CN107442114A - A kind of Pt loads 3DOMSn4+Adulterate TiO2The preparation of material - Google Patents
A kind of Pt loads 3DOMSn4+Adulterate TiO2The preparation of material Download PDFInfo
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- CN107442114A CN107442114A CN201710617876.4A CN201710617876A CN107442114A CN 107442114 A CN107442114 A CN 107442114A CN 201710617876 A CN201710617876 A CN 201710617876A CN 107442114 A CN107442114 A CN 107442114A
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- 239000000463 material Substances 0.000 title claims description 8
- 238000002360 preparation method Methods 0.000 title claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000002131 composite material Substances 0.000 claims abstract description 33
- 239000011941 photocatalyst Substances 0.000 claims abstract description 16
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000013078 crystal Substances 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000007540 photo-reduction reaction Methods 0.000 claims abstract description 12
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims abstract description 6
- 229910002621 H2PtCl6 Inorganic materials 0.000 claims abstract description 5
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims abstract description 5
- 238000005470 impregnation Methods 0.000 claims abstract description 4
- 238000010189 synthetic method Methods 0.000 claims abstract 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 53
- 229910008861 Sn—TiO2 Inorganic materials 0.000 claims description 45
- 229910021650 platinized titanium dioxide Inorganic materials 0.000 claims description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 229910052724 xenon Inorganic materials 0.000 claims description 4
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 230000001678 irradiating effect Effects 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical compound CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000008247 solid mixture Substances 0.000 claims description 2
- -1 volume is 0.1 mL Inorganic materials 0.000 claims description 2
- 150000001805 chlorine compounds Chemical class 0.000 claims 1
- 239000000084 colloidal system Substances 0.000 claims 1
- 239000000284 extract Substances 0.000 claims 1
- 229910052979 sodium sulfide Inorganic materials 0.000 claims 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 12
- 239000001257 hydrogen Substances 0.000 abstract description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 11
- 239000004793 Polystyrene Substances 0.000 abstract description 11
- 239000003292 glue Substances 0.000 abstract description 10
- FDZZZRQASAIRJF-UHFFFAOYSA-M malachite green Chemical compound [Cl-].C1=CC(N(C)C)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](C)C)C=C1 FDZZZRQASAIRJF-UHFFFAOYSA-M 0.000 abstract description 10
- 229940107698 malachite green Drugs 0.000 abstract description 10
- 238000006303 photolysis reaction Methods 0.000 abstract description 6
- 230000015843 photosynthesis, light reaction Effects 0.000 abstract description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 5
- 238000012876 topography Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 4
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 238000001354 calcination Methods 0.000 abstract description 2
- 230000000593 degrading effect Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 229920002223 polystyrene Polymers 0.000 description 9
- 230000015556 catabolic process Effects 0.000 description 8
- 238000006731 degradation reaction Methods 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- 239000000975 dye Substances 0.000 description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000004088 simulation Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- 230000000149 penetrating effect Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000003841 chloride salts Chemical class 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 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
- 239000000446 fuel Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052709 silver Inorganic materials 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
- B01J23/56—Platinum group metals
- B01J23/62—Platinum group metals with gallium, indium, thallium, germanium, tin or lead
- B01J23/622—Platinum group metals with gallium, indium, thallium, germanium, tin or lead with germanium, tin or lead
- B01J23/626—Platinum group metals with gallium, indium, thallium, germanium, tin or lead with germanium, tin or lead with tin
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
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- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/63—Pore volume
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- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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Abstract
Pt is prepared by photo-reduction synthetic method on the basis of glue crystal template the invention discloses one kind and loads 3DOM Sn4+Adulterate TiO2Composite photo-catalyst, belong to chemical industry technical field.Using polystyrene (PS) glueballs as macropore template, using C12H28O4Ti(TTIP)、SnCl4、H2PtCl6·6H2O is raw material, and after vacuum impregnation, three-dimensional ordered macroporous Sn is obtained by calcining4+Adulterate TiO2(it is labeled as 3DOM Sn TiO2)；Again after photo-reduction, 3DOM Pt/Sn TiO are obtained2.Its surface topography, microstructure, photocatalytic activity are determined, properties of product improve a lot in terms of the photocatalysis of degrading malachite green and photolysis water hydrogen.
