CN107552033A - A kind of preparation method of oxygen-containing vacancy strontium titanate visible light catalyst - Google Patents

A kind of preparation method of oxygen-containing vacancy strontium titanate visible light catalyst Download PDF

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CN107552033A
CN107552033A CN201710767477.6A CN201710767477A CN107552033A CN 107552033 A CN107552033 A CN 107552033A CN 201710767477 A CN201710767477 A CN 201710767477A CN 107552033 A CN107552033 A CN 107552033A
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srtio
oxygen
preparation
visible light
strontium titanate
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CN107552033B (en
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李越湘
干超
彭绍琴
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Ruijin Industrial Investment Development Co ltd
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Nanchang University
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    • 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

A kind of preparation method of oxygen-containing vacancy strontium titanate visible light catalyst, the surface that elemental metals are supported on to strontium titanates obtain elemental metals/strontium titanates, and then, under reducibility gas or inert gas atmosphere, low temperature calcination obtains elemental metals/SrTiO3‑x.The elemental metals loaded in the present invention are in addition to as co-catalyst, moreover it is possible to temperature needed for generation Lacking oxygen is greatly lowered.Such as Pt/SrTiO3In H2/N2Lower 150 DEG C of gaseous mixture can obtain Lacking oxygen, and reaction condition is gentle, energy consumption is low.The hydrogen manufacturing performance of the oxygen-containing vacancy photochemical catalyst of preparation significantly improves.

Description

A kind of preparation method of oxygen-containing vacancy strontium titanate visible light catalyst
Technical field
The invention belongs to photocatalyst material preparing technical field, is related to the preparation of strontium titanates hydrogen production photocatalyst.
Background technology
The progress of human society causes energy resource consumption sharp increase with developing rapidly for industry, also results in the environment of getting worse Pollution.Hydrogen as a kind of cleaning, reusable edible, high fuel value chemical fuel and cause people widely to pay close attention to.Produce hydrogen The method of gas has a variety of, and main source is natural gas, oil, biomass and coal etc. at present, but these methods need to consume not Reproducible fossil fuel, while GHG carbon dioxide can be also produced, it is unfavorable for environmental protection.Therefore, find it is new can The hydrogen production process of regeneration turns into people's focus of attention.Solar energy is the inexhaustible disposable energy.Utilize solar energy photocatalytic Hydrogen production by water decomposition is preferable hydrogen production process.Therefore, people are developing efficient hydrogen production photocatalyst always.
In numerous catalyst, Ca-Ti ore type semiconductor light-catalyst SrTiO3Due to stable structure and excellent Photocatalysis performance and receive much concern.In SrTiO3Surface Creation Lacking oxygen, be advantageous to light induced electron by SrTiO3Surface Lacking oxygen Capture, so as to prevent the compound of light induced electron and hole, SrTiO can be improved3Photocatalysis performance.But due to SrTiO3It is brilliant Body Stability Analysis of Structures, the combination of oxygen can be higher, the extremely difficult generation of Lacking oxygen.SrTiO at present3The condition for obtaining Lacking oxygen is very severe Carve, it is necessary under reducing atmosphere or high vacuum high temperature（More than 800 DEG C）Calcining, or Ar under high temperature high vacuum+Ion beam sputtering.For Reduction Lacking oxygen SrTiO3Preparation temperature, Tan etc. are by by NaBH4And SrTiO3Mixed calcining, 300 DEG C can obtain oxygen sky Position.But NaBH4Cost is high, limits practical application.Therefore, it is necessary to the gentle Lacking oxygen SrTiO of developing low-cost, reaction condition3 Preparation method.
The content of the invention
It is an object of the invention to provide a kind of preparation method of oxygen-containing vacancy strontium titanate visible light catalyst, on strontium titanates surface Generate Lacking oxygen.
Lacking oxygen strontium titanates composition of the present invention is SrTiO3-x, x expression strontium titanates surface loses oxygen generation Lacking oxygen Amount.
