CN109926070A - A kind of Mn0.5Cd0.5S/WO3The preparation method of/Au loaded photocatalyst - Google Patents
A kind of Mn0.5Cd0.5S/WO3The preparation method of/Au loaded photocatalyst Download PDFInfo
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Abstract
The invention discloses a kind of Mn0.5Cd0.5S/WO3/ Au loaded photocatalyst and preparation method thereof, belongs to inorganic functional material field.By WO3Mn is loaded to Au0.5Cd0.5Support type Mn is made on S0.5Cd0.5S photochemical catalyst, in which: Mn0.5Cd0.5S、WO3It is 1:0.2-0.5:0.02-0.05 with Au mass ratio.In the present invention, Mn0.5Cd0.5S and WO3Z- system photocatalytic system is formd, the combined efficiency of electron-hole is reduced；The introducing of nanometer Au particle can not only be with Mn0.5Cd0.5S/WO3System, which forms surface plasma body resonant vibration, enhances light absorption, also helps Mn0.5Cd0.5The migration of S conduction band electron greatly improves the photocatalytic activity of loaded catalyst.
Description
Technical field
The invention belongs to technical field of inorganic material, and in particular to a kind of Mn0.5Cd0.5S/WO3/ Au loaded photocatalyst
And preparation method thereof.
Background technique
With the continuous development of society, energy crisis is got worse, due to the continuous exploitation and consumption of fossil fuel, therewith
Bring environmental pollution constantly aggravates, therefore is badly in need of developing a kind of novel reliable, the environmentally friendly energy at present to solve to work as
Preceding problem.Hydrogen is the most element of nature, is the highest substance of content in universe, accounts for about 75%, Hydrogen Energy be it is a kind of efficiently,
Cleaning, sustainable " no charcoal " energy.The generation of photocatalysis technology can use solar energy to decompose water hydrogen making, not only solve
Energy crisis of having determined protects environment again.
Mn0.5Cd0.5S solid solution has good visible light absorption capacity and relatively narrow and adjustable forbidden bandwidth, from
And get more and more people's extensive concerning, it is a kind of very promising photocatalysis hydrogen production material.But due to Mn0.5Cd0.5S solid solution exists
The quick combination of electrons and holes under the action of light, quantum efficiency is low, limits its photocatalytic activity.The present invention is by WO3And Au
Load to Mn0.5Cd0.5The surface S, Mn0.5Cd0.5S and WO3Direct Z- system photocatalytic system is formd, electron-hole is reduced
Combined efficiency, make more light induced electrons for photodissociation aquatic products hydrogen process, greatly improve Mn0.5Cd0.5The quantum efficiency of S
With photolysis water hydrogen efficiency；Light absorption not only can be enhanced in the addition of Au nanoparticle, can also promote electron transfer rate,
Reduce the compound of light induced electron and hole, to further improve photocatalytic activity.
Summary of the invention
The present invention provides Mn that is a kind of easy to operate and being easily achieved0.5Cd0.5S/WO3/ Au loaded photocatalyst
Preparation method, Mn made from this method0.5Cd0.5S/WO3/ Au loaded photocatalyst has quantum efficiency height, photocatalysis hydrogen production
The advantages that activity is good.
A kind of Mn0.5Cd0.5S/WO3/ Au loaded photocatalyst, by WO3Mn is loaded to Au0.5Cd0.5It is made on S,
Structure feature is: Mn0.5Cd0.5S、WO3It is 1:0.2-0.5:0.02-0.05 with Au mass ratio.Mn in catalyst0.5Cd0.5S、
WO3It is 1:0.2-0.5:0.02-0.05 with Au mass ratio；In XRD 13.9 °, 22.8 °, 25.0 °, 26.8 °, 28.1 °,
28.6 °, 36.5 ° there are diffraction maximums；In XPS 35.9eV, 38.2eV, 84.3eV, 88.0eV, 161.3eV, 162.4eV,
404.85eV, 411.6eV, 530.35eV, 641.1 eV and 652.3eV, which exist, combines energy.Above-mentioned data allow that there are upper and lower 0.1
Deviation.
