CN105457656A - Preparation method and application of heterojunction photocatalyst - Google Patents
Preparation method and application of heterojunction photocatalyst Download PDFInfo
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- CN105457656A CN105457656A CN201510936930.2A CN201510936930A CN105457656A CN 105457656 A CN105457656 A CN 105457656A CN 201510936930 A CN201510936930 A CN 201510936930A CN 105457656 A CN105457656 A CN 105457656A
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229910052980 cadmium sulfide Inorganic materials 0.000 claims abstract description 60
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 claims abstract description 54
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 24
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 15
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical compound N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 claims abstract description 11
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 35
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical compound O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 claims description 28
- 238000001035 drying Methods 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 20
- 238000005406 washing Methods 0.000 claims description 20
- 238000001914 filtration Methods 0.000 claims description 19
- 239000002105 nanoparticle Substances 0.000 claims description 14
- 239000000725 suspension Substances 0.000 claims description 14
- 230000015556 catabolic process Effects 0.000 claims description 10
- 238000006731 degradation reaction Methods 0.000 claims description 10
- 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 description 10
- 229940043267 rhodamine b Drugs 0.000 claims description 10
- 238000007144 microwave assisted synthesis reaction Methods 0.000 claims description 8
- 230000015572 biosynthetic process Effects 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000003786 synthesis reaction Methods 0.000 claims description 7
- 238000005286 illumination Methods 0.000 claims description 6
- 239000010865 sewage Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 238000006555 catalytic reaction Methods 0.000 claims description 3
- 230000002349 favourable effect Effects 0.000 claims description 2
- 229910052738 indium Inorganic materials 0.000 abstract description 28
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 abstract description 27
- 230000001699 photocatalysis Effects 0.000 abstract description 11
- 239000004065 semiconductor Substances 0.000 abstract description 8
- 238000007146 photocatalysis Methods 0.000 abstract description 5
- 239000002131 composite material Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 abstract 1
- 238000001308 synthesis method Methods 0.000 abstract 1
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 5
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000975 dye Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- -1 CdS compound Chemical class 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229910002367 SrTiO Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/847—Vanadium, niobium or tantalum or polonium
- B01J23/8472—Vanadium
-
- 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
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention relates to the technical field of semiconductor photocatalysis, in particular to a preparation method and application of an InVO4-CdS heterojunction photocatalyst. According to the method, a visible-light response indium vanadate and cadmium sulfide composite photocatalyst material is obtained by taking cadmium acetate, thiourea, indium nitrate and ammonium metavanadate as raw materials through a microwave synthesis method and a hydrothermal method.
Description
Technical field
The present invention relates to Photocatalitic Technique of Semiconductor field, refer in particular to a kind of InVO
4the preparation method of/CdS heterojunction photocatalyst and purposes, utilize microwave process for synthesizing and hydro-thermal method two step to synthesize vanadic acid indium and cadmium sulfide heterojunction photocatalyst, rhdamine B of degrading under can be used for visible ray.
Background technology
In recent years, development and utilization is green, free of contamination solar energy is for solving the environmental pollution that day by day increases and energy crisis is study hotspot always, and Photocatalitic Technique of Semiconductor can farthest utilize solar energy to realize sewage purification, energy conversion, Photocatalitic Technique of Semiconductor is that the electron-hole pair with higher oxygen reducing power utilizing semiconductor light-catalyst material to produce under light illumination realizes removing the degraded of organic pollution, this technology is because of thorough to organic pollutant degradation, energy-conservation, efficiently, the advantages such as secondary pollution is little are developed rapidly, at present, study more semiconductor light-catalyst, as: TiO
2, SrTiO
3the photocatalyst material that isoreactivity is higher can only respond the ultraviolet light only accounting for incident sunshine total amount 5%, greatly limit the utilization of solar energy, and therefore, the efficient visible light catalyst of development of new is the focus of current photocatalysis technology research.
Vanadic acid indium (InVO
4) be the semiconductor light-catalyst that a kind of novel visible responds, band gap width is at about 2.0eV, can by excited by visible light, its conduction band (CB) and valence band (VB) produce the electron-hole pair with higher oxygen reducing power respectively, realize the effective degraded to organic pollution, at present, InVO
4mostly by the synthesis of hydro-thermal method, sol-gel process and high-temperature solid phase calcination method, the particle size of acquisition is comparatively large, pattern irregularity, makes InVO
4photocatalytic activity not high, therefore, we utilize Microwave-assisted synthesis method to synthesize particle diameter is less, the InVO of regular appearance
4nano particle.