The preparation method of a kind of oxygen-containing vacancy strontium titanate visible light catalyst of the present invention, it is characterised in that by elemental gold The surface that category is supported on strontium titanates obtains elemental metals/strontium titanates.Then, it is low under reducibility gas or inert gas atmosphere Temperature calcining obtains elemental metals/SrTiO3-x。
Described elemental metals include Pt, Pd, Ru, Rh, Cu, Ni, Co or Fe.It is preferred that Pt.
Described reducibility gas is H2Or H2/N2Gaseous mixture.In the atmosphere, calcining heat is 150-400 DEG C, optimization Temperature be 200-300 DEG C.
Described inert gas is N2Or Ar.In the atmosphere, calcining heat is 300-500 DEG C；The temperature of optimization is 400 ℃。
Reacted in photocatalysis hydrogen production, elemental metals typically play co-catalyst.It is an advantage of the invention that elemental metals remove As outside co-catalyst, moreover it is possible to temperature needed for generation Lacking oxygen is greatly lowered.Such as Pt/SrTiO3In H2/N2Under gaseous mixture 150 DEG C can obtain Lacking oxygen, and reaction condition is gentle, energy consumption is low.The hydrogen manufacturing performance of the oxygen-containing vacancy photochemical catalyst of preparation is notable Improve.
Brief description of the drawings
Fig. 1 is in embodiment 1, and photo-reduction carries Pt amounts 0.50 wt%, H2/N2Under gaseous mixture atmosphere, prepared by different temperatures calcining Pt/SrTiO3-xXRD.
Fig. 2 is in embodiment 1, and photo-reduction carries Pt amounts 0.50 wt%, H2/N2Under gaseous mixture atmosphere, prepared by different temperatures calcining Pt/SrTiO3-xUV-vis diffusing reflection absorption spectrums.
Fig. 3 is in embodiment 1, and photo-reduction carries Pt amounts 0.50wt%, H2/N2Under gaseous mixture atmosphere, prepared by different temperatures calcining Pt/SrTiO3-xProduction hydrogen activity figure.
Fig. 4 is in embodiment 1, and photo-reduction carries Pt amounts 0.50wt%, H2/N2Under gaseous mixture atmosphere, prepared by 300 DEG C of calcining 1h Pt/SrTiO3-x-H2/N2- 300 DEG C of production stabilized hydrogen test chart.
Fig. 5 is in embodiment 2, and photo-reduction carries Pt amounts 1.0wt%, H2/N2Under gaseous mixture atmosphere, prepared by different temperatures calcining Pt/SrTiO3-xXRD.
Fig. 6 is in embodiment 2, and photo-reduction carries Pt amounts 1.0wt%, H2/N2Under gaseous mixture atmosphere, prepared by different temperatures calcining Pt/SrTiO3-xProduction hydrogen activity figure.
Fig. 7 is NaBH in embodiment 34Electronation carries Pt amounts 0.50wt%, H2/N2Under gaseous mixture atmosphere, 200 DEG C of calcinings Pt/SrTiO prepared by 1h3-x -H2/N2- 200 DEG C of production hydrogen activity figure.
Fig. 8 is in embodiment 4, and photo-reduction carries Pt amounts 0.50wt%, N2Under atmosphere, the Pt/ prepared is calcined with different temperatures SrTiO3-xXRD.
Fig. 9 is in embodiment 4, and photo-reduction carries Pt amounts 0.50 wt%, N2Under atmosphere, the Pt/ of different temperatures calcining preparation SrTiO3-xUV-vis diffusing reflection absorption spectrums.
Figure 10 is in embodiment 4, and photo-reduction carries Pt amounts 0.50wt%, N2Under atmosphere, the Pt/ of different temperatures calcining preparation SrTiO3-xProduction hydrogen activity figure.
Embodiment
The present invention will be described further by following examples.But present disclosure is not limited to this.
Embodiment 1.