Pure WO can be obviously observed in XRD data analysis chart3At 13.9 °, 22.8 °, 28.1 °, 36.5 °, there are four to spread out
Peak is penetrated, (100) crystal face, (001) crystal face, (200) crystal face and (201) crystal face, WO are respectively corresponded3XRD spectrum and standard card
JCPDS no.75-2187 is consistent, illustrates WO3Sample successfully synthesizes.Pure Mn0.5Cd0.5S solid solution can be apparent from figure
Observe in 25.0 °, 26.8 °, 28.6 ° there are three diffraction maximums, respectively correspond (100) crystal face, (002) crystal face and (101) it is brilliant
Face is to match with the document reported before.Composite sample Mn0.5Cd0.5S/WO3XRD spectrum in, in addition to Mn0.5Cd0.5S's
Outside diffraction maximum, what we can also be apparent observes WO3(100), (001), (200), (201) crystal face, illustrate WO3With
Mn0.5Cd0.5S success is compound.Mn0.5Cd0.5S/WO3There are Mn in/Au sample0.5Cd0.5S and WO3Diffraction maximum, but diffracting spectrum
In do not observe Au diffraction maximum, this may be to cause since the content of Au is lower or nanometer Au particle diffraction peak is too weak.
XPS analysis Mn0.5Cd0.5S/WO3Element composition in/Au sample, it can be seen that Cd 3d from map5/2And Cd
3d3/2Combination can be 404.85eV and 411.6eV, Mn 2p3/2With Mn 2p1/2Combination can be 641.1eV and 652.3eV.It says
It include Cd element and Mn element in bright sample.S 2p in map3/2With S 2p1/2Combination can be respectively 161.3eV and
162.4eV W 4f5/2With W 4f7/2Combination can be 35.9 eV and 38.2eV.Illustrate in sample comprising S element and W element.Figure
Combination can be 530.35eV in spectrum, correspond to WO3The peak of O element in middle W-O key.Au 4f in map7/2With Au 4f5/2Knot
Closing to be 84.3eV and 88.0eV, illustrate the presence of Au element in sample, while demonstrating the content in XRD spectrum due to Au
It is lower or nanometer Au particle diffraction peak is too weak leads to the reason of Au diffraction maximum is not detected.XPS map observes that three-system is multiple
Include Cd, Mn, S, W, O and Au element in condensation material, further proves to be successfully prepared out Mn0.5Cd0.5S/WO3/ Au composite wood
Material.
Mn0.5Cd0.5S/WO3/ Au composite photocatalyst have passed through XRD and XPS characterization, and XRD shows that there are Mn0.5Cd0.5S
And WO3Diffraction maximum, while not finding other impurity peaks, illustrate that prepared sample purity is very high；Simultaneously because the load of Au
Amount is smaller, and Au diffraction maximum does not detect.XPS shows prepared Mn0.5Cd0.5S/WO3In/Au sample comprising Cd, Mn, S,
Au, W and O element, further demonstrating in prepared sample has Mn0.5Cd0.5S、WO3Exist with Au.
Composite photo-catalyst provided by the invention the preparation method is as follows:
A kind of Mn0.5Cd0.5S/WO3The preparation method of/Au loaded photocatalyst, it is characterised in that include the following steps:
1) tungstate dihydrate acid sodium and sodium chloride are dissolved in deionized water, using hydrochloric acid conditioning solution pH=1.5-2.5, with
Solution is obtained into WO after processing in 160-180 DEG C of progress hydro-thermal reaction afterwards3Solid powder.
Further, in the above-mentioned technical solutions, sodium tungstate and sodium chloride mass ratio are 5:1.
