substances 0.000 abstract description 10
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 10
- 239000001257 hydrogen Substances 0.000 abstract description 10
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 8
- 238000007146 photocatalysis Methods 0.000 abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 7
- 238000006303 photolysis reaction Methods 0.000 abstract description 6
- 230000015843 photosynthesis, light reaction Effects 0.000 abstract description 6
- 238000012876 topography Methods 0.000 abstract description 5
- 238000001354 calcination Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000015556 catabolic process Effects 0.000 description 9
- 238000006731 degradation reaction Methods 0.000 description 9
- 239000013078 crystal Substances 0.000 description 7
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 239000000975 dye Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000003292 glue Substances 0.000 description 4
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 3
- 230000000593 degrading effect Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000000149 penetrating effect Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000004088 simulation Methods 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- 101710134784 Agnoprotein Proteins 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/66—Silver or gold
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses a kind of synthetic method of filling by reducing pressure and prepare Ag doping 3DOM CeO2‑ZrO2Composite photo-catalyst, belongs to chemical industry technical field.It is macropore template with polystyrene (PS) glueballs, and with EO20PO70O20(P123) it is mesoporous template, uses Zr (OC4H9)4、Ce(NO3)3·6H2O、AgNO3For raw material, after being filled by decompression, obtain 3DOM Ag/CeO through dry and calcining2‑ZrO2Composite photo-catalyst.Being determined its surface topography, microstructure, photocatalytic activity, properties of product improve a lot in terms of the photocatalysis of degraded Congo red and photolysis water hydrogen.
Description
Technical field
The present invention relates to Ag doping 3DOM CeO prepared by a kind of fill method that reduces pressure2-ZrO2Composite photo-catalyst, belongs to
Chemical industry technical field.
Background technology
Along with the consumption of the energy, the technology of decomposing water with solar energy hydrogen manufacturing is utilized to cause the extensive concern of people, and ring
One of border problem also factor becoming economic development.Novel photocatalysis technology causes various countries due to its feature such as environmentally friendly
The extensive concern of scientist.Photocatalysis technology mostly with semi-conducting material as photocatalyst, dirt of can degrading under the exciting of light
Dye thing.But, general photocatalyst exists shortcomings such as the utilization rate of sunlight are relatively low, exists so preparing high-efficiency photocatalysis material
Photolysis water hydrogen and degradation of contaminant aspect seem the most meaningful.
Summary of the invention
In order to solve the problems referred to above, it is an object of the invention to provide a kind of decompression completion method synthesis Ag doping 3DOM
CeO2-ZrO2Composite photo-catalyst, one is due to CeO2And ZrO2All there is suitable band gap locations, it is possible to utilize photolysis water
Produce hydrogen.Two, the specific surface area of material can be expanded by preparing three-dimensional ordered macroporous composite (3DOM), increase reaction
Avtive spot, meanwhile, the macroporous structure of the penetrating opening of 3DOM can reduce the resistance to mass tranfer of material, beneficially reactant molecule
Diffusion.Three, the photoresponse scope of catalysis can be made to widen to visible region by the doping of Ag, improve photocatalyst to the sun
The utilization rate of light, and the doping of Ag adds the flyway of composite light induced electron, the multipath of this light induced electron
Migrate the recombination rate inherently reducing photo-generate electron-hole pair, improve the light-catalyzed reaction efficiency of composite.With poly-
Styrene (PS) glueballs is macropore template, and with EO20PO70O20(P123) it is mesoporous template, uses Zr (OC4H9)4、Ce
(NO3)3·6H2O、AgNO3For raw material, after being filled by decompression, obtain 3DOM Ag/CeO through dry and calcining2-ZrO2Compound
Photocatalyst.
The technical solution adopted for the present invention to solve the technical problems is: decompression completion method synthesis Ag doping 3DOM CeO2-
ZrO2Composite photo-catalyst, weighs P123, and quality is 0.050 ± 0.005 g, isopropanol (IPA), and volume is 17 mL, PS, matter
Amount is 0.500 ± 0.010 g, Zr (OC4H9)4, volume is 1.5 mL, Ce (NO3)3·6H2O, quality is 0.167 ± 0.002 g,
AgNO3, quality is 0.023 ± 0.001 g.Ce(NO3)3·6H2O and AgNO3It is dissolved in 2 mL IPA standby.P123 is added
In IPA and stir to dripping Zr (OC after being completely dissolved4H9)4, it is subsequently added Ce (NO3)3With AgNO3Solution is to forming Ag/
CeO2-ZrO2Colloidal sol, is placed in Ag/CeO by PS template2-ZrO2In colloidal sol, carry out decompression after stirring a period of time and fill.By product
Putting in baking oven to being dried, set and dry temperature 60 ± 2 DEG C, dried obtained product is calcined 7 h at 600 DEG C, is obtained three
Dimension ordered big hole composite A g/CeO2-ZrO2(it is labeled as 3DOM Ag/CeO2-ZrO2)。
The invention has the beneficial effects as follows: use decompression completion method synthesis to have the 3DOM Ag/ of relatively high visible response
CeO2-ZrO2Composite photo-catalyst.Composite is by Emission in Cubic Ag, Emission in Cubic CeO2With Tetragonal ZrO2Composition, and the introducing of Ag
Improve the photocatalyst absorption in visible region.3DOM Ag/CeO2-ZrO2The three-dimensional ordered macroporous structure having makes material have
There is bigger specific surface area.Compared with P25, Congo red is had preferably under simulation daylight and visible ray by composite photo-catalyst
Light degradation effect.It addition, composite catalyst is at Na2S-Na2SO3For having higher product hydrogen effect under conditions of sacrifice agent, this is
Due to the introducing of Ag, expand the scope that composite is visible light-responded, add the flyway of light induced electron simultaneously, suppression
In composite, photo-generate electron-hole is to being combined, thus improves its photocatalytic activity.
