CN107970951A - A kind of preparation method of flower-shaped meso-hole structure CdS-ZnO composite materials - Google Patents
A kind of preparation method of flower-shaped meso-hole structure CdS-ZnO composite materials Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000000725 suspension Substances 0.000 claims abstract description 27
- 239000004246 zinc acetate Substances 0.000 claims abstract description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004202 carbamide Substances 0.000 claims abstract description 10
- 238000005119 centrifugation Methods 0.000 claims abstract description 9
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000010992 reflux Methods 0.000 claims abstract description 7
- CKLJMWTZIZZHCS-REOHCLBHSA-N L-aspartic acid Chemical compound OC(=O)[C@@H](N)CC(O)=O CKLJMWTZIZZHCS-REOHCLBHSA-N 0.000 claims abstract description 6
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 claims abstract description 6
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 5
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical group NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000003763 carbonization Methods 0.000 claims abstract 3
- 229910052980 cadmium sulfide Inorganic materials 0.000 claims description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 235000019441 ethanol Nutrition 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 9
- 239000000047 product Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- CKLJMWTZIZZHCS-UHFFFAOYSA-N D-OH-Asp Natural products OC(=O)C(N)CC(O)=O CKLJMWTZIZZHCS-UHFFFAOYSA-N 0.000 claims description 5
- CKLJMWTZIZZHCS-UWTATZPHSA-N L-Aspartic acid Natural products OC(=O)[C@H](N)CC(O)=O CKLJMWTZIZZHCS-UWTATZPHSA-N 0.000 claims description 5
- 229960005261 aspartic acid Drugs 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 3
- 239000013049 sediment Substances 0.000 claims description 3
- DWNBOPVKNPVNQG-LURJTMIESA-N (2s)-4-hydroxy-2-(propylamino)butanoic acid Chemical compound CCCN[C@H](C(O)=O)CCO DWNBOPVKNPVNQG-LURJTMIESA-N 0.000 claims description 2
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 239000012153 distilled water Substances 0.000 claims 2
- 239000013067 intermediate product Substances 0.000 claims 1
- 238000010025 steaming Methods 0.000 claims 1
- 238000001291 vacuum drying Methods 0.000 claims 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 abstract description 60
- 239000011787 zinc oxide Substances 0.000 abstract description 47
- 230000001699 photocatalysis Effects 0.000 abstract description 14
- 238000007146 photocatalysis Methods 0.000 abstract description 12
- 239000004065 semiconductor Substances 0.000 abstract description 8
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- 239000003795 chemical substances by application Substances 0.000 abstract description 5
- 238000009830 intercalation Methods 0.000 abstract description 2
- 230000002687 intercalation Effects 0.000 abstract description 2
- 230000009257 reactivity Effects 0.000 abstract description 2
- LIAVVEHHDCBKEB-UHFFFAOYSA-L zinc urea diacetate Chemical compound NC(=O)N.C(C)(=O)[O-].[Zn+2].C(C)(=O)[O-] LIAVVEHHDCBKEB-UHFFFAOYSA-L 0.000 abstract 2
- 235000003704 aspartic acid Nutrition 0.000 abstract 1
- OQFSQFPPLPISGP-UHFFFAOYSA-N beta-carboxyaspartic acid Natural products OC(=O)C(N)C(C(O)=O)C(O)=O OQFSQFPPLPISGP-UHFFFAOYSA-N 0.000 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 235000013904 zinc acetate Nutrition 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 6
- 238000004821 distillation Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 230000009102 absorption Effects 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- DJWUNCQRNNEAKC-UHFFFAOYSA-L zinc acetate Chemical class [Zn+2].CC([O-])=O.CC([O-])=O DJWUNCQRNNEAKC-UHFFFAOYSA-L 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
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- 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
-
- B01J35/39—
-
- B01J35/60—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
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- 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
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- 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
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- 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
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- 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
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- 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
- C02F2101/34—Organic compounds containing oxygen
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- 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
- C02F2101/38—Organic compounds containing nitrogen
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- 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
Abstract
The present invention provides a kind of flower-shaped meso-hole structure CdS ZnO, it is that green template agent is first used as using aspartic acid, thiocarbamide forms urea zinc acetate suspension by ultrasonic disperse by a flower-shaped CdS of step Hydrothermal Synthesiss, then by urea and zinc acetate with cadmium acetate in ethanol water mixed liquid；Then CdS suspension will be obtained in absolute ethyl alcohol by CdS ultrasonic disperses, then CdS suspension will be placed in oil bath, and add urea zinc acetate suspension; continue oil bath 6 ~ 7h of reflux, product centrifugation, washing; dry, then calcining carbonization under nitrogen protection, obtains flower-shaped mesoporous CdS ZnO composite materials.Film like structures are presented in zinc oxide in the composite material, and intercalation between flower-shaped CdS semiconductors branch, effectively increases the reactivity site of composite material well.Simultaneously because the introducing of zinc oxide, effectively increases the visible absorption efficiency of CdS, thus the photocatalysis performance of composite material can be effectively improved.
