CN104998663B - A kind of composite photo-catalyst CdS Pt@CeO2And its preparation method and application - Google Patents
A kind of composite photo-catalyst CdS Pt@CeO2And its preparation method and application Download PDFInfo
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- CN104998663B CN104998663B CN201510484406.6A CN201510484406A CN104998663B CN 104998663 B CN104998663 B CN 104998663B CN 201510484406 A CN201510484406 A CN 201510484406A CN 104998663 B CN104998663 B CN 104998663B
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Abstract
The invention discloses a kind of composite photo-catalyst CdS Pt@CeO2And its preparation method and application, belong to photocatalysis field.Composite photo-catalyst of the invention is the nano material synthesized by secondary precipitation, by ceria（CeO2）, cadmium sulfide（CdS）And platinum（Pt）Three components are constituted.Step precipitation is obtained Pt@CeO to the present invention in an inert atmosphere2, synthesis component, the adjustable CdS Pt CeO of pattern are precipitated again by adjusting cadmium source and sulphur source2Composite.Obtained photochemical catalyst of the invention, shows the activity and stability of good visible light catalytic hydrogen production by water decomposition, has widened the range of application of composite, and its preparation method is simple and easy to apply, is conducive to the large-scale promotion in visible photocatalysis water hydrogen manufacturing.
Description
Technical field
The technical field with photocatalytic hydrogen production by water decomposition is prepared the invention belongs to new material, and in particular to a kind of complex light
Catalyst CdS-Pt@CeO2And its preparation method and application.
Background technology
Increasingly serious with energy crisis and problem of environmental pollution, the Faced In Sustainable Development of human society is huge to be chosen
How war, effectively utilize solar energy and carry out pollution administration and tap a new source of energy that oneself causes the extensive concern of countries in the world.In recent years,
Photocatalitic Technique of Semiconductor is subject to various fields section because of the important application prospect in hydrogen energy source exploitation and environmental pollution improvement
The extensive concern of worker, but due to traditional TiO2It is low low with solar energy utilization ratio to there is quantum efficiency in based photocatalyst
Shortcoming, constrains the practical application of photocatalysis technology, and the exploitation design of new and effective visible light catalyst is controlled using solar energy
One of key technology of reason environmental pollution and exploitation hydrogen energy source.
The content of the invention
It is an object of the invention to provide a kind of composite photo-catalyst CdS-Pt@CeO2And its preparation method and application, system
Equipment, the synthesis condition that Preparation Method is simple and easy to apply, do not need complex and expensive gently, are conducive to promoting；It is applied to visible light catalytic
Hydrogen production by water decomposition, has the advantages that separation of charge efficiency high, catalysis activity be high and good stability.
To achieve the above object, the present invention is adopted the following technical scheme that：
A kind of composite photo-catalyst, the composite CdS-Pt@being made up of ceria, cadmium sulfide and the component of platinum three
CeO2；The mole percent of wherein ceria, cadmium sulfide and platinum is：Ceria 20 ~ 80%, cadmium sulfide 20 ~ 80%, platinum 0.01
~ 2%, the mole percent sum of three components is 100%.
Preparation method is using two-step precipitation synthetic method.Comprise the following steps that：
（1）The one step precipitation method prepare Pt@CeO2
Solid cerium salt is dissolved in deionized water cerium source solution is obtained；Alkaline matter is dissolved in deionized water alkali soluble is obtained
Liquid；Platinum source solution is obtained in deionized water using being dissolved in as the compound in platinum source；Inert gas is passed through in the solution of cerium source, while stirring
Mix side and aqueous slkali be added dropwise, continue to stir 10 ~ 60min, add platinum source solution to continue to stir 60 ~ 180min, naturally cool to room temperature,
Inert gas is closed down, precipitation uses water and ethanol centrifuge washing respectively, to ion concentration<10ppm, 40 ~ 120 DEG C of dryings 6 ~ 24 are small
When, obtain Pt@CeO2Powder；
（2）The two step precipitation method prepare CdS-Pt@CeO2
Cadmium salt is made into cadmium source solution；Sulfosalt is made into sulphur source solution；By step（1）Obtained Pt@CeO2It is scattered in
In ionized water, stirring is lower to add cadmium source solution, stirs 10 ~ 60min, adds sulphur source solution, stirs 0.5 ~ 3 h, naturally cools to
Room temperature, centrifugation, precipitation water and ethanol centrifuge washing, to ion concentration<10ppm, 40 ~ 120 DEG C of vacuum drying 6 ~ 24 are small
When, grinding obtains CdS-Pt@CeO2Powder.