Description
Technical field
The present invention relates to a kind of Pt load 3DOM Sn prepared on the basis of glue crystal template using photoreduction met hod4+Doping
TiO2Composite photo-catalyst, belong to chemical industry technical field.
Background technology
Global energy crisis and environmental problem are more and more prominent, because fossil fuel constantly consumption and non-renewable, hydrogen
As cleaning, can store and environmental protection fuel be considered as the most promising substitute of fossil fuel.Although have studied more than 40 years,
But TiO2For based photocatalyst because it possesses rich content, cost is low, and stability is high, it is non-toxic the features such as, be still now that light is urged
Change research main flow.However, due to higher electron-hole recombination rate so that its conversion efficiency to solar energy is low, in visible ray
The low rate and weak absorbing in region are widely applied it to suffer from limitation.Largely report prove, by with compared with
The metal nanoparticle (such as Ag, Au, Pt and Pd) of big work function is to TiO2Surface be modified turn into improve photogenerated charge current-carrying
The effective way of son separation.Adulterated simultaneously using other elements with TiO2Conduction band and valence band between form intermediate level, extensively
It is general to be used to reduce its band gap magnitude, therefore TiO2Absorption edge extend to visible region.
The content of the invention
In order to solve the above problems, it is an object of the invention to provide one kind to utilize photo-reduction on the basis of glue crystal template
Method prepares Pt load 3DOM Sn4+Adulterate TiO2Composite photo-catalyst, first, Sn4+The incorporation of ion makes TiO2Possess suitable mixed
Synthetic phase structure, what is formed mutually has the raising beneficial to its photocatalytic activity, while light decomposition water can be utilized to produce hydrogen.
Two, the specific surface area of material can be expanded by preparing three-dimensional ordered macroporous composite (3DOM), increase the active sites of reaction
Point；Meanwhile the macroporous structure of the penetrating openings of 3DOM can reduce the resistance to mass tranfer of material, be advantageous to the diffusion of reactant molecule.
Three, by Pt load the photoresponse scope of catalysis can be made to widen to visible region, improve profit of the photochemical catalyst to sunshine
Add the flyway of composite light induced electron with the load of rate, and Pt, the multipath migration of this light induced electron from
The recombination rate of photo-generate electron-hole pair is substantially reduced, improves the light-catalyzed reaction efficiency of composite.With polystyrene
(PS) glueballs is macropore template, using C12H28O4Ti(TTIP)、H2PtCl6·6H2O、SnCl4For raw material, pass through vacuum impregnation
Afterwards, 3DOM Sn are obtained by drying and calcination4+Adulterate TiO2Composite photo-catalyst；Pt is supported on by its table by photo-reduction again
On face, so as to obtain 3DOM Pt/Sn-TiO2。
The technical solution adopted for the present invention to solve the technical problems is：Photoreduction met hod is utilized on the basis of glue crystal template
Synthesize Pt load 3DOM Sn4+Adulterate TiO2Composite photo-catalyst, PS glueballs being weighed, quality is 2.000 ± 0.010 g,
C12H28O4Ti (TTIP), volume are 1.0 mL, anhydrous SnCl4, volume is 0.1 mL, H2PtCl6·6H2O, volume are 0.3 mL.