2) l-cysteine is dissolved in deionized water, adjusts pH value of solution=10-11 with NaOH, forms A mixed solution；
Acetate dihydrate cadmium and acetate dihydrate manganese are dissolved in deionized water, B mixed solution is formed；B mixed solution is added drop-wise to A to mix
In solution, solution is then obtained into Mn after processing in 120-140 DEG C of progress hydro-thermal reaction0.5Cd0.5S nano particle.
Further, in the above-mentioned technical solutions, cadmium acetate and manganese acetate molar ratio are 1:1.
3) by Mn obtained by step 2)0.5Cd0.5WO obtained by S nano particle and step 1)3Powder, which is scattered in methanol solution, to be surpassed
Sound, then in 60-90 DEG C of circulating reflux；Mn is obtained after processing0.5Cd0.5S/WO3Compound.
Further, in the above-mentioned technical solutions, Mn0.5Cd0.5S/WO3Mass ratio is 1:0.2-0.5.
4) by Mn obtained by step 3)0.5Cd0.5S/WO3Compound is scattered in deionized water, and chlorauric acid solution is then added dropwise
Ultrasound is carried out, NaBH is subsequently added into4Solution obtains Mn after post-processing0.5Cd0.5S/WO3/ Au loaded photocatalyst.
Further, in the above-mentioned technical solutions, Mn0.5Cd0.5S、WO3It is 1:0.2-0.5:0.02- with Au mass ratio
0.05。
The Mn prepared according to the method described above0.5Cd0.5S/WO3/ Au loaded photocatalyst carries out producing hydrogen experiment:
Operating condition: light source: 300W xenon lamp；The amount of catalyst: 0.05g；The concentration of sacrifice agent: the Na of 0.1mol/L2S
With the Na of 0.1mol/L2SO3.It can be seen that pure Mn0.5Cd0.5The hydrogen-producing speed of S catalyst is 23.17 μm of ol h-1, and
Mn0.5Cd0.5S/WO3The hydrogen-producing speed of/Au loaded optic catalyst is up to 90.28 μm of ol h-1, the light for showing to be remarkably reinforced urges
Change hydrogen manufacturing performance.
In order to which above-mentioned Mn is further described0.5Cd0.5S/WO3The preparation method of/Au loaded photocatalyst, it is typical to grasp
It is specific as follows to make step:
(1)WO3Preparation: the tungstate dihydrate acid sodium and sodium chloride for weighing certain mass are dissolved in deionized water, sodium tungstate and
Sodium chloride mass ratio is 5:1, and continues to stir 6h, and the pH=2 of solution is then adjusted with concentrated hydrochloric acid, continues to stir 3h, stir
Solution is transferred in polytetrafluoroethylkettle kettle after, is kept for 24 hours under conditions of 160-180 DEG C.To be cooled to after reaction
Obtained product is passed through deionized water and dehydrated alcohol filtering and washing by room temperature, and vacuum drying obtains WO3Solid powder.
(2)Mn0.5Cd0.5The preparation of S nano particle: the l-cysteine for weighing certain mass is dissolved in deionized water, so
Solution is adjusted with 6M NaOH afterwards, makes pH value of solution=10.6, forms A mixed solution；Weigh the acetate dihydrate cadmium and two of certain mass
Water acetic acid manganese is dissolved in deionized water, cadmium acetate and manganese acetate molar ratio 1:1, forms B mixed solution；B mixed under stirring molten
Drop is added in A mixed solution, and obtained uniformly mixed solution is transferred in polytetrafluoroethylkettle kettle, is protected at 120-140 DEG C
10 hours are held, are cooled to room temperature to the end of reacting, obtained product are passed through into deionized water and dehydrated alcohol filtering and washing, very
Sky is dried to obtain Mn0.5Cd0.5S nano particle.