（1）Solvent hot preparation SrTiO3。
Weigh 10mmol tetra-n-butyl titanates be dissolved in 50mL ethylene glycol, magnetic stirring 1h be designated as solution A；Weigh 10mmol nitre Sour strontium is dissolved in 10mL H2O is designated as solution B；Solution B is slowly dropped in solution A, continue stir 30min obtain gluey mixing Thing C；The 10mLNaOH aqueous solution (5.0mol/L) is slowly added dropwise into colloidal mixture C, continues stirring 30min and obtains mixed solution D.Mixed solution D is transferred in 100mL polytetrafluoroethylliner liners, in autoclave after 180 DEG C of reaction 16h, with distillation For several times, 60 DEG C of vacuum drying, grinding obtains SrTiO for water, ethanol eccentric cleaning3。
（2）SrTiO3Photo-reduction carries Pt（0.50wt%）.
Weigh SrTiO3The g of sample 1.0, measure H2PtCl6Solution 13.3mL（1.93×10-3 Mol/L, carry Pt amounts 0.50wt%）, it is added to ultrasonic 20min in 20mL absolute ethyl alcohols and is uniformly dispersed, the lower ultraviolet high-pressure mercury lamps illumination of nitrogen protection 2h, with distilled water, ethanol eccentric cleaning for several times, 60 DEG C of vacuum drying, grinding obtain Pt/SrTiO3。
（3）H2/N2Gaseous mixture calcining prepares Pt/SrTiO3-x。
Take Pt/SrTiO3Sample 0.15g, is put into tube furnace, leads to H2/N2（Hydrogen volume concentration is 5 %）Gaseous mixture is forged Burn, temperature is respectively 150 DEG C, 200 DEG C, 300 DEG C, 400 DEG C, calcination time 1h.Obtain Pt/SrTiO3-x, it is expressed as Pt/ SrTiO3-x-H2/N2-150℃、Pt/SrTiO3-x-H2/N2-200℃、Pt/SrTiO3-x-H2/N2-300℃、Pt/SrTiO3-x- H2/N2-400℃。
（4）Photocatalysis hydrogen production performance test.
Light-catalyzed reaction is carried out in a Pyrex flasks of the about 190mL with plane light window.By 0.050g catalyst, 0.10g glucose and 100mL NaOH（Concentration 1.0 × 10-2mol/L）The aqueous solution is added in illumination bottle.Using 400W high-pressure mercury Lamp is as light source.Supersonic oscillations 5min dispersed catalysts are used before reaction, logical high pure nitrogen 20min drives the oxygen in reaction system Gas, reaction carry out 3h at room temperature, catalyst is kept suspended state by magnetic agitation.Bottleneck silicone rubber seal, reaction Gas-phase product uses chromatographic by silicon rubber sampling analysis（Detector is TCD, carrier gas N2, splitter is NaX points Son sieve post）, quantified by external standard method.
Fig. 1 is H2/N2Under gaseous mixture atmosphere, the Pt/SrTiO of different temperatures calcining preparation3-xXRD.Can from Fig. 1 Go out, strontium titanates is cubic perovskite structure, and photo-reduction carries Pt（Carry Pt amounts 0.50wt%）, and in H2/N2Under gaseous mixture atmosphere, with not Before and after synthermal calcining, XRD spectrum is essentially identical, and crystal formation does not change.
Fig. 2 is H2/N2Under gaseous mixture atmosphere, the Pt/SrTiO of different temperatures calcining preparation3-xUV-vis diffusing reflections absorb Spectrum.As can be seen from Figure 2, H2/N2Under mixed atmosphere, 150 DEG C of calcinings, Pt/SrTiO is obtained3-x-H2/N2- 150 DEG C of visible ray Light absorbs are compared to Pt/SrTiO3It is remarkably reinforced, illustrates that 150 DEG C of existing Lacking oxygens produce.With the raising of calcining heat, UV- Vis diffusing reflection absorption spectrums are in visible region（Wavelength is more than 400 nm）Absorption steps up, and illustrates the higher generation oxygen of temperature Room is more.