Take 2.000 ± 0.010 g PS glueballs to be impregnated with methanol, filtered after stirring 30 min, treat its natural drying.2 mL TTIP are taken again
It is put into 0.1 mL anhydrous stannic chlorides in beaker, the PS balls handled well is slowly added to after well mixed, then stir 1 h；It is complete
It is placed in vacuum drying chamber and vacuumizes after.Finally the solid mixture for completing vacuum is put into Muffle furnace, forged at 600 DEG C
Burn 8 h and obtain the prepared three-dimensional ordered macroporous Sn of sample4+Adulterate TiO2(it is labeled as 3DOM Sn-TiO2)。
Take 0. 3000 ± 0.0010 g 3DOM Sn-TiO2In deionized water, 10 min of ultrasound, light is placed on also
In former reactor, 3.000 ± 0.010 g vulcanized sodium (as sacrifice agent), 0.3 mL platinum acid chloride solution are separately added into.Mixing
After irradiating 1 h using 300 W xenon lamps under vacuum conditions after uniformly, washed 3-4 times with deionized water and ethanol respectively, vacuum is done
Dry 10 h obtains composite 3DOM Pt/Sn-TiO2。
The beneficial effects of the invention are as follows：Using photoreduction met hod synthesis there is high light catalysis to live on the basis of glue crystal template
The 3DOM Pt/Sn-TiO of property2Composite photo-catalyst.Composite is by metal simple-substance Pt, Anatase TiO2And Rutile Type
TiO2Composition, and Pt introducing improves absorption of the photochemical catalyst in visible region.3DOM Pt/Sn-TiO2The three-dimensional having has
Sequence macroporous structure makes material have larger specific surface area.Compared with P25, composite photo-catalyst is under simulation daylight and visible ray
There is preferable light degradation effect to malachite green.In addition, composite catalyst has higher production in alcohol-water mixed solution
Hydrogen effect, this is due to Pt introducing, adds the flyway of light induced electron, it is suppressed that light induced electron-sky in composite
Cave pair it is compound；Trap is captured at the same time as electronics, new avtive spot is provided for light-catalyzed reaction；Urged so as to improve its light
Change activity.
Brief description of the drawings
The present invention will be further described with reference to the accompanying drawings and detailed description.
Fig. 1 is PS glue crystal template surface topography maps.
Fig. 2 is 3DOM Pt/Sn-TiO2Composite photo-catalyst surface topography map.
Fig. 3 is 3DOM Pt/Sn-TiO2The HR-TEM photos of composite photo-catalyst.
Fig. 4 is TiO2、3DOM Sn-TiO2、Pt/Sn-TiO2With 3DOM Pt/Sn-TiO2The XRD of composite photo-catalyst.
Fig. 5 (a) is Pt/Sn-TiO2The N of composite photo-catalyst2Absorption-desorption isotherm.
Fig. 5 (b) is 3DOM Pt/Sn-TiO2The N of composite photo-catalyst2Absorption-desorption isotherm.
Fig. 6 is TiO2、Sn-TiO2、3DOM Sn-TiO2、Pt/Sn-TiO2With 3DOM Pt/Sn-TiO2The UV- of photochemical catalyst
Vis schemes.
Fig. 7 is direct light degradation, P25, Sn-TiO under ultraviolet light2、3DOM Sn-TiO2、Pt/Sn-TiO2With 3DOM Pt/
Sn-TiO2Catalytic degradation malachite green kinetic results figure.
Fig. 8 is direct light degradation, P25, Sn-TiO under visible ray2、3DOM Sn-TiO2、Pt/Sn-TiO2With 3DOM Pt/
Sn-TiO2Catalytic degradation malachite green reaction result figure.
Fig. 9 is direct light degradation, P25, Sn-TiO under simulation daylight2、3DOM Sn-TiO2、Pt/Sn-TiO2And 3DOM
Pt/Sn-TiO2Catalytic degradation malachite green reaction result figure.
Figure 10 (a) is 3DOM Pt/Sn-TiO2The photolysis water hydrogen result figure in ethanol-water solution.
Figure 10 (b) is P25 and 3DOM Pt/Sn-TiO2The photolysis water hydrogen comparative result figure in ethanol-water solution.