(3)Mn0.5Cd0.5S/WO3The preparation of composite sample: by Mn obtained by step (2)0.5Cd0.5S nano particle and step 1)
Gained WO3Powder, according to Mn0.5Cd0.5S/WO3Mass ratio is 1:0.2-0.5, and mixing is scattered in ultrasound 30min in methanol solution,
Then circulating reflux 3h is carried out in 60-90 DEG C of water-bath；Be cooled to room temperature to the end of reacting, by obtained product through the past from
Sub- water and dehydrated alcohol filtering and washing, vacuum drying, obtain Mn0.5Cd0.5S/WO3Compound.
(4)Mn0.5Cd0.5S/WO3The preparation of/Au composite sample: by Mn obtained by step (3)0.5Cd0.5S/WO3Compound dispersion
In deionized water, chlorauric acid solution ultrasound 30min is then added dropwise, sodium borohydride aqueous solution is added after ultrasound, continues to stir
3h is mixed, obtained product is passed through into deionized water and dehydrated alcohol filtering and washing, vacuum drying, grinding after complete reaction, is obtained
To Mn0.5Cd0.5S、WO3The Mn for being 1:0.2-0.5:0.02-0.05 with Au mass ratio0.5Cd0.5S/WO3/ Au support type photocatalysis
Agent.
The invention has the advantages that:
The present invention is prepared as Z- system photochemical catalyst, and the introducing of nanometer Au particle then can be with Mn0.5Cd0.5S and WO3
Surface plasma body resonant vibration is formed, Mn is accelerated0.5Cd0.5The migration rate of electronics on the conduction band of S reduces light induced electron and hole
It is compound, further increase Z- system Mn0.5Cd0.5S/WO3The light-catalysed H2-producing capacity of/Au.
Detailed description of the invention
Attached drawing 1 is Mn prepared by the embodiment of the present invention 10.5Cd0.5S、Mn0.5Cd0.5S/WO3、 Mn0.5Cd0.5S/WO3/Au
XRD spectrum；
A-g is Mn prepared by the embodiment of the present invention 1 in attached drawing 20.5Cd0.5S/WO3The XPS of/Au loaded photocatalyst
Map；
Attached drawing 3 is Mn prepared by the embodiment of the present invention 10.5Cd0.5S、Mn0.5Cd0.5S/WO3、 Mn0.5Cd0.5S/WO3/Au
Photocatalytic water hydrogen generation efficiency figure.
Specific embodiment:
The present invention is further described with reference to embodiments.It is noted that the present invention is not limited to following each embodiments.
Embodiment 1
1)WO3Preparation: weigh 2gNa2WO4-2H2O and 0.4g NaCl is dissolved in 30mL deionized water, and continues to stir
Then 6h adjusts the pH=2 of solution with concentrated hydrochloric acid, continue to stir 3h, solution is transferred to 50ml polytetrafluoroethyl-ne after the completion of stirring
In alkene kettle, kept for 24 hours under conditions of 160 DEG C.Be cooled to room temperature to the end of reacting, by obtained product by deionized water and
Dehydrated alcohol filtering and washing, vacuum drying obtain WO3Solid powder.
2)Mn0.5Cd0.5The preparation of S nano particle: it weighs 2.884gL- cystine and is dissolved in 40mL deionized water, then
Solution is adjusted with 6M NaOH, makes pH value of solution=10.6, forms A mixed solution；Weigh 0.532g Cd (CH3COO)2-2H2O and
0.490g Mn(CH3COO)2-2H2O is dissolved in 25mL deionized water, forms B mixed solution；B mixed solution is added dropwise under stirring
It into A mixed solution, obtains uniformly mixed solution and is transferred in the polytetrafluoroethylkettle kettle of 100mL, 10 are kept at 120 DEG C
Hour, it is cooled to room temperature to the end of reacting, obtained product is passed through into deionized water and dehydrated alcohol filtering and washing, vacuum drying
Obtain Mn0.5Cd0.5S nano particle.