Step（1）Described in solid cerium salt be one kind in cerous nitrate, cerium chloride, described alkaline matter is hydrogen-oxygen
Change the one kind in sodium, potassium hydroxide, ammoniacal liquor, the described compound as platinum source is the one kind in chloroplatinic acid, potassium chloroplatinate, institute
The concentration of the cerium source solution stated is 0.01 ~ 2 mol/L, and the concentration of described aqueous slkali is 0.1 ~ 2 mol/L, and described platinum source is molten
The concentration of liquid is 2 ~ 10 g/mL, and described inert gas is the one kind in nitrogen, argon gas；Step（2）Described in cadmium salt be vinegar
One kind in sour cadmium, cadmium nitrate, caddy, described sulfosalt is the one kind in vulcanized sodium, thioacetamide, thiocarbamide, described
The concentration of cadmium source solution is 0.01 ~ 2 mol/L, and the concentration of described sulphur source solution is 0.01 ~ 2 mol/L.
Step（1）Described in the mol ratio in alkali and cerium source be 20 ~ 120: 1, described platinum source is with the mol ratio in cerium source
0.001~0.1∶1；Step（2）Described cadmium source and Pt@CeO2Mass ratio be 0.1 ~ 5: 1, described sulphur source and Pt@CeO2's
Mass ratio is 0.1 ~ 5: 1.
Described composite photo-catalyst CdS-Pt@CeO2It is applied to visible light catalytic hydrogen production by water decomposition.
Remarkable advantage of the invention is：
（1）The present invention provide method without band press operation, without high-temperature roasting, using the reproducibility and platinum in trivalent cerium source
The step of the oxidisability one precipitation synthesis of source material, saves the expense of energy consumption, material and device, also with advantage easy to operate,
Be conducive to large-scale promotion.
（2）The present invention provides a kind of CdS-Pt@CeO first2Composite photo-catalyst, can convert the solar into chemistry
Can, efficient-decomposition aquatic products hydrogen can be under visible light realized, with the excellent of separation of charge efficiency high, catalysis activity and good stability
Point.
Brief description of the drawings
Fig. 1 is CdS-Pt@CeO in the embodiment of the present invention 12X-ray diffraction（XRD）Figure.
Fig. 2 is CdS-Pt@CeO in the embodiment of the present invention 12X-ray photoelectron power spectrum（XPS）Figure.
Fig. 3 is CdS-Pt@CeO in the embodiment of the present invention 12Transmission electron microscope（TEM）Figure.
Fig. 4 is CdS-Pt@CeO in the embodiment of the present invention 12As the situation of catalyst photolysis water hydrogen.
Fig. 5 is CdS-Pt@CeO in the embodiment of the present invention 12As the stability of catalyst photolysis water hydrogen.
Specific embodiment
Photochemical catalyst of the invention is CdS-Pt@CeO2Composite photo-catalyst, is applied to visible light catalytic hydrogen production by water decomposition.