Embodiment
Photoreduction met hod synthesis Pt load 3DOM Sn are utilized on the basis of glue crystal template4+Adulterate TiO2Composite photo-catalyst
(3DOM Pt/Sn-TiO2), pipette the C for being purchased from Shanghai Mai Ruier chemical technologies Co., Ltd 99.0%12H28O4Ti (TTIP), body
Product is 1.0 mL;With the anhydrous stannic chloride (SnCl for being purchased from Tianjin recovery fine chemistry industry research institute 99.0%4), volume 0.1
ML mixing for standby use.PS templates (are synthesized using the emulsification method of emulsifier-free, and obtain PS glue crystal template by centrifugal drying),
Quality is that 2.000 ± 0.010 g are placed in SnCl4-TiO2In solution, the h of vacuum impregnation 12 is carried out after stirring a period of time.Obtain production
Thing obtains three using 7 h are calcined at 600 DEG C in the SX-2.5-12 type chamber type electric resistance furnaces of Tianjin Stettlen Instrument Ltd.
Tie up ordered big hole Sn4+Adulterate TiO2Composite (is labeled as 3DOM Sn-TiO2).Weigh and produced obtained by 0.3000 ± 0.0010 g
Thing 3DOM Sn-TiO2It is placed in Photoreactor, adds 3.000 ± 0.010 g and be purchased from Tianjin recovery fine chemistry industry research institute
99.0% vulcanized sodium (as sacrifice agent), adds the H for being purchased from Shanghai Jing Chun biochemical technologies Co., Ltd2PtCl6·6H2O(Pt
Content is that 37.5%), volume is 0.3 mL；Under vacuum conditions using Beijing Bo Feilai Science and Technology Ltd.s after well mixed
After PLS-SXE300/300UV xenon sources irradiate 1 h, washed 3-4 times with deionized water and ethanol respectively, be dried in vacuo 10 h
Obtain composite 3DOM Pt/Sn-TiO2
3DOM Pt/Sn-TiO2The structure of composite photo-catalyst and performance measurement：
First, surface topography and microstructure
3DOM Pt/Sn-TiO2The surface topography and Micro-Structure Analysis result of sample are shown in Fig. 1-6.It can be clearly viewed by Fig. 1
Arrive, synthesized PS glue crystal templates are neat and orderly in three dimensions, and size is homogeneous.Due in self assembling process by
Extruding, so hexagonal shape is presented in PS glueballs.Fig. 2 SEM results show, sample is in aligned orderly, in penetrating big of opening
Pore structure, macropore is neat and orderly and is hexagonal shape, and because PS glue crystal template is face-centered cubic arrangement, so can
Three apertures are seen at each macropore.Fig. 3 is sample 3DOM Pt/Sn-TiO2HR-TEM photos, as we can see from the figure
Pt (111) crystal face, Anatase TiO2(101) crystal face and Rutile Type TiO2(110) crystal face.Fig. 4 is prepared material
The XRD of material, from the figure, it can be seen that composite 3DOM Pt/Sn-TiO2In Anatase TiO be present2And Rutile Type
TiO2Characteristic peak.Fig. 5 is the N of composite2Absorption-desorption isotherm, as can clearly see from the figure, due to compared with
Big specific surface area, the thermoisopleth of three-dimensional ordered macroporous composite significantly move up.Also may be used from Fig. 6 UV-Vis figures
To prove, the load of precious metals pt makes photochemical catalyst 3DOM Sn-TiO2There is obvious absorption in visible region.
2nd, photocatalysis performance determines
To synthesized 3DOM Pt/Sn-TiO2Photocatalytic activity carried out degrading malachite green and the light of photolysis water hydrogen is urged
Change experiment.In order to evaluate the photocatalysis effect of synthesized composite, from commercially available P25, Sn-TiO2、Pt/Sn-TiO2And
3DOM Sn-TiO2Test as a comparison.