3)Mn0.5Cd0.5S/WO3The preparation of composite sample: 0.2gMn obtained by step (2) is weighed0.5Cd0.5S nano particle and
0.04gWO obtained by step 1)3Powder mixing is scattered in ultrasound 30min in 50mL methanol solution, then in 60 DEG C of water-baths into
Row circulating reflux 4h；It is cooled to room temperature to the end of reacting, obtained product is passed through into deionized water and dehydrated alcohol filtering and washing,
Vacuum drying, obtains Mn0.5Cd0.5S/WO3Compound.
4)Mn0.5Cd0.5S/WO3The preparation of/Au composite sample: 0.2gMn obtained by step (3) is weighed0.5Cd0.5S/WO3It is compound
Object is scattered in 30mL deionized water, and chlorauric acid solution (m is then added dropwiseMn0.5Cd0.5S:mAu=1:0.04), ultrasonic 30min surpasses
40mL sodium borohydride aqueous solution (n is added after soundNaHB4:nAu=5:1), continue to stir 3h, will obtain after complete reaction
Product passes through deionized water and dehydrated alcohol filtering and washing, vacuum drying, grinding, obtains Mn0.5Cd0.5S/WO3/ Au support type light
Catalyst.
This it appears that the Mn of preparation from attached drawing 10.5Cd0.5S/WO3There are Mn in/Au sample0.5Cd0.5S and WO3's
Diffraction maximum illustrates prepared Mn0.5Cd0.5S and WO3Sample purity is relatively high.But Au diffraction maximum is not observed in diffracting spectrum,
This may be to cause since the content of Au is lower or nanometer Au particle diffraction peak is too weak.The successful load of nanometer Au particle can
Further to be confirmed by XPS.
This it appears that prepared Mn from attached drawing 20.5Cd0.5S/WO3It include Cd, Mn, S, Au, W in/Au sample
With O element, further demonstrating in prepared sample has Mn0.5Cd0.5S、WO3Exist with Au.
It can be seen that prepared three-system Mn from attached drawing 30.5Cd0.5S/WO3/ Au sample hydrogen output is than two systems
Mn0.5Cd0.5S/WO3With pure Mn0.5Cd0.5S sample hydrogen output height (wherein, pure Mn0.5Cd0.5S catalyst hydrogen-producing speed is 23.17 μ
mol h-1, Mn0.5Cd0.5S/WO3Hydrogen generation efficiency is 48.66 μm of ol h-1,Mn0.5Cd0.5S/WO3The production hydrogen of/Au loaded optic catalyst
Rate is up to 90.28 μm of ol h-1).Illustrate nanometer Au particle and a WO3Introducing, effectively enhance photocatalysis performance.
Embodiment 2
1)WO3Preparation: weigh 1.5gNa2WO4-2H2O and 0.3g NaCl is dissolved in 30mL deionized water, and persistently stirs
6h is mixed, the pH=2 of solution is then adjusted with concentrated hydrochloric acid, continues to stir 3h, solution is transferred to 50ml polytetrafluoro after the completion of stirring
In ethylene kettle, kept for 24 hours under conditions of 160 DEG C.It is cooled to room temperature to the end of reacting, obtained product is passed through into deionized water
With dehydrated alcohol filtering and washing, vacuum drying obtains WO3Solid powder.
2)Mn0.5Cd0.5The preparation of S nano particle: it weighs 2.163gL- cystine and is dissolved in 40mL deionized water, then
Solution is adjusted with 6M NaOH, makes pH value of solution=10.6, forms A mixed solution；Weigh 0.399g Cd (CH3COO)2-2H2O and
0.368g Mn(CH3COO)2-2H2O is dissolved in 25mL deionized water, forms B mixed solution；B mixed solution is added dropwise under stirring
It into A mixed solution, obtains uniformly mixed solution and is transferred in 100mL polytetrafluoroethylkettle kettle, keep 10 small at 140 DEG C
When, it is cooled to room temperature to the end of reacting, obtained product is passed through into deionized water and dehydrated alcohol filtering and washing, is dried in vacuo
To Mn0.5Cd0.5S nano particle.