Fig. 3 is H2/N2Under gaseous mixture atmosphere, the Pt/SrTiO of different temperatures calcining preparation3-xProduction hydrogen activity figure.From Fig. 3 It can be seen that Pt/SrTiO3-xCompare Pt/SrTiO3Photocatalytic hydrogen production activity significantly improves, living when calcining heat is 300 DEG C Property highest, illumination 3h reaches 261 μm of ol, is Pt/SrTiO3（116μmol）2.25 times.
Fig. 4 is Pt/SrTiO3-x -H2/N2- 300 DEG C of production stabilized hydrogen test chart.By 0.050 g catalyst, 0.10g Portugals Grape sugar and the 100mL NaOH aqueous solution（Concentration is 10-2mol/L）It is placed in illumination bottle.Using 400W high-pressure sodium lamp as light Source, illumination 3h is a cycle at room temperature；When doing next cycle, centrifugation divides the catalysis that recovery catalyst, polishing lose on a small quantity Agent rejoins electron donor to 0.050 g.As shown in figure 4,5 cycles of catalyst reaction, stability in 15 hours compared with It is good.
Embodiment 2.
（1）SrTiO3Preparation with the step of embodiment 1（1）.
（2）SrTiO3Photo-reduction carries Pt（1.0wt%）.
Weigh SrTiO3The g of sample 1.0, measure H2PtCl6Solution 26.6mL（1.93×10-3 Mol/L, carry Pt amounts 1.0wt%）, it is added to ultrasonic 20min in 20mL absolute ethyl alcohols and is uniformly dispersed, the lower ultraviolet high-pressure mercury lamps illumination 2h of nitrogen protection, With distilled water, ethanol eccentric cleaning for several times, 60 DEG C of vacuum drying, grinding obtain photo-reduction and carry the Pt/ that Pt amounts are 1.0wt% SrTiO3。
（3）H2/N2Gaseous mixture calcining prepares Pt/SrTiO3-xWith the step of embodiment 1（3）.
（4）Photocatalysis hydrogen production performance test is the same as the step of embodiment 1（4）.
Fig. 5 is H2/N2Under gaseous mixture atmosphere, the Pt/SrTiO of different temperatures calcining preparation3-xXRD.Can from Fig. 5 Go out, strontium titanates carries Pt in photo-reduction（Carry Pt amounts 1.0wt%）, in H2/N2Under gaseous mixture atmosphere, before and after different temperatures calcining, XRD Compose essentially identical, crystal formation does not change.
Fig. 6 is H2/N2Under gaseous mixture atmosphere, the Pt/SrTiO of different temperatures calcining preparation3-xProduction hydrogen activity figure.From Fig. 6 It can be seen that, when load Pt amounts are 1.0wt%, different temperatures（200℃、300℃、400℃）Calcining, obtained Pt/SrTiO3-xLight Catalyzing manufacturing of hydrogen activity is essentially identical（Illumination 3h hydrogen outputs are about 210 μm of ol）, but Pt/SrTiO3-xWith Pt/SrTiO3（Illumination 3h hydrogen outputs are 103 μm of ol）Compare, photocatalytic hydrogen production activity all significantly improves.
Embodiment 3.
（1）SrTiO3Preparation with the step of embodiment 1（1）.
（2）NaBH4Electronation carries Pt（0.50wt%）.
Weigh SrTiO3The g of sample 1.0, measure H2PtCl6Solution 13.3mL（1.93×10-3 Mol/L, carry Pt amounts 0.50wt%）, it is added to ultrasonic 20min in 50mL distilled water and is uniformly dispersed.Weigh NaBH49.7 mg are dissolved in 10mL distilled water (NaBH4With H2PtCl6Mol ratio be 10：1), it is slowly dropped to above-mentioned SrTiO3With H2PtCl6Mixed liquor in, normal temperature magnetic stirs Mix 4h.With distilled water, ethanol eccentric cleaning for several times, 60 DEG C of vacuum drying, grinding obtain NaBH4Electronation carries Pt amounts 0.50wt% Pt/SrTiO3。
（3）H2/N2Gaseous mixture calcining prepares Pt/SrTiO3-xWith the step 3 of embodiment 1, calcining heat is 200 DEG C
（4）Photocatalysis hydrogen production performance test is the same as the step of embodiment 1（4）.