Description
Technical field
The present invention relates to a kind of preparation method of flower-shaped meso-hole structure CdS-ZnO composite materials, it is mainly used for organic contamination
The photocatalytic degradation of thing, belongs to composite material and prepares and photocatalytic applications field.
Background technology
With industrial expansion, water pollution has seriously affected the life and health of the mankind and other biological.Tradition
Administer sewage method in cost and effect there are it is certain the defects of.In recent years, photocatalysis organic pollutant degradation skill
Art due to its green, low energy consumption, it is efficient the features such as be widely studied in terms of water process.Semiconductor light-catalyst is therefore extensive
Exploitation, wherein CdS have proved to be a kind of excellent visible light-responded due to its relatively narrow bandwidth, excellent visible light activity
Photochemical catalyst.But single CdS has obvious photoetch phenomenon, therefore the lifting to CdS photocatalysis efficiency is applied to have
It is very helpful.Related experiment is the results show that the pattern of semiconductor light-catalyst has large effect to its catalytic activity.Separately
The outer heterojunction structure with bigger serface that forms CdS and other semiconductors couplings can also effectively adjust semiconductor band gap
With spectral absorption scope, and then lifted catalyst photocatalytic activity.
The content of the invention
The object of the present invention is to provide a kind of preparation method with flower-shaped meso-hole structure CdS-ZnO composite materials.
First, the preparation of flower-shaped meso-hole structure CdS-ZnO composite materials
The present invention prepares the method with flower-shaped meso-hole structure CdS-ZnO, comprises the following steps that：
（1）The preparation of three-dimensional flower-shaped CdS
Cadmium acetate and thiocarbamide are pressed 1:2~1:3 molar ratio is dissolved in deionized water, adds L-Aspartic acid solution, is continued
Stir 20 ~ 30min and form uniform solution, then react 4 ~ 6h in 180 ± 5 DEG C；Sediment is washed by centrifugation, ethanol and distillation
Wash, it is dry, obtain three-dimensional flower-shaped CdS.
The addition of L-Aspartic acid prevents CdS from reuniting as structure directing agent, the mole and cadmium acetate of L-Aspartic acid
Mole ratio is 1:2~1:3.
（2）The preparation of flower-shaped mesoporous CdS-ZnO
By urea and zinc acetate by ultrasonic disperse with forming homogeneous suspension in ethanol-water mixture；Will dry flower-shaped CdS ultrasounds
It is scattered in absolute ethyl alcohol and obtains yellow suspension, then suspension is placed in oil bath, above-mentioned urea and second is added in 80 ~ 90 DEG C
The suspension of sour zinc, continues 80 ~ 90 DEG C of oil baths 6 ~ 7h of reflux of holding, product centrifugation, ethanol and distillation water washing, is dried in vacuo,
Then 1.5 ~ 2h is calcined in 200 ~ 300 DEG C under nitrogen protection, obtains flower-shaped mesoporous CdS-ZnO.
In the mixed liquor of alcohol-water, the volume ratio of ethanol and water is 1:1~1:1.5.
The mole of cadmium sulfide and zinc acetate is controlled 1:0.5~1:Between 1.5；Urea and zinc acetate molar ratio are 1.5:1
~2:1.In CdS-ZnO composite materials, the molar ratio of CdS and ZnO are 1:1~1:2.