The preparation method of the photochemical catalyst is two-step precipitation；
Comprise the following steps that：
A step precipitates Pt@CeO processed in inert atmosphere2：Solid cerium salt is obtained concentration for 0.1 ~ 2mol/ in being dissolved in deionized water
The cerium source solution of L；A kind of in chloroplatinic acid or chloroplatinate is dissolved in deionized water that concentration is obtained is the platinum source of 2-10 mg/mL
Solution；It is the aqueous slkali of 0.1-2 mol/L that alkaline matter be dissolved in deionized water to be obtained concentration；Cerium source solution side in an inert atmosphere
Stirring side is added dropwise alkali source solution, continues to stir 10 ~ 60 minutes, adds platinum source solution to continue to stir 60-180 in an inert atmosphere
Min, naturally cools to room temperature, and precipitation washs centrifugation for several times with water and ethanol respectively（To ion concentration<10ppm）, 40 ~ 120 DEG C
Drying obtains the Pt@CeO of black for 6 ~ 24 hours2Composite sample powder；Described alkali source is 20: 1~120 with the mol ratio in cerium source
∶1；The ratio between described platinum source and the amount of material in cerium source are 0.001: 1~1: 1；Described stirring is magnetic agitation, mixing speed
It is 400 ~ 1000 rad/min.
Two steps precipitation prepares CdS-Pt@CeO2：Cadmium salt is dissolved in deionized water concentration is obtained for 0.01 ~ 2mol/L cadmiums source
Solution；It is 0.01 ~ 2mol/L sulphur source solution that concentration will be obtained in sulfosalt deionized water；By obtained Pt@CeO2Be scattered in from
In sub- water, stirring is lower to add cadmium source solution, stirs 10-60min, adds sulphur source solution, stirs 0.5-3 h, naturally cools to room
Temperature, is precipitated after centrifugation, precipitation water and ethanol centrifuge washing, to ion concentration<10ppm, 40 ~ 120 DEG C of vacuum
Dry 6 ~ 24 hours, grinding obtains CdS-Pt@CeO2Composite photo catalyst powder, described cadmium source and Pt@CeO2Mass ratio
It is 0.1 ~ 5: 1；Described sulphur source and Pt@CeO2Mass ratio be 0.1 ~ 5: 1.
The composite photo-catalyst CdS-Pt@CeO of embodiment 12Preparation
Weigh 2.2 g Ce (NO3)3·6H2O is dissolved in the middle of 100 mL deionized waters, leads to nitrogen, stirs 10 min, is added
The NaOH solution 10mL of 5mol/L, continues to instill 5mg/mL H after stirring 10 min2PtCl6 The mL of solution 2, stirs 1 h, cooling
To room temperature, nitrogen is closed down, eccentric cleaning, 80 DEG C of 12 h of vacuum drying obtain Pt@CeO2；Weigh 0.344 g Pt@CeO2Ultrasound
It is scattered in 100 mL water, adds 0.1 mol/L Cd (CH3COO)2The mL of solution 20, stirs 20 min, adds while stirring
0.1 mol/L Na2The mL of S solution 20, continues to stir 2h, is cooled to room temperature, centrifuge washing, and 80 DEG C dry 12h, obtain CdS-
Pt@CeO2。
Fig. 1 illustrates composite Pt@CeO of the invention2With CdS-Pt@CeO2X-ray diffraction（XRD）Figure, from figure
It can be found that the Pt@CeO for preparing2Sample is 4 diffraction maximums occurred at 28.6 °, 33.1 °, 47.6 ° and 56.4 ° in 2 θ, respectively
Correspondence Tetragonal CeO2（JCPDS-43-1002)（111）、（200）、（220) with the characteristic diffraction peak of (311) crystal face, crystal grain
Size is about 5.3nm, is the characteristic diffraction peak that cube Pt is occurred in that at 40 ° in 2 θ；The CdS-Pt@CeO of synthesis2In not only observe
To cubic CeO2Characteristic diffraction peak, corresponded to it was additionally observed that 3 diffraction maximums, respectively at 26.5 °, 44.0 ° and 52 ° in 2 θ vertical
Square phase CdS（JCPDS：(111) 42-1411), the characteristic diffraction peak of (220) and (311) crystal face, corresponding grain size is about
4.6 nm。
Fig. 2 illustrates composite CdS-Pt@CeO of the invention2X-ray photoelectron power spectrum（XPS）Figure, can from figure
To be clearly apparent the electron binding energy peak of the element such as Cd, S, Pt, Ce and O in sample, wherein the combination energy at 71.1 and 74.3 eV
Peak corresponds to the Pt4f of simple substance Pt7/2And Pt4f5/2。
Fig. 3 is CdS-Pt@CeO in the present invention2Transmission electron microscope picture.Particle size is the CeO of 5-6 nm as can be seen from FIG.2
Nanometer sheet, and particle size is in 4-6 nm CdS particles, particle size 2-3nm Pt particles is uniform-distribution with, in CdS-Pt@
CeO2 HRTEM figures in, spacing of lattice be 0.227 nm, 0.31 nm and 0.336 nm, respectively correspond to cube Pt (111)
Crystal face, cubic CeO2's（111）Crystal face is with four directions CdS's（111）Interplanar distance.