Accompanying drawing explanation
The present invention will be further described with detailed description of the invention below in conjunction with the accompanying drawings.
Fig. 1 is PS glue crystal template surface topography map.
Fig. 2 is 3DOM Ag/CeO2-ZrO2Composite photo-catalyst surface topography map.
Fig. 3 is 3DOM Ag/CeO2-ZrO2The HR-TEM photo of composite photo-catalyst.
Fig. 4 is 3DOM Ag/CeO2-ZrO2The XRD figure of composite photo-catalyst.
Fig. 5 is 3DOM Ag/CeO2-ZrO2The N of composite photo-catalyst2Adsorption-desorption isothermal.
Fig. 6 is 3DOM Ag/CeO2-ZrO2The XPS figure of composite photo-catalyst.
Fig. 7 is direct light degradation, P25, CeO under ultraviolet light2、ZrO2、Ag/CeO2-ZrO2With 3DOM Ag/CeO2-ZrO2Urge
Change degraded Congo red kinetic results figure.
Fig. 8 is direct light degradation, P25, CeO under visible ray2、ZrO2、Ag/CeO2-ZrO2With 3DOM Ag/CeO2-ZrO2Urge
Change degraded Congo red reaction result figure.
Fig. 9 is direct light degradation, P25, CeO under simulation daylight2、ZrO2、Ag/CeO2-ZrO2With 3DOM Ag/CeO2-ZrO2
Catalytic degradation Congo red reaction result figure.
Figure 10 is P25, ZrO2、3DOM ZrO2、Ag/CeO2-ZrO2With 3DOM Ag/CeO2-ZrO2At Na2S-Na2SO3Molten
Photolysis water hydrogen result figure in liquid.
Detailed description of the invention
Decompression completion method synthesis Ag doping 3DOM CeO2-ZrO2Composite photo-catalyst, weighs and is purchased from close europeanized of Tianjin section
Ce (the NO of reagent company limited 99.0%3)3·6H2O, quality is Ce (NO3)3·6H2O, 0.167 ± 0.002 g, and it is purchased from sky
The AgNO of Jinshi City's recovery fine chemistry industry institute 99.8%3, quality be 0.023 ± 0.001 g be dissolved in be purchased from Tianjin recovery essence
In the IPA of the 99.7% of thin chemical institute, volume is that 2 mL are standby.To be purchased from Shanghai Sa En chemical technology company limited Mn ~
The P123 of 5800, quality is that 0.050 ± 0.005 g joins in the 15 mL IPA that volume is and stirring is dripped after being completely dissolved
Add the Zr (OC being purchased from Shanghai Mai Ruier chemical technology company limited 80.0%4H9)4, volume is 1.5 mL, is subsequently added Ce (NO3)3
With AgNO3Solution is to forming Ag/CeO2-ZrO2Colloidal sol, by PS template (use emulsifier-free emulsification method synthesis, and by from
The heart is dried acquisition PS glue crystal template), quality is that 0.500 ± 0.010 g is placed in Ag/CeO2-ZrO2In colloidal sol, stir a period of time
After carry out decompression fill.Being put into by product in baking oven to being dried, set and dry temperature 60 ± 2 DEG C, dried obtained product uses
The SX-2.5-12 type chamber type electric resistance furnace of Tianjin Stettlen Instrument Ltd. calcines 7 h at 600 DEG C, obtains three-dimensional order
Macropore composite A g/CeO2-ZrO2(it is labeled as 3DOM Ag/CeO2-ZrO2)。
The structure of 22 composite photo-catalysts and performance measurement:
One, surface topography and microstructure
3DOM Ag/CeO2-ZrO2Surface topography and the Micro-Structure Analysis result of sample are shown in Fig. 16.Can clearly be seen by Fig. 1
Observing, synthesized PS glue crystal template is neat and orderly in three dimensions, and size is homogeneous.Owing to being subject in self assembling process
To extruding, so PS glueballs presents hexagonal shape.The SEM result of Fig. 2 shows, sample is in arrangement in order, penetrating in opening
Macroporous structure, macropore is neat and orderly and be hexagonal shape, and owing to PS glue crystal template is face-centered cubic arrangement, so energy
Enough at each macropore, see three apertures.Fig. 3 is sample 3DOM Ag/CeO2-ZrO2HR-TEM photo, can from figure
To (111) crystal face of Emission in Cubic Ag, Emission in Cubic CeO2(111) crystal face and Tetragonal ZrO2(011) crystal face.Fig. 4 is prepared
The XRD figure of material, from the figure, it can be seen that composite 3DOM Ag/CeO2-ZrO2In there is Ag, CeO2And ZrO2Spy
Levy peak.Fig. 5 is the N of composite2Adsorption-desorption isothermal, as can clearly see from the figure, owing to having bigger ratio table
Area, the isothermal line of three-dimensional ordered macroporous composite significantly moves up.Can also prove from the XPS figure of Fig. 6,
3DOM Ag/CeO2-ZrO2There is two kinds of valence states and Ag presented in simple substance in middle Ce.