Fig. 7 is NaBH4Electronation carries Pt, Pt/SrTiO3-x -H2/N2- 200 DEG C of production hydrogen activity figure.Can from Fig. 7 Go out, NaBH4When electronation, load Pt amounts are 0.50wt%, calcining heat is 200 DEG C, and illumination 3h hydrogen outputs reach 157 μm of ol, are Pt/SrTiO3（Illumination 3h hydrogen outputs are 102 μm of ol）1.54 times.In embodiment 1, Pt is carried using photo-reduction method, 200 DEG C are forged Burn, illumination 3h hydrogen outputs reach 235 μm of ol, are not calcine Pt/SrTiO3（Illumination 3h hydrogen outputs are 116 μm of ol）2.03 times. Two kinds of load Pt methods（Photo-reduction carries Pt and NaBH4Electronation carries Pt）Compare, photo-reduction carries Pt and obtains Pt/SrTiO3And forge Pt/SrTiO is obtained after burning3-x, the photocatalysis hydrogen production performance of catalyst is all higher than NaBH4Chemical reduction method carries Pt/ made from Pt SrTiO3And Pt/SrTiO3-x。
Embodiment 4.
（1）SrTiO3Preparation with the step of embodiment 1（1）
（2）SrTiO3Photo-reduction carries Pt（0.50wt%）With the step of embodiment 1（2）.
（3）N2The calcining of atmosphere different temperatures prepares Pt/SrTiO3-x。
Take Pt/SrTiO3Sample 0.15g, it is put into tube furnace and leads to N2Atmosphere is calcined, temperature is respectively 200 DEG C, 300 DEG C, 400 DEG C, calcination time 1h.Obtain Pt/SrTiO3-x, it is expressed as Pt/SrTiO3-x-N2-200℃、Pt/SrTiO3-x-N2- 300℃、Pt/SrTiO3-x-N2-400℃。
（4）Photocatalysis hydrogen production performance test is the same as the step of embodiment 1（4）.
Fig. 8 is N2The Pt/SrTiO that under atmosphere prepared by different temperatures calcining3-xXRD.As can be seen from Figure 8, photo-reduction carries Pt SrTiO3And in N2Before and after atmosphere is calcined with different temperatures, XRD spectrum is essentially identical, and crystal formation does not change.
Fig. 9 is N2The Pt/SrTiO that under atmosphere prepared by different temperatures calcining3-xUV-vis diffusing reflection absorption spectrums.From Fig. 9 It can be seen that, N2The lower 200 DEG C of calcinings of atmosphere, Pt/SrTiO3-x-H2/N2- 200 DEG C of light absorbs are compared to Pt/SrTiO3It is only faint Enhancing, illustrates N2This temperature is seldom to produce the amount of Lacking oxygen under atmosphere.Calcining heat brings up to 300 DEG C, UV-vis diffusing reflections Absorption spectrum is in visible region（Wavelength is more than 400 nm）Absorption is remarkably reinforced, and illustrates SrTiO3N after load Pt2Lower 300 DEG C of atmosphere Calcining can produce Lacking oxygen.
Figure 10 is N2The Pt/SrTiO that under atmosphere prepared by different temperatures calcining3-xProduction hydrogen activity figure.As can be seen from Figure 10 Pt/SrTiO3-xCompare Pt/SrTiO3Photocatalytic hydrogen production activity increases, catalyst Pt/SrTiO3-x-N2- 200 DEG C of illumination 3h hydrogen outputs reach 136 μm of ol, are Pt/SrTiO3（Illumination 3h hydrogen outputs are 116 μm of ol）1.17 times, now SrTiO3Oxygen is empty The content of position is seldom, activity lifting unobvious；Catalyst Pt/SrTiO3-x-N2- 400 DEG C of illumination 3h hydrogen outputs reach 175 μm of ol, It is Pt/SrTiO31.51 times, now SrTiO3The content of Lacking oxygen is more, and activity is obviously improved.