The composite photo-catalyst CdS-Pt@CeO of embodiment 22Preparation
Weigh 2.2 g Ce (NO3)3·6H2O is dissolved in the middle of 100 mL deionized waters, leads to nitrogen, stirs 10 min, is added
The NaOH solution 10mL of 5mol/L, continues to instill 5mg/mL K after stirring 10 min2PtCl6 The mL of solution 2, stirs 1 h, cooling
To room temperature, nitrogen is closed down, eccentric cleaning, 80 DEG C of vacuum drying 12h obtain Pt@CeO2；Weigh 0.344 g Pt@CeO2Ultrasound point
Dissipate in 100mL water, add 0.1mol/L CdCl2The mL of solution 20, stirs 20 min, and 0.1 mol/L sulphur is added while stirring
The mL of urea solution 20, continues to stir 2 h, is cooled to room temperature, centrifuge washing, and 80 DEG C dry 12h, obtain CdS-Pt@CeO2。
The composite photo-catalyst CdS-Pt@CeO of embodiment 32Preparation
Weigh 2.2 g CeCl3·7H2O is dissolved in the middle of 100 mL deionized waters, leads to nitrogen, stirs 10 min, is added
The NaOH solution 10mL of 5mol/L, continues to instill 5mg/mL K after stirring 10 min2PtCl6 The mL of solution 2, stirs 1 h, cooling
To room temperature, nitrogen is closed down, eccentric cleaning, 80 DEG C of 12 h of vacuum drying obtain Pt@CeO2；Weigh 0.344 g Pt@CeO2Ultrasound point
Dissipate in 100 mL water, add 0.1mol/L CdCl2The mL of solution 20, stirs 20 min, and 0.1 mol/L is added while stirring
Na2The mL of S 20, continue to stir 2 h, are cooled to room temperature centrifuge washing, and 80 DEG C of h of drying 12 obtain CdS-Pt@CeO2。
The composite photo-catalyst CdS-Pt@CeO of embodiment 42Preparation
Weigh 2.2 g Ce (NO3)3·6H2O is dissolved in the middle of 100 mL deionized waters, leads to nitrogen, stirs 10 min, is added
The KOH solution 10mL of 5mol/L, continues to instill 5mg/mL H after stirring 10 min2PtCl6 The mL of solution 2, stirs 1 h, cooling
To room temperature, nitrogen is closed down, eccentric cleaning, 80 DEG C of 12 h of vacuum drying obtain Pt@CeO2；Weigh 0.344 g Pt@CeO2Ultrasound
It is scattered in 100 mL water, adds 0.1 mol/L Cd (CH3COO)2The mL of solution 20, stirs 20 min, adds while stirring
The mL of 0.1 mol/L thioacetyls amine aqueous solution 20, continues to stir 2 h, is cooled to room temperature centrifuge washing, and 80 DEG C of h of drying 12 are obtained
CdS-Pt@CeO2。
The composite photo-catalyst CdS-Pt@CeO of embodiment 52Preparation
Weigh 2.2 g Ce (NO3)3·6H2O is dissolved in the middle of 100 mL deionized waters, leads to argon gas, stirs 10 min, adds 5
The mL of NaOH solution 10 of mol/L, continues to instill 5 mg/mL K after stirring 10 min2PtCl6 The mL of solution 2, stirs 1 h, cold
But to room temperature, argon gas is closed down, eccentric cleaning, 80 DEG C of 12 h of vacuum drying obtain Pt@CeO2；Weigh 0.344 g Pt@CeO2Ultrasound point
Dissipate in 100 mL water, add 0.1 mol/L CdCl2The mL of solution 20, stirs 20 min, and 0.1mol/L is added while stirring
Na2The mL of S solution 20, continues to stir 2 h, is cooled to room temperature centrifuge washing, and 80 DEG C of h of drying 12 obtain CdS-Pt@CeO2。
The composite photo-catalyst CdS-Pt@CeO of embodiment 62Preparation