Preferably to form heterojunction structure and increase composite material specific surface area between two kinds of semiconductors, by sheet
ZnO is dispersed between CdS, and the dispersion liquid substep that urea is formed with zinc acetate is added in flower-shaped CdS suspension, and is first added
Enter half, stir 50 ~ 60min, add remaining dispersion liquid, continue 5 ~ 6h of stirring and keep 5 ~ 6h of oil bath reflux；Product centrifuges,
Washing, dry, calcining, obtains flower-shaped mesoporous CdS-ZnO.
Drying in above steps is dried in vacuo at 50 ~ 60 DEG C.
2nd, the structure of flower-shaped mesoporous CdS-ZnO composite materials
Fig. 1 is the flower-shaped CdS for adding green template agent synthesis.Understand, CdS semiconductor structure is in regular floriform appearance.Fig. 2 is
Flower-shaped mesoporous CdS-ZnO composite materials scanning electron microscope (SEM) photograph prepared by the present invention.From fig. 2 it can be seen that structure directing agent L- days
The introducing of winter propylhomoserin effectively controls the irregular agglomeration of CdS；Zinc oxide is presented in flower-shaped mesoporous CdS-ZnO composite materials
Film like structures, and intercalation between flower-shaped CdS semiconductors branch, effectively increases the reaction active site of composite material well
Point.
Fig. 3 is the UV absorption figure of CdS and CdS-ZnO.It can be seen in figure 3 that the introducing of zinc oxide, effectively improves
The visible absorption efficiency of CdS, thus the photocatalysis performance of composite material can be effectively improved.
3rd, the photocatalysis performance of flower-shaped mesoporous CdS-ZnO composite materials
Fig. 4 is the photocatalysis efficiency of CdS and CdS-ZnO.It can be seen in fig. 4 that the photo-catalysis capability of flower-shaped CdS is better than list
One CdS.It is higher since the heterojunction structure of formation enhances the photoelectron transfer speed of composite material after zinc oxide is introduced
Specific surface area also effectively increases reactivity site.Therefore flower-shaped mesoporous CdS-ZnO shows excellent photocatalysis efficiency.
CdS and CdS-ZnO photocatalysis organic matter degradation is tested：It is accurate to prepare 10 mgL-1RhB solution, pipette 50
ML RhB solution is in quartz reactor, and then to 50 mg photochemical catalysts are added, 1 h of magnetic agitation, makes under dark condition
RhB molecules reach adsorption-desorption balance in catalyst surface and solution；Then the simulated visible light source of 200W is opened, cold
But temperature of reaction system is made to maintain 25 DEG C or so under water cycling condition.Taken in the process of photocatalysis experiment every same time
The sample of about 4 mL centrifuges supernatant in centrifuge tube, is existed with UV-2550 types visible spectrophotometer measure centrifugate
λmaxAbsorbance at=554 nm, and according to the change of the concentration of RhB and initial concentration in clear liquid after reaction, calculate photocatalysis
Agent is as follows to the removal rate of RhB, the calculation formula of use：
In formula, η % be RhB removal rate, C0For the initial concentration of RhB；C is the concentration of RhB after light-catalyzed reaction.
Test result：After illumination 25min, single CdS is 55 ~ 60% for the removal rate of RhB；CdS-ZnO removes RhB
Except rate is 80 ~ 90%.
Brief description of the drawings
Fig. 1 is the three-dimensional flower-shaped CdS prepared dried scanning electron microscope (SEM) photographs at 60 DEG C of the invention.
Scanning electron microscope (SEM) photographs of the Fig. 2 for the three-dimensional flower-shaped CdS-ZnO of the invention prepared at 60 DEG C after dry and heat treatment.
Fig. 3 is three-dimensional flower-shaped CdS and CdS-ZnO UV absorptions spectrogram prepared by the present invention.
Fig. 4 is the single CdS of the invention prepared, flower-shaped CdS, 1:0.5、1:1、1:1.5 ZnO doping amounts it is flower-shaped mesoporous
CdS-ZnO photocatalysis comparison diagrams.