Cadmium sulfide (CdS) is a kind of important metal sulfide, band gap width is 2.4eV, can be good at responding to visible light, but single CdS is not high to the degradation effect of pollutant, the electron-hole pair produced under being mainly illumination very easily compound, at present, utilize different semi-conducting material and CdS compound, construct hetero-junctions, effectively can promote the separation of interface electron-hole pair, reach the object improving photocatalytic activity, such as: CdS/WO
3, CdS/Bi
2moO
6and CdS/BiPO
4the photocatalytic activity of CdS can be significantly improved Deng heterojunction photocatalyst, but so far, also do not find to utilize hydro-thermal method to prepare InVO
4the report of/CdS heterojunction photocatalyst and photocatalytic applications thereof.
Summary of the invention
The object of the present invention is to provide a kind of novel I nVO
4the preparation method of/CdS heterojunction photocatalyst material, the method is with cadmium acetate, and thiocarbamide, indium nitrate and ammonium metavanadate are raw material, utilize microwave process for synthesizing, hydro-thermal method, the vanadic acid indium responded under obtaining visible ray and cadmium sulfide photocatalysis composite.
A kind of visible light-responded InVO provided by the invention
4the preparation method of/CdS heterojunction photocatalyst material, is characterized in that comprising the following steps:
Step:
(1) vanadic acid indium is prepared: take indium nitrate and ammonium metavanadate is dissolved in pure water, heating for dissolving obtains yellow presoma suspension, be transferred to afterwards in there-necked flask, react in microwave reactor, obtain vanadic acid In nanoparticles finally by washing, filtration, drying.
Described indium nitrate is 1:1 with the amount of substance ratio of ammonium metavanadate, and microwave reaction is 800W, 100 DEG C, 5h.
The average grain diameter of the vanadic acid indium A that described preparation draws is 20nm, and pattern is spherical nano particle, and favorable dispersibility is shown in accompanying drawing 3.
By the InVO that Microwave-assisted synthesis method is synthesized
4nano particle diameter is less, regular appearance, InVO
4nano particle is extremely important in the invention process, and Main Function is by carrying out hydro-thermal compound with cadmium sulfide, constructing heterojunction boundary closely, accelerates the right separation of photo-generate electron-hole with this, and then improves the photocatalytic activity of composite.
(2) prepare cadmium sulfide: take cadmium acetate and thiocarbamide is dissolved in pure water, ultrasonic disperse obtains clear solution, is transferred to afterwards in hydrothermal reaction kettle, reacts in baking oven, finally by washing, filter, drying obtains cadmium sulfide B.
Described cadmium acetate is 1:2 with the amount of substance ratio of thiocarbamide, and hydro-thermal reaction is 160 DEG C, 24h.
(3) vanadic acid indium and cadmium sulfide heterojunction photocatalyst is prepared: take the InVO that Microwave-assisted synthesis method is synthesized
4nano particle, cadmium acetate and thiocarbamide are dissolved in pure water, and ultrasonic disperse obtains faint yellow presoma suspension, is transferred to afterwards in water heating kettle, reacts in baking oven, obtain vanadic acid indium and cadmium sulfide heterojunction material C finally by washing, filtration, drying.
Described InVO
4the mass ratio of nano particle and cadmium sulfide is 10-60:100, and the amount of substance of cadmium acetate and thiocarbamide is than being 1:2, and hydrothermal reaction condition is 160 DEG C, 24h.
InVO in the present invention
4the crystal structure of/CdS heterojunction photocatalyst is determined by powder x-ray diffraction (XRD), as shown in Figure 1, obviously can observe the characteristic peak of CdS in XRD, corresponding with standard card 77-2306; In addition, along with InVO
4compound quantity increase, also observe its diffraction maximum and diffraction peak intensity significantly increases thereupon, meet with standard card 48-0898; XRD spectra shows InVO
4/ CdS heterojunction photocatalyst is successfully prepared by microwave process for synthesizing and hydro-thermal method.
InVO
4the surface chemistry composition of/CdS heterojunction photocatalyst and element valence are determined by x-ray photoelectron spectroscopy (XPS), as shown in Figure 2, have occurred Cd in xps energy spectrum figure, the characteristic peak of S, In, V and O, this spectrogram shows, by the InVO prepared by microwave process for synthesizing and hydro-thermal method
4/ CdS heterojunction photocatalyst contains its all elements had.