Weigh 2.2 g Ce (NO3)3·6H2O is dissolved in the middle of 100 mL deionized waters, leads to nitrogen, stirs 10 min, is added
The KOH solution 10mL of 5mol/L, continues to instill 5 mg/mL H after stirring 10 min2PtCl6 The mL of solution 2, stirs 1 h, cooling
To room temperature, argon gas is closed down, eccentric cleaning, 80 DEG C of 12 h of vacuum drying obtain Pt@CeO2；Weigh 0.344 g Pt@CeO2Ultrasonic disperse
In 100 mL water, 0.1 mol/LCd (NO are added3)2Solution 20mL, stirs 20 min, and 0.1mol/ is added while stirring
LNa2The mL of S solution 20, continues to stir 2 h, is cooled to room temperature, centrifuge washing, and 80 DEG C of h of drying 12 obtain CdS-Pt@CeO2。
The composite photo-catalyst CdS-Pt@CeO of embodiment 72Photocatalytic hydrogen production by water decomposition
By CdS-Pt@CeO obtained in embodiment 12Composite photocatalyst hydrogen production by water decomposition, photolysis water hydrogen
Reaction is carried out in a circulating system for atmospheric pressure sealed, and reactor is that the visible light catalytic that volume is 250 mL is decomposed
Water hydrogen manufacturing standard reaction device, using 300W xenon sources（Plus the optical filter of 420nm）, weigh 80 mg samples in reactor, so
After add 70 mL H2O and 10 mL lactic acid, and it is uniform by magnetic stirrer.Whole system first uses mechanical pump before illumination
Vacuumize, be then charged with high-purity Ar, repeat this process 3 times, eliminate air in system, open agitator and gas circulator, inhale
Turned on light after 30 min of attached balance.Gas-phase product in During Illumination squeezes into six-way valve by gas circulator, is examined by on-line chromatograph
Survey analysis.The situation of photodissociation aquatic products hydrogen as shown in figure 4, there is hydrogen to produce from figure it can be seen that after turning on light, and with
The yield increase of the extension hydrogen of light application time, when illumination 5 hours, its hydrogen output was about 8.04 mmol, and average hydrogen-producing speed is about
It is 1.62 mmolh-1, it is respectively CdS（0.076 mmol·h-1）And Pt-CdS（0.227 mmol·h-1）The 21 of sample and 7
Times, and under same illumination condition, P25 does not produce hydrogen activity.
Fig. 5 is CdS-Pt@CeO obtained in embodiment 12The product hydrogen activity stability that composite sample shines by four circulation lights
Experimental result picture, as seen from the figure first round test light shine 8 h, hydrogen output is about 1.286 mmol, through turning off the light, after system vacuumizes
Second and the three, the 4th and the 5th light cycle tests of 8 h are re-started, hydrogen output is held at being 1.285
Mmol or so, shows the CdS-Pt@CeO for preparing2Sample has very excellent product stabilized hydrogen.
The foregoing is only presently preferred embodiments of the present invention, all impartial changes done according to scope of the present invention patent with
Modification, should all belong to covering scope of the invention.