Embodiment
It is described further below by the preparation of instantiation meso-hole structure CdS-ZnO flower-shaped to the present invention, performance etc..
Embodiment 1
（1）The preparation of three-dimensional flower-shaped CdS
1mmoL cadmium acetates and 3mmoL thiocarbamides are added in 50mL deionized waters and stirred to dissolve, is slowly added in the process
The L-Aspartic acid solution 20mL of the good 0.01mmoL/mL of configured in advance, continues to stir 30min formation uniform solutions, then will
Uniform solution is transferred in 100 mL reaction kettles, and 180 DEG C of reaction 4h, sediment passes through centrifugation, ethanol and distillation water washing number
Secondary, product obtains three-dimensional flower-shaped CdS in 60 DEG C of dry 12h of drying box.
（2）The preparation of flower-shaped meso-hole structure CdS-ZnO composite materials
By 2mmol urea and 1mmol zinc acetates in 10ml ethanol-water mixtures（7ml ethanol and 3ml water）Ultrasonic disperse is formed
Homogeneous urea-zinc acetate suspension；
The 1mmol flower-shaped CdS ultrasonic disperses dried are obtained into yellow suspension in absolute ethyl alcohol, are placed in returning in 80 DEG C of oil baths
Stream, while above-mentioned urea-zinc acetate suspension half is added dropwise in oil bath system, after stirring 60min, it is slowly added dropwise another
Half urea-zinc acetate suspension, continues to keep 80 DEG C of oil bath reflux 5h, product centrifugation, ethanol is done with distillation water washing, drying box
Dry 12h, continues 200 DEG C of calcining 2h in the case where tube furnace nitrogen is protected and obtains flower-shaped mesoporous CdS-ZnO composite materials.In CdS-ZnO
The mole ratio of CdS- and ZnO is 1:1, CdS-ZnO is 61.5% to the removal rate of RhB.
Embodiment 2
（1）The preparation of three-dimensional flower-shaped CdS：With embodiment 1.
（2）The preparation of flower-shaped meso-hole structure CdS-ZnO composite materials
By 3mmol urea and 1.5mmol zinc acetates in 10ml ethanol-water mixtures（7ml ethanol and 3ml water）Ultrasonic disperse shape
Into homogeneous urea-zinc acetate suspension；
The 1mmol flower-shaped CdS ultrasonic disperses dried are obtained into yellow suspension in absolute ethyl alcohol, are placed in returning in 80 DEG C of oil baths
Stream, while above-mentioned urea-zinc acetate suspension half is added dropwise in oil bath system, after stirring 60min, it is slowly added dropwise another
Half urea-zinc acetate suspension, continues to keep 80 DEG C of oil bath reflux 5h, product centrifugation, ethanol is done with distillation water washing, drying box
Dry 12h, continues 200 DEG C of calcining 2h in the case where tube furnace nitrogen is protected and obtains flower-shaped mesoporous CdS-ZnO composite materials.In CdS-ZnO
The mole ratio of CdS- and ZnO is 1:1.5, CdS-ZnO be 81.3% to the removal rate of RhB.
Embodiment 3
（1）The preparation of three-dimensional flower-shaped CdS：With embodiment 1.
（2）The preparation of flower-shaped meso-hole structure CdS-ZnO composite materials
By 4mmol urea and 2mmol zinc acetates in 10ml ethanol-water mixtures（7ml ethanol and 3ml water）Ultrasonic disperse is formed
Homogeneous urea-zinc acetate suspension；
The 1mmol flower-shaped CdS ultrasonic disperses dried are obtained into yellow suspension in absolute ethyl alcohol, are placed in returning in 80 DEG C of oil baths
Stream, while above-mentioned urea-zinc acetate suspension half is added dropwise in oil bath system, after stirring 60min, it is slowly added dropwise another
Half urea-zinc acetate suspension, continues to keep 80 DEG C of oil bath reflux 5h, product centrifugation, ethanol is done with distillation water washing, drying box
Dry 12h, continues 200 DEG C of calcining 2h in the case where tube furnace nitrogen is protected and obtains flower-shaped mesoporous CdS-ZnO composite materials.In CdS-ZnO
The mole ratio of CdS- and ZnO is 1:2, CdS-ZnO be 76.2% to the removal rate of RhB.