In addition, in the present invention by InVO that Microwave-assisted synthesis method and conventional hydrothermal method are synthesized
4pattern and microstructure determined by transmission electron microscope (TEM) and SEM (SEM), as shown in Figure 3, the InVO of Microwave-assisted synthesis method synthesis
4pattern is spherical particle, and average grain diameter is at 20nm, and the InVO of conventional hydrothermal method synthesis
4pattern is also spherical, but average grain diameter is at 3-5 μm.
Another object of the present invention: one, preparation InVO is provided
4the test method of/CdS heterojunction photocatalyst material; Two, by InVO
4/ CdS is used for photocatalytically degradating organic dye sewage under visible ray as catalysis material.
Beneficial effect
Utilize the InVO prepared by microwave process for synthesizing and hydro-thermal method
4/ CdS heterojunction photocatalyst material, rhodamine B degradation dyestuff demonstrates excellent photocatalytic activity under visible light; Present invention process is simple to operate, with low cost, and the reaction time is shorter, can effective photocatalytically degradating organic dye, reaches the object of protection of the environment.
Accompanying drawing explanation
The x-ray diffraction pattern (XRD) of Fig. 1 sample prepared by embodiment of the present invention 1-4, InVO in figure
4/ CdS heterojunction photocatalyst demonstrates InVO respectively
4with the characteristic peak of CdS composition.
The InVO of Fig. 2 prepared by the embodiment of the present invention 3
4the x-ray photoelectron spectroscopy figure (XPS) of/CdS heterojunction photocatalyst: element composes (a) entirely, Cd3d5 (b), S2p (c), In3d (d), V2p (e) and O1s (f), describe XPS spectrum figure and show it and possessed all elements of synthesized sample.
Fig. 3 is in embodiment of the present invention 1-4 and comparative example 5, the InVO that the different-grain diameter synthesized by Microwave-assisted synthesis method and conventional hydrothermal method is distributed
4transmission electron microscope (TEM) figure and SEM (SEM) comparison diagram.
The design sketch of Fig. 4 sample photocatalytic degradation rhodamine B under visible light conditions prepared by embodiment of the present invention 1-4.Pure CdS and InVO can be found out in figure
4the degradation rate of rhodamine B is very low under visible light, and InVO
4the degradation rate of/CdS heterojunction photocatalyst is then very high, describes the InVO of synthesis
4/ CdS heterojunction photocatalyst significantly can promote photocatalysis performance, and well can be applied to the degraded of rhodamine B sewage.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in detail, and to make those skilled in the art understand the present invention better, but the present invention is not limited to following examples.
Embodiment 1
Step (1): take 1mmol indium nitrate (0.382g) and 1mmol ammonium metavanadate (0.117g) is dissolved in 100mL pure water, heating for dissolving obtains yellow presoma suspension, be transferred to afterwards in the there-necked flask of 250mL, microwave reaction 800W, 100 DEG C, 5h, obtains vanadic acid indium A finally by washing, filtration, drying.Step (2): take 1mmol cadmium acetate (0.266g) and 2mmol thiocarbamide (0.076g) is dissolved in 40mL pure water, ultrasonic disperse obtains clear solution, be transferred to afterwards in the water heating kettle of 50mL, hydro-thermal reaction 160 DEG C, 24h, obtains cadmium sulfide B finally by washing, filtration, drying.
Step (3): take 0.015g vanadic acid indium A, 1mmol cadmium acetate (0.266g) and 2mmol thiocarbamide (0.076g) are dissolved in 40mL pure water, ultrasonic disperse obtains faint yellow presoma suspension, be transferred to afterwards in the water heating kettle of 50mL, hydro-thermal reaction 160 DEG C, 24h, obtains vanadic acid indium and cadmium sulfide heterojunction material C finally by washing, filtration, drying.
Embodiment 2
Step (1): take 1mmol indium nitrate (0.382g) and 1mmol ammonium metavanadate (0.117g) is dissolved in 100mL pure water, heating for dissolving obtains yellow presoma suspension, be transferred to afterwards in there-necked flask, microwave reaction 800W, 100 DEG C, 5h, obtains vanadic acid indium A finally by washing, filtration, drying.
Step (2): take 1mmol cadmium acetate (0.266g) and 2mmol thiocarbamide (0.076g) is dissolved in 40mL pure water, ultrasonic disperse obtains clear solution, be transferred to afterwards in the water heating kettle of 50mL, hydro-thermal reaction 160 DEG C, 24h, obtains cadmium sulfide B finally by washing, filtration, drying.