3)Mn0.5Cd0.5S/WO3The preparation of composite sample: 0.15gMn obtained by step (2) is weighed0.5Cd0.5S nano particle and
0.045gWO obtained by step 1)3Powder mixing is scattered in ultrasound 30min in 50mL methanol solution, then in 80 DEG C of water-baths into
Row circulating reflux 3h；To room temperature to the end of reacting cooling, obtained product is passed through into deionized water and dehydrated alcohol filtering and washing,
Vacuum drying, obtains Mn0.5Cd0.5S/WO3Compound.
4)Mn0.5Cd0.5S/WO3The preparation of/Au composite sample: 0.15gMn obtained by step (3) is weighed0.5Cd0.5S/WO3It is compound
Object is scattered in 30mL deionized water, and chlorauric acid solution (m is then added dropwiseMn0.5Cd0.5S:mAu=1:0.04), ultrasonic 30min surpasses
30mL sodium borohydride aqueous solution (n is added after soundNaHB 4:nAu=5:1), continue to stir 3h, will obtain after complete reaction
Product pass through deionized water and dehydrated alcohol filtering and washing, vacuum drying, grinding, obtain Mn0.5Cd0.5S/WO3/ Au support type
Photochemical catalyst.
Embodiment 3
1)WO3Preparation: weigh 3gNa2WO4-2H2O and 0.6g NaCl is dissolved in 30mL deionized water, and continues to stir
Then 6h adjusts the pH=2 of solution with concentrated hydrochloric acid, continue to stir 3h, solution is transferred to 50mL polytetrafluoroethyl-ne after the completion of stirring
In alkene kettle, kept for 24 hours under the conditions of 160 DEG C.It is cooled to room temperature to the end of reacting, obtained product is passed through into deionized water and nothing
Water-ethanol filtering and washing, vacuum drying obtain WO3Solid powder.
2)Mn0.5Cd0.5The preparation of S nano particle: it weighs 3.605gL- cystine and is dissolved in 40mL deionized water, then
Solution is adjusted with 6M NaOH, makes pH value of solution=10.6, forms A mixed solution；Weigh 0.665g Cd (CH3COO)2-2H2O and
0.613g Mn(CH3COO)2-2H2O is dissolved in 25mL deionized water, forms B mixed solution；B mixed solution is added dropwise under stirring
It into A mixed solution, obtains uniformly mixed solution and is transferred in 100mL polytetrafluoroethylkettle kettle, keep 10 small at 140 DEG C
When, it is cooled to room temperature to the end of reacting, obtained product is passed through into deionized water and dehydrated alcohol filtering and washing, is dried in vacuo
To Mn0.5Cd0.5S nano particle.
3)Mn0.5Cd0.5S/WO3The preparation of composite sample: 0.25gMn obtained by step (2) is weighed0.5Cd0.5S nano particle and
0.075gWO obtained by step 1)3Powder mixing is scattered in ultrasound 30min in 50mL methanol solution, then in 90 DEG C of water-baths into
Row circulating reflux 3h；It is cooled to room temperature to the end of reacting, obtained product is passed through into deionized water and dehydrated alcohol filtering and washing,
Vacuum drying, obtains Mn0.5Cd0.5S/WO3Compound.
4)Mn0.5Cd0.5S/WO3The preparation of/Au composite sample: 0.25gMn obtained by step (3) is weighed0.5Cd0.5S/WO3It is compound
Object is scattered in 30mL deionized water, and chlorauric acid solution (m is then added dropwiseMn0.5Cd0.5S:mAu=1:0.04), ultrasonic 30min surpasses
50mL sodium borohydride aqueous solution (n is added after soundNaHB4:nAu=5:1), continue to stir 3h, will obtain after complete reaction
Product passes through deionized water and dehydrated alcohol filtering and washing, vacuum drying, grinding, obtains Mn0.5Cd0.5S/WO3/ Au support type light
Catalyst.