Two, photocatalysis performance measures
To synthesized 3DOM Ag/CeO2-ZrO2Photocatalytic activity carried out the degrading light of Congo red and photolysis water hydrogen urge
Change experiment.In order to evaluate the photocatalysis effect of synthesized composite, select commercially available P25, simple substance CeO2, simple substance ZrO2、Ag/
CeO2-ZrO2And 3DOM ZrO2Test as a comparison.
, different samples on the impact of ultraviolet degradation Congo red speed as shown in Figure 7.According to experimental data, according to formula- ln(C t /C 0 )=kt+bCalculate, wherein,C t Exist for dyestufftConcentration (the mg L in moment-1),C 0 It it is dyestuff initial concentration
(mg·L-1),kIt is speed constant (min-1),bFor intercept.As seen from Figure 7,-ln(C t /C 0 )With the response timetThe most linearly
Relation, pseudo-first order reaction kinetics is followed in the degraded of this explanation dyestuff Congo red.It is computed, direct light degradation, P25, CeO2、
ZrO2、Ag/CeO2-ZrO2With 3DOM Ag/CeO2-ZrO2The apparent reaction rate constant of ultraviolet light photocatalysis degradation Congo red
It is respectively 0.00053,0.00813,0.00652,0.00484,0.00902 and 0.01331 min-1.At visible ray and simulating sun
Congo red result of degrading under optical condition is shown in Fig. 8, Fig. 9,3DOM Ag/CeO2-ZrO2The degraded of Congo red is all presented by composite
Go out the highest photocatalytic activity, exceed well over commercially available P25.
2, photolysis water hydrogen P25, ZrO2、3DOM ZrO2、Ag/CeO2-ZrO2With 3DOM Ag/CeO2-ZrO2Different samples
At Na2S-Na2SO3In solution, hydrogen-producing speed result is as shown in Figure 10.Result shows, 3DOMAg/CeO2-ZrO2Composite has
Best hydrogen production potential.
Claims (2)
1. an Ag doping 3DOM CeO2-ZrO2The decompression fill method of composite photo-catalyst, weighs P123, and quality is 0.050
± 0.005 g, isopropanol (IPA), volume is 17 mL, PS, and quality is 0.500 ± 0.010 g, Zr (OC4H9)4, volume is 1.5
ML, Ce (NO3)3·6H2O, quality is 0.167 ± 0.002 g, AgNO3, quality is 0.023 ± 0.001 g.Ce(NO3)3·
6H2O and AgNO3It is dissolved in 2 mL IPA standby.P123 is joined in IPA and stir and drip Zr after being completely dissolved
(OC4H9)4, it is subsequently added Ce (NO3)3With AgNO3Solution is to forming Ag/CeO2-ZrO2Colloidal sol, is placed in Ag/CeO by PS template2-
ZrO2In colloidal sol, carry out decompression after stirring a period of time and fill.Product is put in baking oven to being dried, set dry temperature 60 ±
2 DEG C, dried obtained product calcines 7 h at 600 DEG C, obtains three-dimensional ordered macroporous composite A g/CeO2-ZrO2(mark
It is designated as 3DOM Ag/CeO2-ZrO2)。
3DOM Ag/CeO the most according to claim 12-ZrO2Synthetic method is filled in the decompression of composite photo-catalyst, and it is special
Levying and be: weigh P123, quality is 0.050 ± 0.005 g, IPA, and volume is 17 mL, PS, and quality is 0.500 ± 0.010 g, Zr
(OC4H9)4, volume is 1.5 mL, Ce (NO3)3·6H2O, quality is 0.167 ± 0.002 g, AgNO3, quality is 0.023 ±
0.001 g.The product prepared by decompression completion method is put in baking oven to being dried, and sets and dries temperature 60 ± 2 DEG C, after drying
Obtained product calcines 7 h at 600 DEG C, obtains three-dimensional ordered macroporous composite A g/CeO2-ZrO2。
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