Step (3): take 0.030g vanadic acid indium A, 1mmol cadmium acetate (0.266g) and 2mmol thiocarbamide (0.076g) are dissolved in 40mL pure water, ultrasonic disperse obtains faint yellow presoma suspension, be transferred to afterwards in the water heating kettle of 50mL, hydro-thermal reaction 160 DEG C, 24h, obtains vanadic acid indium and cadmium sulfide heterojunction material C finally by washing, filtration, drying.
Embodiment 3
Step (1): take in 1mmol indium nitrate (0.382g) and 1mmol ammonium metavanadate (0.117g) 100mL pure water, heating for dissolving obtains yellow presoma suspension, be transferred to afterwards in there-necked flask, microwave reaction 800W, 100 DEG C, 5h, obtains vanadic acid indium A finally by washing, filtration, drying.
Step (2): take 1mmol cadmium acetate (0.266g) and 2mmol thiocarbamide (0.076g) is dissolved in 40mL pure water, ultrasonic disperse obtains clear solution, be transferred to afterwards in the water heating kettle of 50mL, hydro-thermal reaction 160 DEG C, 24h, obtains cadmium sulfide B finally by washing, filtration, drying.
Step (3): take 0.060g vanadic acid indium A, 1mmol cadmium acetate (0.266g) and 2mmol thiocarbamide (0.076g) are dissolved in 40mL pure water, ultrasonic disperse obtains faint yellow presoma suspension, be transferred to afterwards in the water heating kettle of 50mL, hydro-thermal reaction 160 DEG C, 24h, obtains vanadic acid indium and cadmium sulfide heterojunction material C finally by washing, filtration, drying.
Embodiment 4
Step (1): take 1mmol indium nitrate (0.382g) and 1mmol ammonium metavanadate (0.117g) is dissolved in 100mL pure water, heating for dissolving obtains yellow presoma suspension, be transferred to afterwards in there-necked flask, microwave reaction 800W, 100 DEG C, 5h, obtains vanadic acid indium A finally by washing, filtration, drying.
Step (2): take 1mmol cadmium acetate (0.266g) and 2mmol thiocarbamide (0.076g) is dissolved in 40mL pure water, ultrasonic disperse obtains clear solution, be transferred to afterwards in the water heating kettle of 50mL, hydro-thermal reaction 160 DEG C, 24h, obtains cadmium sulfide B finally by washing, filtration, drying.
Step (3): take 0.090g vanadic acid indium A, 1mmol cadmium acetate (0.266g) and 2mmol thiocarbamide (0.076g) are dissolved in 40mL pure water, ultrasonic disperse obtains faint yellow presoma suspension, be transferred to afterwards in the water heating kettle of 50mL, hydro-thermal reaction 160 DEG C, 24h, obtains vanadic acid indium and cadmium sulfide heterojunction material C finally by washing, filtration, drying.
Comparative example 5
Step (1): take 1mmol indium nitrate (0.382g) and 1mmol ammonium metavanadate (0.117g) is dissolved in 40mL pure water, heating for dissolving obtains yellow presoma suspension, be transferred to afterwards in the water heating kettle of 50mL, hydro-thermal reaction 140 DEG C, 12h, obtain vanadic acid indium A finally by washing, filtration, drying, the particle diameter of vanadic acid indium A is 3-5 μm, pattern is spherical, sees accompanying drawing 3.
Step (2): take 1mmol cadmium acetate (0.266g) and 2mmol thiocarbamide (0.076g) is dissolved in 40mL pure water, ultrasonic disperse obtains clear solution, be transferred to afterwards in the water heating kettle of 50mL, hydro-thermal reaction 160 DEG C, 24h, obtains cadmium sulfide B finally by washing, filtration, drying.
Step (3): take 0.060g vanadic acid indium A, 1mmol cadmium acetate (0.266g) and 2mmol thiocarbamide (0.076g) are dissolved in 40mL pure water, ultrasonic disperse obtains faint yellow presoma suspension, be transferred to afterwards in the water heating kettle of 50mL, hydro-thermal reaction 160 DEG C, 24h, obtains vanadic acid indium and cadmium sulfide heterojunction material C finally by washing, filtration, drying.
Added the mass ratio of different vanadic acid indium and cadmium sulfide by regulation and control, prepare InVO through microwave process for synthesizing and hydro-thermal method
4/ CdS heterojunction photocatalyst composite, investigate them respectively with same catalyst amount (50mg) condition, under visible light illumination to the degradation effect of rhodamine B solution (10mg/L), photocatalysis result shows the InVO that a small amount of vanadic acid indium and cadmium sulfide compound are prepared
4/ CdS heterojunction photocatalyst significantly can promote photocatalytic activity.In addition, show best catalytic performance with the heterojunction photocatalyst of 40wt% vanadic acid indium synthesis, under 40min illumination, rhodamine B degradation rate can reach 93.1%, describes prepared InVO
4/ CdS heterojunction photocatalyst can be applied to the improvement of rhodamine B sewage.