Claims (3)
1. a kind of composite photo-catalyst CdS-Pt@CeO2Preparation method, it is characterised in that：Composite CdS-Pt@CeO2By two
Cerium oxide, cadmium sulfide and the component of platinum three are constituted；The mole percent of wherein ceria, cadmium sulfide and platinum is：Ceria 20 ~
80%th, cadmium sulfide 20 ~ 80%, platinum 0.01 ~ 2%, the mole percent sum of three components is 100%；
The composite photo-catalyst uses two-step precipitation synthetic method；It is comprised the following steps that：
（1）The one step precipitation method prepare Pt@CeO2
Solid cerium salt is dissolved in deionized water cerium source solution is obtained；Alkaline matter is dissolved in deionized water aqueous slkali is obtained；
Platinum source solution is obtained in deionized water using being dissolved in as the compound in platinum source；Inert gas, side stirring are passed through in the solution of cerium source
Side is added dropwise aqueous slkali, continues to stir 10 ~ 60min, adds platinum source solution to continue to stir 60 ~ 180min, naturally cools to room temperature, closes
Stop inert gas, precipitation uses water and ethanol centrifuge washing respectively, to ion concentration<10ppm, 40 ~ 120 DEG C of dryings 6 ~ 24 hours,
Obtain Pt@CeO2Powder；
（2）The two step precipitation method prepare CdS-Pt@CeO2
Cadmium salt is made into cadmium source solution；Sulfur-containing compound is made into sulphur source solution；By step（1）Obtained Pt@CeO2It is scattered in
In ionized water, stirring is lower to add cadmium source solution, stirs 10 ~ 60min, adds sulphur source solution, stirs 0.5 ~ 3 h, naturally cools to
Room temperature, centrifugation, precipitation water and ethanol centrifuge washing, to ion concentration<10ppm, 40 ~ 120 DEG C of vacuum drying 6 ~ 24 are small
When, grinding obtains CdS-Pt@CeO2Powder；
Step（1）Described in solid cerium salt be one kind in cerous nitrate, cerium chloride, described alkaline matter is hydroxide
One kind in sodium, potassium hydroxide, ammoniacal liquor, the described compound as platinum source is the one kind in chloroplatinic acid, potassium chloroplatinate, described
The concentration of cerium source solution be 0.01 ~ 2 mol/L, the concentration of described aqueous slkali is 0.1 ~ 2 mol/L, described platinum source solution
Concentration be 2 ~ 10 g/mL, described inert gas is the one kind in nitrogen, argon gas；Step（2）Described in cadmium salt be acetic acid
One kind in cadmium, cadmium nitrate, caddy, described sulfur-containing compound is the one kind in vulcanized sodium, thioacetamide, thiocarbamide, institute
The concentration of the cadmium source solution stated is 0.01 ~ 2 mol/L, and the concentration of described sulphur source solution is 0.01 ~ 2 mol/L.
2. composite photo-catalyst CdS-Pt@CeO according to claim 12Preparation method, it is characterised in that：Step（1）
Described in the mol ratio in alkali and cerium source be 20 ~ 120: 1, described platinum source and the mol ratio in cerium source is 0.001 ~ 0.1: 1；Step
（2）Described cadmium source and Pt@CeO2Mass ratio be 0.1 ~ 5: 1, described sulphur source and Pt@CeO2Mass ratio be 0.1 ~ 5: 1.
3. composite photo-catalyst CdS-Pt@CeO obtained in a kind of preparation method as claimed in claim 12Application, its feature exists
In：Described composite photo-catalyst CdS-Pt@CeO2It is applied to visible light catalytic hydrogen production by water decomposition.
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| CN103055900A (en) * | 2013-01-28 | 2013-04-24 | 上海电力学院 | Pt/CdS composite visible-light-induced photocatalyst and preparation method thereof |
| CN104689835A (en) * | 2015-03-18 | 2015-06-10 | 湖南大学 | CeO2 (Cerium Oxide) nano-particle/CdS (Cadmium Sulfide) nano-rod composite photo-catalyst as well as preparation method and application thereof |
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| CN103055900A (en) * | 2013-01-28 | 2013-04-24 | 上海电力学院 | Pt/CdS composite visible-light-induced photocatalyst and preparation method thereof |
| CN104689835A (en) * | 2015-03-18 | 2015-06-10 | 湖南大学 | CeO2 (Cerium Oxide) nano-particle/CdS (Cadmium Sulfide) nano-rod composite photo-catalyst as well as preparation method and application thereof |
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