Embodiment 4
Produce hydrogen experiment:
Operating condition: light source: 300W xenon lamp；The amount of catalyst: 0.05g；The concentration of sacrifice agent: 0.1mol/L Na2S and
0.1mol/L Na2SO3.As can be known from Fig. 3, pure Mn0.5Cd0.5S catalyst hydrogen-producing speed is 23.17 μm of ol g-1h-1, and use
Mn obtained in embodiment 10.5Cd0.5S/WO3The hydrogen-producing speed of/Au loaded optic catalyst is up to 90.28 μm of ol g-1h-1, performance
The photocatalysis hydrogen production performance being remarkably reinforced out.There is increasing in conjunction with attached drawing 1, attached drawing 2 and provable be successfully made of 3 result of attached drawing
Strong photocatalysis hydrogen production performance Mn0.5Cd0.5S/WO3/ Au loaded photocatalyst.
Composite photo-catalyst is prepared using embodiment 2-3 and obtains similar production hydrogen effect.
Embodiment above describes basic principles and main features of the invention and advantages.The technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe originals of the invention
Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (10)
1. a kind of Mn0.5Cd0.5S/WO3/ Au loaded photocatalyst, it is characterised in that: Mn in catalyst0.5Cd0.5S、WO3With Au
Mass ratio is 1:0.2-0.5:0.02-0.05；At 13.9 °, 22.8 °, 25.0 °, 26.8 °, 28.1 °, 28.6 °, 36.5 ° in XRD
There are diffraction maximums；In XPS 35.9eV, 38.2eV, 84.3eV, 88.0eV, 161.3eV, 162.4eV, 404.85eV,
411.6eV, 530.35eV, 641.1eV and 652.3eV, which exist, combines energy.
2. a kind of Mn as described in claim 10.5Cd0.5S/WO3The preparation method of/Au loaded photocatalyst, it is characterised in that packet
Include following steps:
1) tungstate dihydrate acid sodium and sodium chloride are dissolved in deionized water, using hydrochloric acid conditioning solution pH=1.5-2.5, then will
Solution obtains WO after processing in 160-180 DEG C of progress hydro-thermal reaction3Powder；
2) l-cysteine is dissolved in deionized water, adjusts pH value of solution=10-11 with NaOH, forms A mixed solution；By two water
Cadmium acetate and acetate dihydrate manganese are dissolved in deionized water, form B mixed solution；B mixed solution is added dropwise to A mixed solution
In, solution is then obtained into Mn after processing in 120-140 DEG C of progress hydro-thermal reaction0.5Cd0.5S nano particle；
3) by Mn obtained by step 2)0.5Cd0.5WO obtained by S nano particle and step 1)3Powder is scattered in ultrasound in methanol solution, with
Mn is obtained after 60-90 DEG C of circulating reflux, processing afterwards0.5Cd0.5S/WO3Compound；
4) by Mn obtained by step 3)0.5Cd0.5S/WO3Compound is scattered in deionized water, and chlorauric acid solution is then added dropwise and is surpassed
Sound is then added sodium borohydride solution, obtains Mn after processing0.5Cd0.5S/WO3/ Au loaded photocatalyst.
3. the preparation method of loaded photocatalyst according to claim 2, it is characterised in that: wolframic acid described in step 1)
Sodium and sodium chloride mass ratio are 5:1.
4. the preparation method of loaded photocatalyst according to claim 2, it is characterised in that: acetic acid described in step 2)
Cadmium and manganese acetate molar ratio are 1:1.
5. the preparation method of loaded photocatalyst according to claim 2, it is characterised in that: described in step 3)
Mn0.5Cd0.5S/WO3Mass ratio is 1:0.2-0.5.
6. the preparation method of loaded photocatalyst according to claim 2, it is characterised in that: described in step 4)
Mn0.5Cd0.5S、WO3It is 1:0.2-0.5:0.02-0.05 with Au mass ratio；NaBH4With Au molar ratio 5:1.