Meanwhile, comparative example 5 has synthesized 40wt%InVO by conventional hydrothermal method
4/ CdS heterojunction photocatalyst, and with the 40wt%InVO of microwave assisting method and water heat transfer
4/ CdS heterojunction photocatalyst has carried out the rhodamine B degradation experiment under the same terms, and result shows, under 40min illumination, and the InVO of conventional hydrothermal method synthesis
4/ CdS heterojunction photocatalyst only has 43.6% to rhodamine B degradation rate, sees accompanying drawing 4, therefore, by the InVO of microwave assisting method and water heat transfer
4/ CdS heterojunction photocatalyst has higher visible light catalysis activity, has remarkable result to waste water control.
Claims (8)
1. a preparation method for heterojunction photocatalyst, is characterized in that: the InVO taking the synthesis of Microwave-assisted synthesis method
4nano particle, cadmium acetate and thiocarbamide are dissolved in pure water, and ultrasonic disperse obtains faint yellow presoma suspension, is transferred to afterwards in water heating kettle, reacts in baking oven, obtain InVO finally by washing, filtration, drying
4/ CdS heterojunction photocatalyst.
2. the preparation method of a kind of heterojunction photocatalyst as claimed in claim 1, is characterized in that: described InVO
4the mass ratio of nano particle and cadmium sulfide is 10-60:100.
3. the preparation method of a kind of heterojunction photocatalyst as claimed in claim 2, is characterized in that: described InVO
4the mass ratio of nano particle and cadmium sulfide is the InVO of 40:100, preparation
4/ CdS heterojunction photocatalyst, under 40min illumination, rhodamine B degradation rate can reach 93.1%.
4. the preparation method of a kind of heterojunction photocatalyst as claimed in claim 1, is characterized in that: the amount of substance of cadmium acetate and thiocarbamide is than being 1:2, and hydrothermal reaction condition is 160 DEG C, 24h.
5. the preparation method of a kind of heterojunction photocatalyst as claimed in claim 1, is characterized in that the InVO that described Microwave-assisted synthesis method is synthesized
4the preparation method of nano particle is as follows: take indium nitrate and ammonium metavanadate is dissolved in pure water, heating for dissolving obtains yellow presoma suspension, be transferred to afterwards in there-necked flask, react in microwave reactor, obtain vanadic acid In nanoparticles finally by washing, filtration, drying.
6. the preparation method of a kind of heterojunction photocatalyst as claimed in claim 5, is characterized in that: described indium nitrate is 1:1 with the amount of substance ratio of ammonium metavanadate, and microwave reaction is 800W, 100 DEG C, 5h.
7. the preparation method of a kind of heterojunction photocatalyst as claimed in claim 1, is characterized in that: described InVO
4the average grain diameter of nano particle is 20nm, and pattern is spherical nano particle, favorable dispersibility.
8. the InVO for preparing of preparation method as claimed in claim 1
4/ CdS heterojunction photocatalyst is used for photocatalytically degradating organic dye sewage under visible light as catalysis material.
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| CN107224986A (en) * | 2017-07-21 | 2017-10-03 | 江苏大学 | A kind of molybdenum disulfide/niobic acid tin composite nano materials and purposes |
| CN108855140A (en) * | 2018-07-18 | 2018-11-23 | 四川大学 | A kind of CuS/Bi2WO6Heterojunction photocatalyst and its preparation method and application |
| CN110575837A (en) * | 2019-08-15 | 2019-12-17 | 长安大学 | InVO4/ZnIn2S4Photocatalyst, preparation method and application |
| CN112495411A (en) * | 2020-09-09 | 2021-03-16 | 同济大学 | Carbon nitride nanosheet loaded indium vanadate quantum dot photocatalyst and preparation and application thereof |
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| CN106340661A (en) * | 2016-09-26 | 2017-01-18 | 大连理工大学 | Fuel cell system of ternary heterojunction photoelectrocatalysis membrane |
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| CN110575837B (en) * | 2019-08-15 | 2022-04-08 | 长安大学 | InVO4/ZnIn2S4Photocatalyst, preparation method and application |
| CN112495411A (en) * | 2020-09-09 | 2021-03-16 | 同济大学 | Carbon nitride nanosheet loaded indium vanadate quantum dot photocatalyst and preparation and application thereof |
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