CN105879888A - Method for preparing CdS/BiOI heterojunction complex photocatalyst - Google Patents
Method for preparing CdS/BiOI heterojunction complex photocatalyst Download PDFInfo
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- CN105879888A CN105879888A CN201610044518.4A CN201610044518A CN105879888A CN 105879888 A CN105879888 A CN 105879888A CN 201610044518 A CN201610044518 A CN 201610044518A CN 105879888 A CN105879888 A CN 105879888A
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- cds
- bioi
- composite photocatalyst
- photocatalyst
- heterojunction composite
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 11
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 14
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 239000002131 composite material Substances 0.000 claims description 16
- ORZGULPODBRYCV-UHFFFAOYSA-M bismuth;oxygen(2-);iodide Chemical compound [O-2].[I-].[Bi+3] ORZGULPODBRYCV-UHFFFAOYSA-M 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 11
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 claims description 6
- 238000006731 degradation reaction Methods 0.000 claims description 6
- 230000015556 catabolic process Effects 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 2
- 229910052740 iodine Inorganic materials 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 229910052797 bismuth Inorganic materials 0.000 claims 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 1
- 239000011630 iodine Substances 0.000 claims 1
- 229910017604 nitric acid Inorganic materials 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 10
- 230000000593 degrading effect Effects 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 4
- WYYQVWLEPYFFLP-UHFFFAOYSA-K chromium(3+);triacetate Chemical compound [Cr+3].CC([O-])=O.CC([O-])=O.CC([O-])=O WYYQVWLEPYFFLP-UHFFFAOYSA-K 0.000 abstract description 3
- 239000008367 deionised water Substances 0.000 abstract description 3
- 229910021641 deionized water Inorganic materials 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- CBACFHTXHGHTMH-UHFFFAOYSA-N 2-piperidin-1-ylethyl 2-phenyl-2-piperidin-1-ylacetate;dihydrochloride Chemical compound Cl.Cl.C1CCCCN1C(C=1C=CC=CC=1)C(=O)OCCN1CCCCC1 CBACFHTXHGHTMH-UHFFFAOYSA-N 0.000 abstract 2
- 230000003197 catalytic effect Effects 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 21
- 238000006555 catalytic reaction Methods 0.000 description 9
- 239000004065 semiconductor Substances 0.000 description 7
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 4
- 239000002114 nanocomposite Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 2
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- CJOBVZJTOIVNNF-UHFFFAOYSA-N cadmium sulfide Chemical compound [Cd]=S CJOBVZJTOIVNNF-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- CRLHSBRULQUYOK-UHFFFAOYSA-N dioxido(dioxo)tungsten;manganese(2+) Chemical compound [Mn+2].[O-][W]([O-])(=O)=O CRLHSBRULQUYOK-UHFFFAOYSA-N 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000001420 photoelectron spectroscopy Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/138—Halogens; Compounds thereof with alkaline earth metals, magnesium, beryllium, zinc, cadmium or mercury
-
- B01J35/39—
Abstract
The invention relates to metal oxyhalogenide, in particular to a method for preparing a CdS/BiOI heterojunction complex photocatalyst with thiocarbamide, chromium acetate and bismuth oxyiodide as raw materials. Thiocarbamide and chromium acetate are added after bismuth oxyiodide is dispersed in deionized water, hydrothermal reaction is carried out after the mixture is stirred and mixed evenly, and then the CdS/BiOI heterojunction complex photocatalyst is obtained, wherein the molar ratio of CdS to BiOI is (0.5-2.0): 1. The prepared nanometer complex photocatalyst has excellent visible light catalytic activity, especially a sample with the molar ratio of CdS to BiOI being 1.0 is best in activity for degrading rhodamine B, the degrading rate reaches 90% after one hour visible light reaction, and the degrading activity is higher than that of pure BiOI and pure CdS.
Description
Technical field
The present invention relates to metal oxyhalide, refer in particular to one and prepare for raw material with thiourea, chromium acetate and Basic bismuth iodide
CdS/BiOI is combined the method for heterogeneous joint composite photo-catalyst, and especially a kind of preparation technology is simple, and product has
The nano composite photo-catalyst preparation method of good visible light catalysis activity.
Background technology
Metal oxyiodide (BiOI) is as a kind of novel semi-conducting material, due to the photocatalysis fall that it is superior
Solution performance receives much concern, and BiOI is a kind of semi-conducting material with high anisotropy, suitable forbidden band width
Degree can responding to visible light, thus have become as focus of attention in photocatalysis field；But, existing metal
The catalysis activity of oxyiodide catalyst is the lowest, it is impossible to meets the demand of reality application, therefore improves electronics
With the separation efficiency in hole reach to improve the catalysis activity of this kind of photocatalyst be still one challenging
Problem.