, the influence of different samples to ultraviolet degradation malachite green speed as shown in Figure 7.According to experimental data, according to public affairs
Formula1/C t -1/C 0 =kt+bCalculated, wherein,C t Exist for dyestufftConcentration (the mgL at moment-1),C 0 It is dyestuff initial concentration
(mg·L-1),kIt is speed constant (min-1),bFor intercept.As seen from Figure 7,1/C t -1/C 0 With the reaction timetBasic linear pass
System, the degraded of this explanation dyestuff malachite green follow quasi- second- order reaction kinetics.Decline solution in visible ray and simulation sunshine condition
Malachite green result is shown in Fig. 8, Fig. 9,3DOM Pt/Sn-TiO2Degraded of the composite to malachite green shows highest light
Catalytic activity, exceed well over commercially available P25.
2、3DOM Pt/Sn-TiO2Shown in photolysis water hydrogen hydrogen output such as Figure 10 (a)；Photolysis water hydrogen P25 and 3DOM
Pt/Sn-TiO2Different samples are in ethanol-water solution shown in hydrogen output result such as Figure 10 (b).As a result show, 3DOM Pt/Sn-
TiO2Composite has excellent hydrogen production potential.
Claims (2)
- A kind of 1. Pt load 3DOM Sn4+Adulterate TiO2The photo-reduction preparation method of material, weighs PS glueballs, and quality is 2.000 ± 0.010 g, C12H28O4Ti (TTIP), volume are 1.0 mL, anhydrous SnCl4, volume is 0.1 mL, H2PtCl6·6H2O, volume For 0.3 mL.Take 2.000 ± 0.050 g PS glueballs to be impregnated with methanol, filtered after stirring 30 min, treat its natural drying.Take again 2 mL TTIP and 0.1 mL anhydrous stannic chlorides are put into beaker, and the PS balls handled well are slowly added to after well mixed, are then stirred Mix 1 h；After the completion of be placed in vacuum drying chamber and vacuumize 12 h.The solid mixture for completing vacuum is finally put into Muffle furnace In, 8 h are calcined at 600 DEG C and obtain the prepared three-dimensional ordered macroporous Sn of sample4+Adulterate TiO2(it is labeled as 3DOM Sn- TiO2).Take 0. 3000 ± 0.0010 g 3DOM Sn-TiO2In deionized water, 10 min of ultrasound, photo-reduction is placed on In reactor, 3.000 ± 0.010 g vulcanized sodium (as sacrifice agent), 0.3 mL platinum acid chloride solution are separately added into.Mixing is equal After irradiating 1 h using 300 W xenon lamps under vacuum conditions after even, washed 3-4 times, be dried in vacuo with deionized water and ethanol respectively 10 h obtain composite 3DOM Pt/Sn-TiO2。
- 2. 3DOM Pt/Sn-TiO according to claim 12The photo-reduction synthetic method of composite photo-catalyst, its feature It is：PS glueballs is weighed, quality is 2.000 ± 0.010 g, C12H28O4Ti (TTIP), volume are 1.0 mL, anhydrous SnCl4, volume For 0.1 mL.The product of preparation is put into vacuum drying chamber by colloid crystal templating and extracts vacuum, institute after the h of vacuum impregnation 12 Obtain product and 7 h are calcined at 600 DEG C, obtain three-dimensional ordered macroporous Sn4+Adulterate TiO2Composite (is labeled as 3DOM Sn- TiO2).The 3DOM Sn-TiO weighed2, quality is 0. 3000 ± 0.0010 g, Na2S·9H2O, quality are 3.000 ± 0.050 G, H2PtCl6·6H2O, volume are 0.3 mL.10 min of ultrasound, are placed in photoreduction device, true after being well mixed After irradiating 1 h using 300 W xenon lamps under dummy status, washed 3-4 times with deionized water and ethanol respectively, 10 h of vacuum drying are obtained Composite 3DOM Pt/Sn-TiO2。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108479765A (en) * | 2018-01-23 | 2018-09-04 | 齐齐哈尔大学 | Counter opal structure Pt/TiO2-ZrO2Synthetic method |