7. a kind of Mn according to claim 20.5Cd0.5S/WO3The preparation method of/Au loaded photocatalyst, feature exist
In: in step 1), 2) and 3) in, operate as follows: being cooled to room temperature after processing, through water and ethyl alcohol filtering and washing, be dried in vacuo.
8. a kind of Mn according to claim 20.5Cd0.5S/WO3The preparation method of/Au loaded photocatalyst, feature exist
In: it is operated in step 4), after processing as follows: through water and ethyl alcohol filtering and washing, vacuum drying, grinding.
9. Mn described according to claim 10.5Cd0.5S/WO3Application of/Au the loaded photocatalyst in Photocatalyzed Hydrogen Production.
10. the Mn according to claim 90.5Cd0.5S/WO3Application of/Au the loaded photocatalyst in Photocatalyzed Hydrogen Production,
It is characterized by: operating condition is, light source: 300W xenon lamp；The amount of catalyst: 0.05g；The concentration of sacrifice agent: 0.1mol/L's
Na2The Na of S and 0.1mol/L2SO3。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910255018.9A CN109926070B (en) | 2019-04-01 | 2019-04-01 | Mn (manganese)0.5Cd0.5S/WO3Preparation method of Au supported photocatalyst |
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| CN110586137A (en) * | 2019-09-24 | 2019-12-20 | 河南师范大学 | Containing Mn0.5Cd0.5Preparation method of S and Au supported photocatalyst |
| CN113649048A (en) * | 2021-08-24 | 2021-11-16 | 青岛科技大学 | C-coated W5O14Quantum dot/C, N, O codoped MnxCd1-xS assembly and preparation method thereof |
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| CN108855143A (en) * | 2018-07-09 | 2018-11-23 | 河南师范大学 | A kind of Z-type structure ZnIn2S4/Ag/Bi2WO6The preparation method of composite photo-catalyst |
| CN108855138A (en) * | 2018-07-09 | 2018-11-23 | 河南师范大学 | A kind of Z-type structure Mn0.5Cd0.5S/Ag/Bi2WO6Composite photocatalyst and preparation method thereof |
| CN108855171A (en) * | 2018-07-09 | 2018-11-23 | 河南师范大学 | A kind of Zn0.5Cd0.5S/Cu2(OH)2CO3The preparation method of/carbon black loaded photocatalyst |
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| CN108855143A (en) * | 2018-07-09 | 2018-11-23 | 河南师范大学 | A kind of Z-type structure ZnIn2S4/Ag/Bi2WO6The preparation method of composite photo-catalyst |
| CN108855138A (en) * | 2018-07-09 | 2018-11-23 | 河南师范大学 | A kind of Z-type structure Mn0.5Cd0.5S/Ag/Bi2WO6Composite photocatalyst and preparation method thereof |
| CN108855171A (en) * | 2018-07-09 | 2018-11-23 | 河南师范大学 | A kind of Zn0.5Cd0.5S/Cu2(OH)2CO3The preparation method of/carbon black loaded photocatalyst |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110586137A (en) * | 2019-09-24 | 2019-12-20 | 河南师范大学 | Containing Mn0.5Cd0.5Preparation method of S and Au supported photocatalyst |
| CN110586137B (en) * | 2019-09-24 | 2022-04-01 | 河南师范大学 | Containing Mn0.5Cd0.5Preparation method of S and Au supported photocatalyst |
| CN113649048A (en) * | 2021-08-24 | 2021-11-16 | 青岛科技大学 | C-coated W5O14Quantum dot/C, N, O codoped MnxCd1-xS assembly and preparation method thereof |
| CN113649048B (en) * | 2021-08-24 | 2023-09-12 | 青岛科技大学 | C cladding W 5 O 14 Quantum dot/C, N, O co-doped Mn x Cd 1-x S assembly and preparation method thereof |
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