Hetero-junctions its due to special band structure and carrier transport characteristic, can effectively press down in light-catalyzed reaction
Light induced electron processed and hole-recombination, improve quantum efficiency, and then the catalysis that photocatalyst is greatly improved be active, sulfur
Cadmium (CdS) have narrower can band and higher conduction band positions, be that a kind of to build heterojunction structure ideal
Semiconductor light-catalyst, at present, does not also have about the hetero-junctions between manganese tungstate and cadmium sulfide and is applied to
The research of photocatalysis degradation organic contaminant.
The present invention utilizes that hydro-thermal method energy consumption is low, productivity is high, product purity is high, reaction condition is controlled, the suitability is wide
Etc. advantage, use two one-step hydrothermal low temperature to synthesize CdS/BiOI heterojunction structure, regulate different sulfurations simultaneously
Cadmium and Basic bismuth iodide mol ratio, common are organic dye by photocatalytic degradation rhodamine B (RhB) and investigate
The catalysis activity of prepared photocatalyst.
Summary of the invention
It is an object of the present invention to provide high efficiency photocatalyst based on bismuthates prepared by a kind of two one-step hydrothermals, it is achieved
The method of the nano composite photo-catalyst of photocatalytic degradation rhodamine B under visible ray.
The present invention is realized by following steps:
(1) Basic bismuth iodide dispersion is added thiourea and cadmium acetate the most afterwards, after being uniformly mixed
Carry out hydro-thermal reaction, and then obtain CdS/BiOI heterojunction composite photocatalyst, wherein CdS and with the rubbing of BiOI
That ratio is 0.5-2.0:1.
Further, the mol ratio of thiourea and cadmium acetate is 1:1.
Further, CdS and the mol ratio with BiOI are 1:1.
Further, the condition of hydro-thermal reaction is: hydro-thermal reaction 12 hours at 160 DEG C.
Further, the preparation method of described Basic bismuth iodide is as follows: takes potassium iodide preparation solution, joins etc. and to rub
Obtaining mixed solution in the solution of your bismuth nitrate, carry out hydro-thermal reaction after stirring, at 160 DEG C, hydro-thermal is anti-
Answer 12 hours, after reaction terminates, precipitation is filtered, washing, dry, obtain Basic bismuth iodide.
Further, stir described in and refer to magnetic agitation 30 minutes at normal temperatures.
(2) the CdS/BiOI heterojunction composite photocatalyst prepared by the present invention, crystallization is complete, pattern rule,
Favorable dispersibility.
(3) X-ray diffractometer (XRD), transmission electron microscope (TEM), X-ray electronic energy are utilized
The instruments such as spectrometer carry out structural analysis to product, carry out photocatalytic degradation with rhodamine B solution for target dyestuff real
Test, measure absorbance by ultraviolet-visible spectrophotometer, to assess its photocatalytic activity.
Accompanying drawing explanation
Fig. 1 is prepared CdS/BiOI heterogeneous semiconductor photocatalyst, the XRD diffraction spectrogram of BiOI, CdS.
Fig. 2 is prepared CdS/BiOI heterogeneous semiconductor photocatalyst transmission electron microscope photo figure.
Fig. 3 is the XPS photoelectron spectroscopy figure of prepared CdS/BiOI heterogeneous semiconductor photocatalyst
Fig. 4 is the time of the visible light photocatalytic degradation rhodamine B of prepared CdS/BiOI heterogeneous semiconductor photocatalyst
-degradation rate graph of a relation.
Detailed description of the invention
The preparation of embodiment 1CdS/BiOI nanometer rods
Solution containing 1mmol potassium iodide joins magnetic agitation 30 points in the solution containing 1mmol bismuth nitrate
Clock, then hydro-thermal reaction after 12 hours at 160 DEG C, the precipitation that centrifugal washing obtains, and under the conditions of 60 DEG C
It is dried to obtain Basic bismuth iodide；Taking and prepare Basic bismuth iodide and be dissolved in deionized water, ultrasonic disperse, in the condition of stirring
The lower equimolar thiourea of addition and cadmium acetate, control the mol ratio of cadmium acetate and Basic bismuth iodide be respectively 0.5,1.0,
With 2.0, carrying out hydro-thermal reaction after being uniformly mixed, at 160 DEG C, hydro-thermal reaction 12 hours, obtain after reaction
Yellow product deionized water and ethanol are cleaned, and filter, 60 DEG C of drying in thermostatic drying chamber.
The phenetic analysis of embodiment 2CdS/BiOI heterojunction composite photocatalyst
As it is shown in figure 1, it can be seen that sample after Fu He has the characteristic peak of BiOI and CdS simultaneously,
Illustrate that we have successfully prepared CdS/BiOI heterojunction composite photocatalyst.
As in figure 2 it is shown, it can be seen that Basic bismuth iodide particulate load is on the surface of pure CdS in figure.