Claims (6)

1. a kind of preparation method of oxygen-containing vacancy strontium titanate visible light catalyst, it is characterised in that elemental metals are supported on strontium titanates Surface obtain elemental metals/strontium titanates, then, under reducibility gas or inert gas atmosphere, low temperature calcination obtains simple substance Metal/SrTiO3-x。
2. the preparation method of a kind of oxygen-containing vacancy strontium titanate visible light catalyst according to claim 1, it is characterised in that described Elemental metals be Pt, Pd, Ru, Rh, Cu, Ni, Co or Fe.
3. the preparation method of a kind of oxygen-containing vacancy strontium titanate visible light catalyst according to claim 1, it is characterised in that described Reducibility gas be H2Or H2/N2Gaseous mixture, in the atmosphere, calcining heat is 150-400 DEG C.
4. the preparation method of a kind of oxygen-containing vacancy strontium titanate visible light catalyst according to claim 3, it is characterised in that described Calcining heat is 200-300 DEG C.
5. the preparation method of a kind of oxygen-containing vacancy strontium titanate visible light catalyst according to claim 1, it is characterised in that described Inert gas be N2Or Ar, in the atmosphere, calcining heat is 300-500 DEG C.
6. the preparation method of a kind of oxygen-containing vacancy strontium titanate visible light catalyst according to claim 5, it is characterised in that described Calcining heat be 400 DEG C.
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CN108421555A (en) * 2018-02-24 2018-08-21 江南大学 A kind of preparation method of cobalt/carboritride hydridization photochemical catalyst
CN108579739B (en) * 2018-04-09 2020-09-22 华北电力大学 Method for preparing aldehyde/ketone by selectively oxidizing alcohol under mild condition
CN108579739A (en) * 2018-04-09 2018-09-28 华北电力大学 Method of the selective oxidation alcohol to prepare aldehyde/ketone under a kind of temperate condition
CN108772069A (en) * 2018-04-13 2018-11-09 天津大学 Composite photo-catalyst of strontium titanates supported copper particle and preparation method thereof and device
CN109046319B (en) * 2018-09-25 2021-04-16 安徽大学 Preparation method of molybdenum strontium oxide photocatalytic material
CN109046319A (en) * 2018-09-25 2018-12-21 安徽大学 A kind of preparation method of molybdenum oxide strontium catalysis material
CN109663584A (en) * 2018-12-19 2019-04-23 中南大学 The preparation method of Lacking oxygen type metal oxide semiconductor photochemical catalyst
CN109663584B (en) * 2018-12-19 2021-07-06 中南大学 Preparation method of oxygen vacancy type metal oxide semiconductor photocatalyst
CN110054215A (en) * 2019-03-20 2019-07-26 常州大学 Morphology controllable SrTiO3The preparation and its application of flower ball-shaped serial nano material
CN110743541A (en) * 2019-10-10 2020-02-04 苏州大学 Rhodium-doped strontium titanate inverse protein material, preparation method thereof and application thereof in removing organic pollutants through piezoelectric synergistic photocatalysis
WO2021068905A1 (en) * 2019-10-10 2021-04-15 苏州大学 Rhodium-doped strontium titanate inverse opal material, preparation method therefor, and application thereof in piezoelectric cooperative photocatalytic removal of organic pollutants
CN113428835A (en) * 2021-06-24 2021-09-24 清华大学 Method for preparing hydrogen by photocatalysis by using lignocellulose
CN113441157A (en) * 2021-07-02 2021-09-28 南昌大学 Photoreduction synthesis method of supported high-dispersion metal monatomic catalyst
CN114471536A (en) * 2022-02-17 2022-05-13 辽宁大学 MnCr with adjustable oxygen vacancy concentration2O4Photocatalyst and preparation method and application thereof
CN114950435A (en) * 2022-06-21 2022-08-30 阜阳师范大学 Preparation method of cobalt-oxygen catalyst, product and application thereof

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