Claims (8)
1. a kind of preparation method of flower-shaped meso-hole structure CdS-ZnO composite materials, comprises the following steps that：
The preparation of three-dimensional flower-shaped CdS
Cadmium acetate and thiocarbamide are pressed 1:2 ~1:3 molar ratio is dissolved in deionized water, adds L-Aspartic acid solution, after
20 ~ 30min of continuous stirring forms uniform solution, then reacts 4 ~ 6h in 180 ± 5 DEG C；Sediment passes through centrifugation, ethanol and distilled water
Washing, it is dry, obtain three-dimensional flower-shaped CdS；
（2）The preparation of flower-shaped mesoporous CdS-ZnO
By urea and zinc acetate by ultrasonic disperse with forming homogeneous urea-zinc acetate suspension in ethanol-water mixture；Will be dry
Dry flower-shaped CdS ultrasonic disperses obtain yellow CdS suspension in absolute ethyl alcohol, then CdS suspension is placed in oil bath, in 80 ~
90 DEG C add above-mentioned urea-zinc acetate-suspension, continue 80 ~ 90 DEG C of oil baths 6 ~ 7h of reflux of holding, product centrifugation, ethanol is with steaming
Distilled water is washed, vacuum drying, and then calcining carbonization under nitrogen protection, obtains flower-shaped mesoporous CdS-ZnO.
2. the preparation method of flower-shaped meso-hole structure CdS-ZnO composite materials as claimed in claim 1, it is characterised in that：Step（2）
In, urea-zinc acetate suspension substep is added in CdS suspension：Half is first added, 50 ~ 60min is stirred, adds residue
Urea-zinc acetate dispersion liquid, continue to stir 80 ~ 90 DEG C of oil baths of holding and flow back 5 ~ 6h.
3. the preparation method of flower-shaped meso-hole structure CdS-ZnO composite materials as claimed in claim 1 or 2, it is characterised in that：L- days
The mole of winter propylhomoserin is 1 with cadmium acetate mole ratio:2~1:3.
4. the preparation method of flower-shaped meso-hole structure CdS-ZnO composite materials as claimed in claim 1 or 2, it is characterised in that：Step
（2）Alcohol-water mixed liquor in, the volume ratio of ethanol and water is 1:1~1:1.5.
5. the preparation method of flower-shaped meso-hole structure CdS-ZnO composite materials as claimed in claim 1 or 2, it is characterised in that：Step
（2）In, the mole of cadmium sulfide and zinc acetate is controlled 1:0.5~1:Between 1.5.
6. the preparation method of flower-shaped meso-hole structure CdS-ZnO composite materials as claimed in claim 1 or 2, it is characterised in that：Step
（2）In, urea and zinc acetate molar ratio are 1.5:1~2:1.
7. the preparation method of flower-shaped meso-hole structure CdS-ZnO composite materials as claimed in claim 1 or 2, it is characterised in that：Step
（2）In, the calcining carbonization is 1.5 ~ 2h of calcining at 200 ~ 300 DEG C.
8. the preparation method of flower-shaped mesoporous CdS-ZnO as claimed in claim 1 or 2, it is characterised in that：Intermediate product drying be
10 ~ 12h is dried in vacuo at 50 ~ 60 DEG C.
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| CN115025787A (en) * | 2022-05-24 | 2022-09-09 | 西南科技大学 | Preparation method and application of CdS quantum dot modified ZnO nanoflower heterojunction |
| CN115888759A (en) * | 2022-11-15 | 2023-04-04 | 南昌大学 | Synthesis method of alternately bridged cadmium sulfide-zinc oxide heterojunction periodic macroporous photocatalytic hydrogen evolution material |
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| CN113198493A (en) * | 2021-05-17 | 2021-08-03 | 陕西科技大学 | Nanometer flower-like zinc cadmium sulfide solid solution photocatalyst and preparation method thereof |
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| CN115888759A (en) * | 2022-11-15 | 2023-04-04 | 南昌大学 | Synthesis method of alternately bridged cadmium sulfide-zinc oxide heterojunction periodic macroporous photocatalytic hydrogen evolution material |
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