As it is shown on figure 3, collection of illustrative plates demonstrates Bi, the existence of O, I, Cd, S element.
The visible light catalysis activity experiment of embodiment 3CdS/BiOI heterojunction composite photocatalyst
(1) compound concentration is 10mg/L rhodamine B solution, and the solution prepared is placed in dark place.
(2) CdS/BiOI heterojunction composite photocatalyst 100mg is weighed (when the mol ratio of CdS with BiOI is
The sample that 0.5:1,1.0:1,2:1 obtain is designated as BC-1, BC-2, BC-3 respectively), it is respectively placed in light-catalyzed reaction
In device, adding the target degradation solution that 100mL step (1) is prepared, magnetic agitation 30min light to be composite is urged
After agent is uniformly dispersed, opens water source, light source, carry out photocatalytic degradation experiment.
(3) every 10min draws the photocatalytic degradation liquid in reactor, for UV-visible absorbance after being centrifuged
Measurement.
(4) nano composite photo-catalyst prepared as seen from Figure 4 has the visible light catalysis activity of excellence, especially
It is that the sample degradation rhodamine B activity that mol ratio is 1.0 of CdS with BiOI is best, it is seen that photoreaction one hour
Rear degradation rate reaches 90%, and the degrading activity than pure BiOI and CdS will be high.
Claims (6)
1. the method preparing CdS/BiOI heterojunction composite photocatalyst, it is characterised in that: iodine is aoxidized
Bismuth dispersion adds thiourea and cadmium acetate the most afterwards, carries out hydro-thermal reaction after being uniformly mixed, and then
Obtaining CdS/BiOI heterojunction composite photocatalyst, wherein CdS and the mol ratio with BiOI are 0.5-2.0:1.
A kind of method preparing CdS/BiOI heterojunction composite photocatalyst, it is special
Levy and be: the mol ratio of thiourea and cadmium acetate is 1:1.
A kind of method preparing CdS/BiOI heterojunction composite photocatalyst, it is special
Levy and be: described CdS and the mol ratio with BiOI are 1:1, and the CdS/BiOI heterojunction photocatalyst of preparation exists
After reacting 90min under visible light conditions, the degradation rate of rhodamine B reaches 90%.
A kind of method preparing CdS/BiOI heterojunction composite photocatalyst, it is special
Levy and be: the condition of hydro-thermal reaction is: hydro-thermal reaction 12 hours at 160 DEG C.
A kind of method preparing CdS/BiOI heterojunction composite photocatalyst, it is special
Levy and be that the preparation method of described Basic bismuth iodide is as follows: take potassium iodide preparation solution, join equimolar nitric acid
The solution of bismuth obtains mixed solution, after stirring, carries out hydro-thermal reaction, hydro-thermal reaction 12 hours at 160 DEG C,
After reaction terminates, precipitation is filtered, washing, dry, obtain Basic bismuth iodide.
A kind of method preparing CdS/BiOI heterojunction composite photocatalyst, it is special
Levy and be: described in stir and refer to magnetic agitation 30 minutes at normal temperatures.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106966429A (en) * | 2017-03-24 | 2017-07-21 | 许昌学院 | A kind of preparation method of n-type optoelectronic thin film material |
| CN106984351A (en) * | 2017-04-01 | 2017-07-28 | 常州大学 | A kind of preparation method of bismoclite@cadmium sulfides/silver carbonate composite visible light catalyst |
| CN107866235A (en) * | 2017-10-26 | 2018-04-03 | 上海电力学院 | A kind of method for preparing heterojunction photocatalyst |
| CN111151274A (en) * | 2020-01-18 | 2020-05-15 | 河南师范大学 | Catalytic material, preparation method thereof, photocatalyst and production method of hydrogen peroxide |
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2016
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106966429A (en) * | 2017-03-24 | 2017-07-21 | 许昌学院 | A kind of preparation method of n-type optoelectronic thin film material |
| CN106984351A (en) * | 2017-04-01 | 2017-07-28 | 常州大学 | A kind of preparation method of bismoclite@cadmium sulfides/silver carbonate composite visible light catalyst |
| CN106984351B (en) * | 2017-04-01 | 2019-11-12 | 常州大学 | A kind of preparation method of bismuth oxychloride@cadmium sulfide/silver carbonate composite visible light catalyst |
| CN107866235A (en) * | 2017-10-26 | 2018-04-03 | 上海电力学院 | A kind of method for preparing heterojunction photocatalyst |
| CN107866235B (en) * | 2017-10-26 | 2020-03-20 | 上海电力学院 | Method for preparing heterojunction photocatalyst |
| CN111151274A (en) * | 2020-01-18 | 2020-05-15 | 河南师范大学 | Catalytic material, preparation method thereof, photocatalyst and production method of hydrogen peroxide |
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Application publication date: 20160824 |