| CN114931949A (en) * | 2022-01-20 | 2022-08-23 | 浙江理工大学 | Photocatalyst for carbon dioxide reduction and preparation method and application thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101850246A (en) * | 2009-04-03 | 2010-10-06 | 中国石油大学(北京) | Novel composite membrane photocatalyst and preparation method thereof |
| CN103599797A (en) * | 2013-11-26 | 2014-02-26 | 同济大学 | Method for preparing SnO2 PC/CdS QDs composite photocatalyst with high-stability visible-light catalytic activity |
| CN103721700A (en) * | 2013-12-13 | 2014-04-16 | 广西大学 | Preparation method of high-activity SnO2-TiO2 composite nanometer photocatalyst |
| CN103981537A (en) * | 2014-05-06 | 2014-08-13 | 同济大学 | Preparation method and application of Pd/3DOM TiO2/BDD electrode used for photoelectrocatalytic reduction treatment of organic pollutants |
| CN104307503A (en) * | 2014-10-28 | 2015-01-28 | 大连工业大学 | Method for preparing SnO2/TiO2 compound micro-spheres with double-shell-layer core/shell structure |
| CN105664914A (en) * | 2016-01-27 | 2016-06-15 | 安徽大学 | Preparation method of titanium dioxide/tin dioxide composite photocatalyst material |
-
2017
- 2017-07-26 CN CN201710617876.4A patent/CN107442114A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101850246A (en) * | 2009-04-03 | 2010-10-06 | 中国石油大学(北京) | Novel composite membrane photocatalyst and preparation method thereof |
| CN103599797A (en) * | 2013-11-26 | 2014-02-26 | 同济大学 | Method for preparing SnO2 PC/CdS QDs composite photocatalyst with high-stability visible-light catalytic activity |
| CN103721700A (en) * | 2013-12-13 | 2014-04-16 | 广西大学 | Preparation method of high-activity SnO2-TiO2 composite nanometer photocatalyst |
| CN103981537A (en) * | 2014-05-06 | 2014-08-13 | 同济大学 | Preparation method and application of Pd/3DOM TiO2/BDD electrode used for photoelectrocatalytic reduction treatment of organic pollutants |
| CN104307503A (en) * | 2014-10-28 | 2015-01-28 | 大连工业大学 | Method for preparing SnO2/TiO2 compound micro-spheres with double-shell-layer core/shell structure |
| CN105664914A (en) * | 2016-01-27 | 2016-06-15 | 安徽大学 | Preparation method of titanium dioxide/tin dioxide composite photocatalyst material |
Non-Patent Citations (3)
| Title |
|---|
| FENGLONG WANG 等: "Tuning Phase Composition of TiO2 by Sn4+ Doping for Efficient Photocatalytic Hydrogen Generation", 《APPLIED MATERIALS & INTERFACES》 * |
| HAI-JIE SUN等: "Multi-layer and open three-dimensionally ordered macroporous TiO2-ZrO2 composite: diversified design and the comparison of multiple mode photocatalytic performance", 《MATERIALS & DESIGN》 * |
| JIAN LIU 等: "Enhancement of photochemical hydrogen evolution over Pt-loaded hierarchical titania photonic crystal", 《ENERGY & ENVIRONMENTAL SCIENCE》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108479765A (en) * | 2018-01-23 | 2018-09-04 | 齐齐哈尔大学 | Counter opal structure Pt/TiO2-ZrO2Synthetic method |
| CN114931949A (en) * | 2022-01-20 | 2022-08-23 | 浙江理工大学 | Photocatalyst for carbon dioxide reduction and preparation method and application thereof |
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